FIELD OF THE INVENTION
[0001] Particulate laundry additive including silicone.
BACKGROUND OF THE INVENTION
[0002] Consumers of laundry detergents enjoy having the ability to customize the technologies
they use in caring for their clothes and household fabrics. This is evidenced by the
vast number of choices of cycles and variations to choose from in modern washing machines,
the variety of pretreatment and wash additives available in the market, and the variety
of laundry treatment compositions to choose from in the market.
[0003] Many consumers have a particular affinity for wearing garments that have a soft feel
and pleasant scent. Liquid fabric enhancers are commonly employed by consumers to
obtain garments having a soft feel and pleasant scent. Since many fabric conditioning
agents are hydrophobic, it can be difficult to provide aqueous liquid products that
include such hydrophobic fabric conditioning agents. Further, many perfume raw materials
have a hydrophobe in their molecular structure. Thus, products that combine hydrophobic
fabric conditioning agents and perfume raw materials having a hydrophobe in their
molecular structure can be difficult to provide to consumers.
[0004] Furthermore, some consumers do not integrate liquid fabric enhancers into their routine
for doing laundry because an extra step that requires care is required. The consumer
must carefully pour the liquid fabric enhancer into the fabric softener dispenser
of the washing machine. Many consumers would prefer a more carefree approach to achieving
the benefit of additional softness and enhanced scent.
[0005] With these limitations in mind, there is a continuing unaddressed need for a product
that combines hydrophobic fabric conditioning agents and perfume that is convenient
to use.
SUMMARY OF THE INVENTION
[0006] A composition comprising: a plurality of first particles comprising: (i) about 30%
to about 98% by weight of said first particles a water soluble first carrier, wherein
said first particles have a first particles onset of melt from about 25 °C to about
120 °C; and perfume carried by said first carrier; and (ii) a plurality of second
particles comprising: about 30% to about 98% by weight of said second particles a
water soluble second carrier, wherein said second particles have a second particles
onset of melt from about 25 °C to about 120 °C; and silicone carried by said second
carrier; wherein said first particles and said second particles are in a package.
[0007] A process for laundering articles of fabric with the composition of the preceding
paragraph comprising the steps of: dispensing said composition according to the preceding
paragraph into a washing machine dispensing into said washing machine a detergent
composition comprising a surfactant, wherein said composition and said detergent composition
are from different packages; placing one or more articles of fabric into said washing
machine; and washing said fabric with said composition and said detergent composition.
BRIEF DESCRIPTION OF THE DRAWINGS
[0008]
Figure 1 is a package containing first particles and second particles, the first particles
are in a first chamber of the package and the second particles are in a second chamber
of the package.
Figure 2 is a package containing first particles and second particles in a single
chamber.
Figure 3 is an apparatus for forming particles.
DETAILED DESCRIPTION OF THE INVENTION
[0009] Particulate laundry additives are known to be attractive to consumers as evidenced
by products such as DOWNY UNSTOPABLES, which is a product that is widely used by consumers.
To date, commercially successful particulate laundry additives have been confined
to stain treatment compositions, such as or including bleach, and laundry scent additives.
One of the attributes of such products is that the consumer enjoys the experience
of dosing such products to the wash and having the feeling of being able to customize
the results obtained from laundering clothing. The consumer can add a lot or a little
of the laundry additive, depending on how the consumer perceives the need and the
level of benefit that is desirable.
[0010] Since there are many tasks to be accomplished in laundering clothes such as, cleaning,
stain removal, brightness, fabric restoration, softness, scent, static control, and
the like, one could in theory provide a separate product for each task to be done
and the consumer could completely customize the kind and amount of each benefit agent
that is applied in the wash. This could become overly complicated for the consumer
and require the consumer to dispense and store multiple products in his or her laundering
area and combine in the optimal quantities. There are thought to be particular combinations
of tasks and benefits to be obtained that the consumer might like to have available
in a single product for which the dose can be customized by the consumer.
[0011] One combination of benefits that consumers are thought to be particularly desirable
of is softness and scent. Silicone is a softening agent that can deliver a particularly
pleasing consumer benefit. Hence, formulating products that include silicone is desirable.
[0012] One approach to formulating such a particulate product might be to provide silicone
and perfume together in a water soluble carrier. The consumer could then dispense
the particles to the wash at the beginning of the wash cycle, during washing and/or
rinsing allowing the water soluble carrier to disperse into water to release the silicone
and perfume, and the silicone and perfume could be deposited on the clothing. Unfortunately,
formulating such a product can prove to be difficult.
[0013] Many water soluble carrier materials are hydrophilic. Hydrophilic water soluble carriers
are desirable since they can be rapidly wetted and dispersed in water. Inconveniently,
many perfume raw materials have a hydrophobic portion and hydrophilic portion. When
silicone and perfume are mixed with a melt of water soluble carrier, it is thought,
without being bound by theory, that possibly the hydrophilic portion of the perfume
raw material is oriented towards the hydrophilic water soluble carrier and the hydrophobic
portion of the perfume raw material is oriented towards the silicone. The interaction
between the hydrophobe of the perfume raw material can drive down the size of the
droplets of silicone in the particles comprising water soluble carrier, perfume, and
silicone. Once the particles are dissolved in water during washing, the small droplets
of silicone may not deposit on fabrics as efficiently as larger droplets. Hence, much
of the silicone, in the form of small droplets, may not be deposited on the fabric
and may be washed away with the rinse water.
[0014] To overcome the difficulties of formulating a particulate product that contains both
silicone and perfume that when dissolved in the wash can provide for large enough
droplets of silicone, it can be convenient to provide the silicone and the perfume
in separate particles in a composition.
[0015] The composition can comprise a plurality of first particles and a plurality of second
particles. The first particles can comprise perfume and the second particles can comprise
silicone. The first particles and second particles can be in a package. Providing
the perfume and silicone in separate particles overcomes the aforesaid problems associated
with trying to provide silicone and perfume in a single particle. The package can
be a package selected from the group consisting of a carton, bottle, water soluble
pouch, and water pervious pouch. The package can have a single chamber or a plurality
of chambers. The package may have two chambers.
[0016] Since the composition comprises both first particles and second particles, combinations
of the two pluralities of particles into a single composition can advantageously be
provided with first particles and second particles that have a first particles onset
of melt and second particles onset of melt that is from about 25 °C to about 120 °C.
First particles and second particles having an onset of melt within such a range can
provide for formula stability from production to use, especially if the first particles
and second particles are packaged together in a single chamber of a package.
[0017] Onset of melt of the particles can provide insight into the ability of the composition
to be stable during shipment, during which the composition might be subjected to elevated
temperatures. For instance, if the composition is expected to be exposed to temperatures
in excess of 35 °C, it can be practical to have the first particles onset of melt
and second particles onset of melt between about 35 °C and about 120 °C. Otherwise,
there is the possibility that the particles forming the composition melt and stick
together, clump, or otherwise become physically combined with one another after production.
Particles that are stuck together end up having a larger mass and may be difficult
to precisely dose to the wash and the masses of particles may not disperse into the
wash water during the washing cycle.
[0018] The first particles can comprise about 30% to about 98% by weight of the first particles
a water soluble first carrier. Such weight fraction of carrier can be practical in
that it leaves enough formulation space in the first particles that benefit agents
can provided in the first particles. The first particles can comprise perfume. The
first particles can comprise encapsulated benefit agents, including encapsulated perfume.
[0019] The second particles can comprise about 30% to about 98% by weight of the second
particles a water soluble second carrier. Such a weight fraction can be practical
for providing formulation space for silicone, and optionally other benefit agents.
[0020] Optionally, the first carrier and the second carrier can be different materials.
By using different carrier materials, the dissolution properties of the first particles
and the second particles can be controlled or set or selected independently. For instance,
it may be beneficial to have the first particles comprising perfume dissolve before
the second particles comprising silicone. Early dissolving perfumed first particles
may provide room bloom of the perfume when the consumer fills the washing tub of a
top load washing machine. Delaying release of the silicone from the second particles
may improve deposition of the silicone on the fabrics in the wash depending on the
wash cycle.
[0021] To simplify manufacturing of the first particles, the first carrier and the perfume
can be mixed with one another. Manufacturing is simplified in that the operator can
provide a mixture of the water soluble carrier and perfume and form the particles
from the mixture. The first carrier and perfume can be mixed with one another or even
homogeneously mixed with one another. Having the perfume dispersed in the first carrier
as a mixture can help to promote controlled release of the perfume as the first particles
dissolve. Release of the perfume can be designed for by employing a particular carrier
that is understood to disperse in the wash at a certain rate at a particular temperature
of the wash liquor.
[0022] Similar to the first carrier and perfume, the second carrier and the silicone can
be mixed with one another. Such an arrangement might provide a benefit of relatively
slow release of silicone which might promote better deposition onto fabrics. The silicone
can be dispersed in the second carrier, and thereby second particles, as droplets.
[0023] The composition can comprise from about 10% to about 90% by weight the first particles
and from about 10% to about 90% by weight the second particles. The first particles
and the second particles can be packaged together. Packaged together, first particles
and second particles in the aforesaid ranges can provide both a scent benefit and
a softness benefit to fabrics when washed in a solution in which such particles are
dissolved. The levels of the two fractions of particles can be set to provide the
desired balance of scent benefit and softness benefit in the final composition when
used. The composition can comprise about 35% by weight first particles and about 65%
by weight second particles.
[0024] Importantly, the options for formulating a composition for consumers is flexible.
For instance, the first particles and second particles may be produced on separate
runs on the same manufacturing line or on separate manufacturing lines. The first
particles and second particles can be mixed together prior to packaging in a single
package to provide a mixture of first particles and second particles. The manufacturer
can choose to balance the mixture of first particles and second particles to provide
consumers with the desired scent benefit and softness benefit. The manufacture may
even choose to provide a lineup of compositions having different levels of the first
particles and second particles. For instance, the manufacturer can provide one composition
that has a balance of first particles and second particles that is most consumer preferred,
a second composition that is weighted towards providing a more noticeable scent benefit
with less of a softness benefit, and a third composition that is weighted towards
providing a more noticeable softness benefit with less of a scent benefit. This approach
can allow the manufacturer to serve a variety of consumers' desires for benefits.
[0025] The composition can be used in process to launder articles of fabric in a washing
machine. The process can comprise the steps as follows. Dispensing a composition comprising
first particles and second particles into the washing machine. Dispensing a detergent
composition comprising a surfactant into the washing machine, wherein the detergent
composition is dispensed independently from the composition comprising first particles
and second particles. Placing articles of fabric with the washing machine. Washing
the fabric with a solution comprising the composition comprising first particles and
second particles and the detergent composition. The detergent composition can comprise
from about 15% to about 90% by weight surfactant. The composition comprising first
particles and second particles can comprise less than 5% by weight surfactant. The
composition comprising first particles and second particles can be dispensed before
or after the detergent composition is dispensed.
[0026] The detergent composition can comprise a fully formulated laundry detergent composition.
Fully formulated laundry detergent compositions can be products including, but not
limited to, TIDE ORIGINAL liquid and TIDE ORIGINAL powder, manufactured by the Procter
& Gamble Co., Cincinnati, Ohio, or similar such laundry detergent compositions. Fully
formulated laundry detergent compositions typically comprise surfactant, perfume,
brighteners, hueing dyes, and the like. The composition comprising first particles
and second particles can be provided in a package separate from the package in which
the detergent composition is provided.
[0027] The composition comprising first particles and second particles can be free of, substantially
free of, or can comprise less than 5% by weight of the composition surfactant, or
less than 1% by weight of the composition surfactant. Such composition of first particles
and second particles may be easier to produce than particles having a higher level
of surfactant.
[0028] The composition can comprise a mixture of first particles and second particles as
described herein. The composition can be first particles and second particles packaged
together. For example, the first particles and the second particles can be packaged
together in a single chamber of package. The first particles and second particles
can be packaged together in a package comprising a first chamber and a second chamber,
wherein the first particles are within the first chamber of the package and the second
particles are within the second chamber of the package.
[0029] The first particles 200 and second particles 210 can be packaged in a package 220,
as shown in Figs. 1 and 2. The first particles 200 and second particles 210 can be
packaged in a first chamber 240 and second chamber 250, respectively, as shown in
Fig. 1. The first particles 200 and the second particles 210 can be packaged in a
single chamber 230 of the package 220, as shown in Fig. 2.
SILICONE
[0030] The second particles can comprise about 0.1% to about 60% by weight of the second
particles silicone. The second particles can comprise about 3% to about 50% by weight
of the second particles silicone. The second particles can comprise about 10% to about
40% by weight of the second particles silicone. The second particles can comprise
about 20% to about 35% by weight of the second particles silicone. The second particles
can comprise about 28% to about 32% by weight of the second particles silicone.
[0031] The first particles can comprise less than 0.1% by weight of the first particles
silicone. The first particles can comprise less than 1% by weight of the first particles
silicone. The first particles can comprise less than 3% by weight of the first particles
silicone.
[0032] Suitable silicones comprise Si-O moieties and may be selected from (a) non-functionalized
siloxane polymers, (b) functionalized siloxane polymers, and combinations thereof.
The molecular weight of the organosilicone is usually indicated by the reference to
the viscosity of the material. In one aspect, the organosilicones may comprise a viscosity
of from about 10 to about 2,000,000 centistokes at 25°C. In another aspect, suitable
organosilicones may have a viscosity of from about 10 to about 800,000 centistokes
at 25°C.
Suitable organosilicones may be linear, branched or cross-linked. In one aspect, the
organosilicones may comprise silicone resins. Silicone resins are highly cross-linked
polymeric siloxane systems. The cross-linking is introduced through the incorporation
of trifunctional and tetrafunctional silanes with monofunctional or difunctional,
or both, silanes during manufacture of the silicone resin. As used herein, the nomenclature
SiO"n"/2 represents the ratio of oxygen and silicon atoms. For example, SiO
1/2 means that one oxygen is shared between two Si atoms. Likewise SiO
2/2 means that two oxygen atoms are shared between two Si atoms and SiO
3/2 means that three oxygen atoms are shared are shared between two Si atoms.
[0033] Silicone materials and silicone resins in particular, can conveniently be identified
according to a shorthand nomenclature system known to those of ordinary skill in the
art as "MDTQ" nomenclature. Under this system, the silicone is described according
to presence of various siloxane monomer units which make up the silicone. Briefly,
the symbol M denotes the monofunctional unit (CH
3)
3SiO
0.5; D denotes the difunctional unit (CH
3)
2SiO; T denotes the trifunctional unit (CH
3)SiO
1.5; and Q denotes the quadra- or tetra-functional unit SiO
2. Primes of the unit symbols (e.g. M', D', T', and Q') denote substituents other than
methyl, and must be specifically defined for each occurrence.
[0034] Other modified silicones or silicone copolymers are also useful herein. Examples
of these include silicone-based quaternary ammonium compounds (Kennan quats) disclosed
in
U.S. Patents 6,607,717 and
6,482,969; end-terminal quaternary siloxanes; silicone aminopolyalkyleneoxide block copolymers
disclosed in
U.S. Patents 5,807,956 and
5,981,681; hydrophilic silicone emulsions disclosed in
U.S. Patent 6,207,782; and polymers made up of one or more crosslinked rake or comb silicone copolymer
segments disclosed in
US Patent 7,465,439. Additional modified silicones or silicone copolymers useful herein are described
in
US Patent Publications 2007/0286837A1 and
2005/0048549A1.
[0035] In alternative embodiments of the present invention, the above-noted silicone-based
quaternary ammonium compounds may be combined with the silicone polymers described
in
US Patents 7,041,767 and
7,217,777 and
US Patent Publication 2007/0041929A1.
In one aspect, the organosilicone may comprise a non-functionalized siloxane polymer
that may have the following formula, and may comprise polyalkyl and/or phenyl silicone
fluids, resins and/or gums.
[R
1R
2R
3SiO
1/2]
n [R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
- i) each R1, R2, R3 and R4 may be independently selected from the group consisting of H, -OH, C1-C20 alkyl, C1-C20 substituted alkyl, C6-C20 aryl, C6-C20 substituted aryl, alkylaryl, and/or C1-C20 alkoxy, moieties;
- ii) n may be an integer from about 2 to about 10, or from about 2 to about 6; or 2;
such that n = j+2;
- iii) m may be an integer from about 5 to about 8,000, from about 7 to about 8,000
or from about 15 to about 4,000;
- iv) j may be an integer from 0 to about 10, or from 0 to about 4, or 0.
[0036] In one aspect, R
2, R
3 and R
4 may comprise methyl, ethyl, propyl, C
4-C
20 alkyl, and/or C
6-C
20 aryl moieties. In one aspect, each of R
2, R
3 and R
4 may be methyl. Each R
1 moiety blocking the ends of the silicone chain may comprise a moiety selected from
the group consisting of hydrogen, methyl, methoxy, ethoxy, hydroxy, propoxy, and/or
aryloxy.
[0037] In one aspect, the organosilicone may be polydimethylsiloxane, dimethicone, dimethiconol,
dimethicone crosspolymer, phenyl trimethicone, alkyl dimethicone, lauryl dimethicone,
stearyl dimethicone and phenyl dimethicone. Examples include those available under
the names DC 200 Fluid, DC 1664, DC 349, DC 346G available from Dow Corning Corporation,
Midland, MI, and those available under the trade names SF1202, SF1204, SF96, and VISCASIL
available from Momentive Silicones, Waterford, NY.
[0038] In one aspect, the organosilicone may comprise a cyclic silicone. The cyclic silicone
may comprise a cyclomethicone of the formula [(CH
3)
2SiO]
n where n is an integer that may range from about 3 to about 7, or from about 5 to
about 6.
[0039] In one aspect, the organosilicone may comprise a functionalized siloxane polymer.
Functionalized siloxane polymers may comprise one or more functional moieties selected
from the group consisting of amino, amido, alkoxy, hydroxy, polyether, carboxy, hydride,
mercapto, sulfate phosphate, and/or quaternary ammonium moieties. These moieties may
be attached directly to the siloxane backbone through a bivalent alkylene radical,
(i.e., "pendant") or may be part of the backbone. Suitable functionalized siloxane
polymers include materials selected from the group consisting of aminosilicones, amidosilicones,
silicone polyethers, silicone-urethane polymers, quaternary ABn silicones, amino ABn
silicones, and combinations thereof.
[0040] In one aspect, the functionalized siloxane polymer may comprise a silicone polyether,
also referred to as "dimethicone copolyol." In general, silicone polyethers comprise
a polydimethylsiloxane backbone with one or more polyoxyalkylene chains. The polyoxyalkylene
moieties may be incorporated in the polymer as pendent chains or as terminal blocks.
Such silicones are described in
US Patent Publication 2005/0098759, and
US Patents 4,818,421 and
3,299,112. Exemplary commercially available silicone polyethers include DC 190, DC 193, FF400,
all available from Dow Corning Corporation, and various SILWET surfactants available
from Momentive Silicones.
[0041] In another aspect, the functionalized siloxane polymer may comprise an aminosilicone.
Suitable aminosilicones are described in
US Patents 7,335,630 B2,
4,911,852, and
US Patent Publication 2005/0170994A1. In one aspect the aminosilicone may be that described in
US Provisional Patent Application 61/221,632. In another aspect, the aminosilicone may comprise the structure of the following
formula:
[R
1R
2R
3SiO
1/2]
n[(R
4Si(X-Z)O
2/2]
k[R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
- i. R1, R2, R3 and R4 may each be independently selected from H, OH, C1-C20 alkyl, C1-C20 substituted alkyl, C6-C20 aryl, C6-C20 substituted aryl, alkylaryl, and/or C1-C20 alkoxy;
- ii. Each X may be independently selected from a divalent alkylene radical comprising
2-12 carbon atoms, -(CH2)s- wherein s may be an integer from about 2 to about 10; - CH2-CH(OH)-CH2-; and/or

- iii. Each Z may be independently selected from-N(R5)2;

and

wherein each R5 may be selected independently selected from H, C1-C20 alkyl; and A- may be a compatible anion. In one aspect, A- may be a halide;
- iv. k may be an integer from about 3 to about 20, from about 5 to about 18 more or
even from about 5 to about 10;
- v. m may be an integer from about 100 to about 2,000, or from about 150 to about 1,000;
- vi. n may be an integer from about 2 to about 10, or about 2 to about 6, or 2, such
that n = j+2; and
- vii. j may be an integer from 0 to about 10, or from 0 to about 4, or 0.
[0042] In one aspect, R
1 may comprise -OH. In this aspect, the organosilicone is amidomethicone. Exemplary
commercially available aminosilicones include DC 8822, 2-8177, and DC-949, available
from Dow Corning Corporation, and KF-873, available from Shin-Etsu Silicones, Akron,
OH.
[0043] In one aspect the silicone may be chosen from a random or blocky organosilicone polymer
having the following formula:
[R
1R
2R
3SiO
1/2]
(j+2)[(R
4Si(X-Z)O
2/2]
k[R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
j is an integer from 0 to about 98; in one aspect j is an integer from 0 to about
48; in one aspect, j is 0;
k is an integer from 0 to about 200, in one aspect k is an integer from 0 to about
50; when k = 0, at least one of R1, R2 or R3 is -X-Z;
m is an integer from 4 to about 5,000; in one aspect m is an integer from about 10
to about 4,000; in another aspect m is an integer from about 50 to about 2,000;
R1, R2 and R3 are each independently selected from the group consisting of H, OH, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, C6-C32 substituted alkylaryl, C1-C32 alkoxy, C1-C32 substituted alkoxy and X-Z;
each R4 is independently selected from the group consisting of H, OH, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, C6-C32 substituted alkylaryl, C1-C32 alkoxy and C1-C32 substituted alkoxy;
each X in said alkyl siloxane polymer comprises a substituted or unsubsitituted divalent
alkylene radical comprising 2-12 carbon atoms, in one aspect each divalent alkylene
radical is independently selected from the group consisting of - (CH2)s- wherein s is an integer from about 2 to about 8, from about 2 to about 4;
in one aspect, each X in said alkyl siloxane polymer comprises a substituted divalent
alkylene radical selected from the group consisting of: -CH2-CH(OH)-CH2-; -CH2-CH2-CH(OH)-; and

each Z is selected independently from the group consisting of



with the proviso that when Z is a quat, Q cannot be an amide, imine, or urea moiety;
for Z An- is a suitable charge balancing anion. In one aspect An- is selected from the group consisting of Cl-, Br-,I-, methylsulfate, toluene sulfonate, carboxylate and phosphate ; and at least one Q
in said organosilicone is independently selected from -CH2-CH(OH)-CH2-R5;



each additional Q in said organosilicone is independently selected from the group
comprising of H, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, C6-C32 substituted alkylaryl, -CH2-CH(OH)-CH2-R5;



wherein each R5 is independently selected from the group consisting of H, C1-C32 alkyl, C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl, C6-C32 substituted alkylaryl, -(CHR6-CHR6-O-)w-L and a siloxyl residue;
each R6 is independently selected from H, C1-C18 alkyl
each L is independently selected from -C(O)-R7 or R7;
w is an integer from 0 to about 500, in one aspect w is an integer from about 1 to
about 200; in one aspect w is an integer from about 1 to about 50;
each R7 is selected independently from the group consisting of H; C1-C32 alkyl; C1-C32 substituted alkyl, C5-C32 or C6-C32 aryl, C5-C32 or C6-C32 substituted aryl, C6-C32 alkylaryl; C6-C32 substituted alkylaryl and a siloxyl residue;
each T is independently selected from H, and


and
wherein each v in said organosilicone is an integer from 1 to about 10, in one aspect,
v is an integer from 1 to about 5 and the sum of all v indices in each Q in the said
organosilicone is an integer from 1 to about 30 or from 1 to about 20 or even from
1 to about 10.
[0044] In one aspect, the organosilicone may comprise amine ABn silicones and quat ABn silicones.
Such organosilicones are generally produced by reacting a diamine with an epoxide.
These are described, for example, in
US Patents 6,903,061,
5,981,681,
5,807,956,
6,903,061 and
7,273,837. These are commercially available under the trade names MAGNASOFT, PRIME, MAGNASOFT
JSS, SILSOFT, and A-858, all from Momentive Silicones.
[0045] In another aspect, the functionalized siloxane polymer may comprise silicone-urethanes,
such as those described in
US Provisional Patent Application 61/170,150. These are commercially available from Wacker Silicones under the trade name SLM-21200.
[0046] When a sample of organosilicone is analyzed, it is recognized by the skilled artisan
that such sample may have, on average, the non-integer indices for Formula (I) and
(II) above, but that such average indices values will be within the ranges of the
indices for Formula (I) and (II) above.
[0047] The silicone can be an aminosilicone having the formula:
[R
1R
2R
3SiO
1/2]
(j+2)[(R
4Si(X-Z)O
2/2]
k[R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
j is 0;
k is an integer from 1 to about 10;
m is an integer from 150 to about 1000; in one aspect m is an integer from about 325
to about 750 ; in another aspect m is an integer from about 400 to about 600 ;
each R1, R2 and R3 is C1-C32 alkoxy and or C1-C32 alkyl;
each R4 is C1-C32 alkyl
each X is selected from the group consisting of -(CH2)s- wherein s is an integer from about 2 to about 8, from about 2 to about 4;
each Z is selected independently from the group consisting of

each Q in said silicone is selected from the group comprising of H;
The silicone can be an aminosilicone having the formula:
[R
1R
2R
3SiO
1/2]
(j+2)[(R
4Si(X-Z)O
2/2]
k[R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
j is 0;
k is an integer from 1 to about 10;
m is an integer from 150 to about 1000; in one aspect m is an integer from about 325
to about 750 ; in another aspect m is an integer from about 400 to about 600 ;
each R1, R2 and R3 is C1-C32 alkoxy and or C1-C32 alkyl;
each R4 is C1-C32 alkyl
each X is selected from the group consisting of -(CH2)s- wherein s is an integer from about 2 to about 8, from about 2 to about 4;
each Z is selected independently from the group consisting of

each Q in said silicone is selected from the group comprising of H;
[0048] The silicone can be an aminosilicone having the formula:
[R
1R
2R
3SiO
1/2]
(j+2)[(R
4Si(X-Z)O
2/2]
k[R
4R
4SiO
2/2]
m[R
4SiO
3/2]
j
wherein:
j is 0;
k is an integer from 1 to about 5;
m is an integer from 250 to about 750; in one aspect m is an integer from about 325
to about 675; in another aspect m is an integer from about 400 to about 600 ;
each R1, R2 and R3 is C1-C32 alkoxy and or C1-C32 alkyl;
each R4 is C1-C32 alkyl
each X is selected from the group consisting of -(CH2)s- wherein s is an integer from about 2 to about 8, from about 2 to about 4;
each Z is selected independently from the group consisting of

each additional Q in said silicone is independently selected from the group consisting
of H, C1-C32 alkyl, C1-C32 substituted alkyl, C6-C32 aryl, C5-C32 substituted aryl,
C6-C32 alkylaryl, C5-C32 substituted alkylaryl; with the proviso that both Q cannot
be H atoms.
[0049] The silicone can be mixed with the second carrier. The silicone can be dispersed
in the second carrier. The silicone can be dispersed in the second carrier as droplets.
The mean particle size of the silicone disposed in the second carrier material can
be from about 2 µm to about 2000 µm. The mean particle size of the silicone disposed
in the second carrier is determined according to the MEAN PARTICLE SIZE method described
herein below.
[0050] The optimal mean particle size of the silicone may depend upon the intended use of
the composition. For instance, a fabric softening product composition for conditioning
fabrics in a laundry process may contain silicone having a mean particle size of from
about 2 µm to about 500 µm, or from about 2 µm to about 120 µm, or from about 2 µm
to about 70 µm. Droplets of silicone that are too small may not adequately deposit
onto fibers of the fabric items being washed. Droplets of silicone that are too large
may result in spotting of the fibers of the fabric items.
[0051] Since the composition is in a solid form, the particle size of the silicone will
generally remain constant during packaging, shipping and storage of the composition.
[0052] The silicone can be dimethyl, methyl (3-aminopropyl) siloxane, trimethylsiloxy-terminated,
CAS-No. 99363-37-8, available from Dow Corning as Dow Corning as DOW CORNING(R) XX-8766 AMINO POLYMER,
product code 000000000004121334. An exemplary silicone can be the following formula.

[0053] The silicone can be an aminosilicone having the following formula:

[0054] The silicone can be an anionic silicone. Examples of anionic silicones are silicones
that incorporate carboxylic, sulphate, sulphonic, phosphate and/or phosphonate functionality.
The anionic silicone may be in the form of the acid or the anion. For example for
the carboxyl functionalised silicone, it may be present as a carboxylic acid or carboxylate
anion. The anionic silicone can have a molecular weight of from 1,000 to 100,000,
or from 2,000 to 50,000, or even more from 5,000 to 50,000, or even from 10,000 to
50,000.
PARTICLES
[0055] Optionally, for any of the compositions and particles disclosed herein, whether they
be first particles or second particles, individual particles can have a mass of from
about 1 mg to about 5000 mg, alternatively from about 5 mg to about 1000 mg, alternatively
from about 5 mg to about 200 mg, alternatively from about 10 mg to about 100 mg, alternatively
from about 20 mg to about 50 mg, alternatively from about 35 mg to about 45 mg, alternatively
about 38 mg, alternatively combinations thereof and any whole numbers or ranges of
whole numbers of mg within any of the aforementioned ranges. First particles and or
second particles having a mass in the aforesaid ranges can have dissolution times
in water that permit the particles to dissolve during a typical wash cycle. Individual
first particles and or second particles can have a shape selected from the group consisting
of spherical, hemispherical, compressed hemispherical, lentil shaped, and oblong.
[0056] The first particles and or second particles can have a mean particle mass of from
about 1 mg to about 5000 mg, alternatively from about 5 mg to about 1000 mg, alternatively
from about 5 mg to about 200 mg, alternatively from about 10 mg to about 100 mg, alternatively
from about 20 mg to about 50 mg, alternatively from about 35 mg to about 45 mg, alternatively
about 38 mg. The first particles and or second particles can have a standard deviation
of mass of less than 30 mg, alternatively less than 15 mg, alternatively less than
5 mg, alternatively about 3 mg. The mean particle mass within the aforesaid ranges
can provide for a dissolution time in water that permits the particles to dissolve
during a typical wash cycle. Without being bound by theory, it is thought that first
particles and or second particles having such a standard deviation of mass can have
a more uniform dissolution time in water as compared to particles having a broader
standard deviation of mass. The smaller the standard deviation of mass of the particles
the more uniform the dissolution time is expected to be. The mass of the individual
first particles and or second particles can be set to provide the desired dissolution
time, which might be some fraction of the length of the typical washing cycle in a
washing machine. Particles formed from polyethylene glycol having a weight average
molecular weight of about 9000 can have mean particle mass of about 38 mg and standard
deviation of mass of about 3 mg. For clarity, the aforesaid disclosure on mean particle
size is meant to apply individually to the first particles, individually to the second
particles, and to the mixture of first particles and second particles.
[0057] An individual first particle or second particle may have a volume from about 0.003
cm
3 to about 5 cm
3, alternatively from about 0.003 cm
3 to about 1 cm
3, alternatively from about 0.003 cm
3 to about 0.5 cm
3, alternatively from about 0.003 cm
3 to about 0.2 cm
3, alternatively from about 0.003 cm
3 to about 0.15 cm
3. Smaller particles are thought to provide for better packing of the particles in
a package and faster dissolution in the wash. For clarity, the aforesaid disclosure
on volume of individual particles is meant to apply individually to the first particles,
individually to the second particles, and to the mixture of first particles and second
particles.
[0058] The composition can comprise first particles and or second particles that are retained
on a number 10 sieve as specified by ASTM International, ASTM E11 - 13. The composition
can comprise first particles and or second particles wherein more than 50% by weight
of the particles are retained on a number 10 sieve as specified by ASTM International,
ASTM E11 - 13. The composition can comprise first particles and or second particles
wherein more than 70% by weight of the particles are retained on a number 10 sieve
as specified by ASTM International, ASTM E11 - 13. The composition can comprise first
particles and or second particles wherein more than 90% by weight of the particles
are retained on a number 10 sieve as specified by ASTM International, ASTM E11 - 13.
For clarity, the aforesaid disclosure on particles retained on a number 10 sieve is
meant to apply individually to the first particles, individually to the second particles,
and to the mixture of first particles and second particles. It can be desirable to
provide particles sized as such because particles retained on a number 10 sieve may
be easier to handle than smaller particles.
[0059] The composition can comprise first particles and or second particles that are retained
on a number 6 sieve as specified by ASTM International, ASTM E11 - 13. The composition
can comprise first particles and or second particles wherein more than 50% by weight
of the particles are retained on a number 6 sieve as specified by ASTM International,
ASTM E11 - 13. The composition can comprise first particles and or second particles
wherein more than 70% by weight of the particles are retained on a number 6 sieve
as specified by ASTM International, ASTM E11 - 13. The composition can comprise first
particles and or second particles wherein more than 90% by weight of the particles
are retained on a number 6 sieve as specified by ASTM International, ASTM E11 - 13.
It can be desirable to provide first particles and or second particles sized as such
because particles retained on a number 6 sieve may be easier to handle than smaller
particles.
[0060] The composition can comprise first particles and or second particles that pass a
sieve having a nominal sieve opening size of 22.6 mm. The composition can comprise
first particles and or second particles that pass a sieve having a nominal sieve opening
size of 22.6 mm and are retained on a sieve having a nominal sieve opening size of
0.841 mm. First particles and or second particles having a size such that they are
retained on a sieve having a nominal opening size of 22.6 mm may tend to have a dissolution
time that is too great for a common wash cycle. First particles and or second particles
having a size such that they pass a sieve having a nominal sieve opening size of 0.841
mm may be too small to conveniently handle. First particles and or second particles
having a size within the aforesaid bounds may represent an appropriate balance between
dissolution time and ease of particle handling.
[0061] First particles and or second particles having the size disclosed herein can be substantial
enough so that they do not readily become airborne when poured from a package, dosing
cup, or other apparatus, into a wash basin or washing machine. Further, such first
particles and or second particles as disclosed herein can be easily and accurately
poured from a package into a dosing cup.
[0062] A plurality of first particles and or second particles may collectively comprise
a dose for dosing to a laundry washing machine or laundry wash basin. A single dose
of the particles may comprise from about 1 g to about 27 g of first particles and
or second particles. A single dose of the first particles and or second particles
may comprise from about 5 g to about 27 g, alternatively from about 13 g to about
27 g, alternatively from about 14 g to about 20 g, alternatively from about 15 g to
about 19 g, alternatively from about 18 g to about 19 g, alternatively combinations
thereof and any whole numbers of grams or ranges of whole numbers of grams within
any of the aforementioned ranges. The individual first particles and or second particles
forming the plurality of particles that can make up the dose can have a mass from
about 1 mg to about 5000 mg, alternatively from about 5 mg to about 1000 mg, alternatively
from about 5 mg to about 200 mg, alternatively from about 10 mg to about 100 mg, alternatively
from about 20 mg to about 50 mg, alternatively from about 35 mg to about 45 mg, alternatively
about 38 mg, alternatively combinations thereof and any whole numbers or ranges of
whole numbers of mg within any of the aforementioned ranges. The plurality of first
particles and or second particles can be made up of particles having different size,
shape, and/or mass. The first particles and or second particles in a dose can each
have a maximum dimension less than 15 mm. Each of the first particles and or second
particles in a dose can have a maximum dimension less than 1 cm.
[0063] The first particles and or second particles disclosed herein can be conveniently
employed to treat laundry articles. The steps of the process can be to provide such
first particles and or second particles comprising the formulation components disclosed
herein. A dose of the first particles and or second particles can be placed in a dosing
cup. The dosing cup can be the closure of a package containing the particles. The
dosing cup can be a detachable and attachable dosing cup that is detachable and attachable
to a package containing the first particles and or second particles or to the closure
of such package. The dose of first particles and or second particles in the dosing
cup can be dispensed into a washing machine. The step of dispensing the particles
in the washing machine can take place by pouring the first particles and or second
particles into the washing machine or placing the dosing cup and the particles contained
therein into the washing machine.
[0064] The composition of first particles and second particles disclosed herein can be convenient
for the consumer to dose into a washing machine. For instance, the consumer can pour
the composition from a package that contains the first particles and second particles.
The first particles and second particles can be a mixture of such particles in a single
chamber of the package. The first particles can be in a first chamber of the package
and the second particles can be in a second chamber of the package.
[0065] Optionally, the consumer can pour the first particles and second particles into a
measuring cup that is separate from the package or in which the composition is provided
or into a measuring cup that is part of the package in which the composition is provided.
The measuring cup can be a closure of the package in which the composition is provided.
The measuring cup can be attachable and detachable from the closure of the package
in which the composition is provided.
[0066] The composition of the mixture of first particles and second particles can have a
coefficient of uniformity of less than 2. Having a coefficient of uniformity of less
than 2 can help reduce the potential for the particles when packaged together in a
single chamber of a package to segregate as compared to mixtures of particles having
a coefficient of uniformity greater than 2. Particle size, coefficient of uniformity,
D50, and D10, as discussed further below, are measured according to ASTM D6913-04(2009)e1.
[0067] The composition can be such that the first particles have a first particles D50 and
the second particles have a second particles D50, wherein the second particles D50
is within about 20% of the first particles D50. The composition can be such that the
first particles have a first particles D50 and the second particles have a second
particles D50, wherein the second particles D50 is within about 10% of the first particles
D50. The composition can be such that the first particles have a first particles D50
and the second particles have a second particles D50, wherein the second particles
D50 is within about 5% of the first particles D50. Having the D50 of the first particles
and the second particles related as such can be practical for simplifying processing
of the first particles and the second particles and mixing the two, with smaller differences
in D50 meaning that the first particles and second particles are more similarly shaped
to one another and easier to manufacture, mix, and store. Further, having the first
particles and second particles have similar D50 sizes can help reduce the potential
for the first particles and second particles to segregate once mixed or packaged together
in a single chamber of a package, with the potential being reduced as the difference
in D50 between the respective particles decreases.
[0068] Depending on the carrier materials employed, there is potential for silicone from
the second particles to migrate into the first particles. Similarly, there is the
potential for perfume in first particles to migrate into the second particles. The
second particles have a weight fraction of silicone greater than the weight fraction
of silicon in the first particles and the weight fraction of silicone in the first
particles can be about zero or zero. Stated similarly, the weight fraction of silicone
in the second particles is greater than the weight fraction of silicone in the first
particles, the weight fraction of silicone in the first particles being as low as
about zero or zero.
[0069] The first particles can have less than 5% by weight of the first particles of silicone.
The first particles can have less than about 2% by weight of the first particles of
silicone. The first particles can have less than about 1% by weight of the first particles
of silicone.
WATER SOLUBLE CARRIER
[0070] The water soluble first carrier and water soluble second carrier can be or comprise
a material selected from the group consisting of water soluble inorganic alkali metal
salt, water-soluble alkaline earth metal salt, water-soluble organic alkali metal
salt, water-soluble organic alkaline earth metal salt, water soluble carbohydrate,
water-soluble silicate, water soluble urea, and any combination thereof. The water
soluble first carrier and the water soluble second carrier can both be the same material
or different materials. Alkali metal salts can be, for example, selected from the
group consisting of salts of lithium, salts of sodium, and salts of potassium, and
any combination thereof. Useful alkali metal salts can be, for example, selected from
the group consisting of alkali metal fluorides, alkali metal chlorides, alkali metal
bromides, alkali metal iodides, alkali metal sulfates, alkali metal bisulfates, alkali
metal phosphates, alkali metal monohydrogen phosphates, alkali metal dihydrogen phosphates,
alkali metal carbonates, alkali metal monohydrogen carbonates, alkali metal acetates,
alkali metal citrates, alkali metal lactates, alkali metal pyruvates, alkali metal
silicates, alkali metal ascorbates, and combinations thereof.
[0071] Alkali metal salts can be selected from the group consisting of, sodium fluoride,
sodium chloride, sodium bromide, sodium iodide, sodium sulfate, sodium bisulfate,
sodium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium
carbonate, sodium hydrogen carbonate, sodium acetate, sodium citrate, sodium lactate,
sodium tartrate, sodium silicate, sodium ascorbate, potassium fluoride, potassium
chloride, potassium bromide, potassium iodide, potassium sulfate, potassium bisulfate,
potassium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate,
potassium carbonate, potassium monohydrogen carbonate, potassium acetate, potassium
citrate, potassium lactate, potassium tartrate, potassium silicate, potassium, ascorbate,
and combinations thereof. Alkaline earth metal salts can be selected from the group
consisting of salts of magnesium, salts of calcium, and the like, and combinations
thereof. Alkaline earth metal salts can be selected from the group consisting of alkaline
metal fluorides, alkaline metal chlorides, alkaline metal bromides, alkaline metal
iodides, alkaline metal sulfates, alkaline metal bisulfates, alkaline metal phosphates,
alkaline metal monohydrogen phosphates, alkaline metal dihydrogen phosphates, alkaline
metal carbonates, alkaline metal monohydrogen carbonates, alkaline metal acetates,
alkaline metal citrates, alkaline metal lactates, alkaline metal pyruvates, alkaline
metal silicates, alkaline metal ascorbates, and combinations thereof. Alkaline earth
metal salts can be selected from the group consisting of magnesium fluoride, magnesium
chloride, magnesium bromide, magnesium iodide, magnesium sulfate, magnesium phosphate,
magnesium monohydrogen phosphate, magnesium dihydrogen phosphate, magnesium carbonate,
magnesium monohydrogen carbonate, magnesium acetate, magnesium citrate, magnesium
lactate, magnesium tartrate, magnesium silicate, magnesium ascorbate, calcium fluoride,
calcium chloride, calcium bromide, calcium iodide, calcium sulfate, calcium phosphate,
calcium monohydrogen phosphate, calcium dihydrogen phosphate, calcium carbonate, calcium
monohydrogen carbonate, calcium acetate, calcium citrate, calcium lactate, calcium
tartrate, calcium silicate, calcium ascorbate, and combinations thereof. Inorganic
salts, such as inorganic alkali metal salts and inorganic alkaline earth metal salts,
do not contain carbon. Organic salts, such as organic alkali metal salts and organic
alkaline earth metal salts, contain carbon. The organic salt can be an alkali metal
salt or an alkaline earth metal salt of sorbic acid (i.e., asorbate). Sorbates can
be selected from the group consisting of sodium sorbate, potassium sorbate, magnesium
sorbate, calcium sorbate, and combinations thereof.
[0072] The water soluble first carrier and water soluble second carrier can be or comprise
a material selected from the group consisting of a water-soluble inorganic alkali
metal salt, a water-soluble organic alkali metal salt, a water-soluble inorganic alkaline
earth metal salt, a water-soluble organic alkaline earth metal salt, a water-soluble
carbohydrate, a water-soluble silicate, a water-soluble urea, and combinations thereof.
The water soluble first carrier and water soluble second carrier can be selected from
the group consisting of sodium chloride, potassium chloride, calcium chloride, magnesium
chloride, sodium sulfate, potassium sulfate, magnesium sulfate, sodium carbonate,
potassium carbonate, sodium hydrogen carbonate, potassium hydrogen carbonate, sodium
acetate, potassium acetate, sodium citrate, potassium citrate, sodium tartrate, potassium
tartrate, potassium sodium tartrate, calcium lactate, water glass, sodium silicate,
potassium silicate, dextrose, fructose, galactose, isoglucose, glucose, sucrose, raffinose,
isomalt, xylitol, candy sugar, coarse sugar, and combinations thereof. In one embodiment,
the first water soluble carrier and/or the second water soluble carrier can be sodium
chloride. In one embodiment, the first water soluble carrier and second water soluble
carrier can be table salt.
[0073] The first water soluble carrier and second water soluble carrier can be or comprise
a material selected from the group consisting of sodium bicarbonate, sodium sulfate,
sodium carbonate, sodium formate, calcium formate, sodium chloride, sucrose, maltodextrin,
corn syrup solids, corn starch, wheat starch, rice starch, potato starch, tapioca
starch, clay, silicate, citric acid carboxymethyl cellulose, fatty acid, fatty alcohol,
glyceryl diester of hydrogenated tallow, glycerol, and combinations thereof. The first
water soluble carrier and the second water soluble carrier can be the same material
or different materials. Employing the same water soluble carrier for the first water
soluble carrier and second water soluble carrier can be practical for simplifying
the manufacturer's supply chain and allowing the manufacturer to apply learnings from
the manufacture of one of the particles to the other particles. Using different materials
for the first water soluble carrier and the second water soluble carrier can be practical
for providing different dissolution behavior in the wash, different tactile feel to
the particles, different visual impression of the particles, and for enabling the
consumer to recognize that the composition she is using comprises two different kinds
of particles.
[0074] The first water soluble carrier and second water soluble carrier can be selected
from the group consisting of water soluble organic alkali metal salt, water soluble
inorganic alkaline earth metal salt, water soluble organic alkaline earth metal salt,
water soluble carbohydrate, water soluble silicate, water soluble urea, starch, clay,
water insoluble silicate, citric acid carboxymethyl cellulose, fatty acid, fatty alcohol,
glyceryl diester of hydrogenated tallow, glycerol, polyethylene glycol, and combinations
thereof.
[0075] The first water soluble carrier and second water soluble carrier can be selected
from the group consisting of disaccharides, polysaccharides, silicates, zeolites,
carbonates, sulfates, citrates, and combinations thereof.
[0076] The first water soluble carrier and second water soluble carrier can be a water soluble
polymer. Examples of water soluble polymers include but are not limited to polyvinyl
alcohols (PVA), modified PVAs; polyvinyl pyrrolidone; PVA copolymers such as PVA/polyvinyl
pyrrolidone and PVA/ polyvinyl amine; partially hydrolyzed polyvinyl acetate; polyalkylene
oxides such as polyethylene oxide; polyethylene glycols; acrylamide; acrylic acid;
cellulose, alkyl cellulosics such as methyl cellulose, ethyl cellulose and propyl
cellulose; cellulose ethers; cellulose esters; cellulose amides; polyvinyl acetates;
polycarboxylic acids and salts; polyaminoacids or peptides; polyamides; polyacrylamide;
copolymers of maleic/acrylic acids; polysaccharides including starch, modified starch;
gelatin; alginates; xyloglucans, other hemicellulosic polysaccharides including xylan,
glucuronoxylan, arabinoxylan, mannan, glucomannan and galactoglucomannan; and natural
gums such as pectin, xanthan, and carrageenan, locus bean, arabic, tragacanth; and
combinations thereof. In one embodiment the polymer comprises polyacrylates, especially
sulfonated polyacrylates and water-soluble acrylate copolymers; and alkylhydroxy cellulosics
such as methylcellulose, carboxymethylcellulose sodium, modified carboxy-methylcellulose,
dextrin, ethylcellulose, propylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose,
maltodextrin, polymethacrylates. In yet another embodiment the polymer comprises PVA;
PVA copolymers; hydroxypropyl methyl cellulose (HPMC); and mixtures thereof.
[0077] The first carrier and second carrier can be selected from the group consisting of
polyvinyl alcohol, modified polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl alcohol/polyvinyl
pyrrolidone, polyvinyl alcohol/polyvinyl amine, partially hydrolyzed polyvinyl acetate,
polyalkylene oxide, polyethylene glycol, acrylamide, acrylic acid, cellulose, alkyl
cellulosics, methyl cellulose, ethyl cellulose, propyl cellulose, cellulose ethers,
cellulose esters, cellulose amides, polyvinyl acetates, polycarboxylic acids and salts,
polyaminoacids or peptides, polyamides, polyacrylamide, copolymers of maleic/acrylic
acids, polysaccharides, starch, modified starch, gelatin, alginates, xyloglucans,
hemicellulosic polysaccharides, xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan,
galactoglucomannan, natural gums, pectin, xanthan, carrageenan, locus bean, arabic,
tragacanth, polyacrylates, sulfonated polyacrylates, water-soluble acrylate copolymers,
alkylhydroxy cellulosics, methylcellulose, carboxymethylcellulose sodium, modified
carboxy-methylcellulose, dextrin, ethylcellulose, propylcellulose, hydroxyethyl cellulose,
hydroxypropyl methylcellulose, maltodextrin, polymethacrylates, polyvinyl alcohol
copolymers, hydroxypropyl methyl cellulose, and mixtures thereof.
[0078] The first carrier and second carrier can be an organic material. Organic carriers
may provide a benefit of being readily soluble in water.
[0079] The first particles can comprise from about 30% by weight to about 98% by weight
of the particles of the water soluble first carrier. The second particles can comprise
from about 30% by weight to about 98% by weight of the second particles of the water
soluble second carrier.
The first particles and second particles can comprise from about 45% by weight to
about 99% by weight of the respective particles of a water soluble carrier, understood
to be the water soluble first carrier and the water soluble second carrier. The first
particles and second particles can comprise from about 45% by weight to about 92%
by weight of the respective particles of a water soluble carrier, understood to be
the water soluble first carrier and the water soluble second carrier. The first particles
and second particles can comprise from about 40% by weight to about 99% by weight
of the respective particles of a water soluble carrier, understood to be the water
soluble first carrier and the water soluble second carrier. .
[0080] The water soluble first carrier and water soluble second carrier can be polyethylene
glycol (PEG). PEG can be a convenient material to employ to make particles because
it can be sufficiently water soluble to dissolve during a wash cycle when the first
particles and second particles are within the aforesaid range of mass. Further, PEG
can be easily processed as melt. The onset of melt temperature of PEG can vary as
a function of molecular weight of the PEG. The first particles and second particles
can comprise more than about 40% by weight PEG having a weight average molecular weight
from about 2000 to about 13000. PEG has a relatively low cost, may be formed into
many different shapes and sizes, minimizes unencapsulated perfume diffusion, and dissolves
well in water. PEG comes in various weight average molecular weights. A suitable weight
average molecular weight range of PEG includes from about 2,000 to about 13,000, from
about 4,000 to about 12,000, alternatively from about 5,000 to about 11,000, alternatively
from about 6,000 to about 10,000, alternatively from about 7,000 to about 9,000, alternatively
combinations thereof. PEG is available from BASF, for example PLURIOL E 8000, or PLURIOL
E 9000, or other PLURIOL product.
[0081] The first particles and second particles can comprise more than about 40% by weight
of the particles of PEG. The first particles and second particles can comprise more
than about 50% by weight of the particles of PEG. The first particles and second particles
can comprise more than about 60% by weight of the particles of PEG. The first particles
and second particles may comprise from about 40% to about 99% by weight of the composition
of PEG. The first particles and second particles may comprise from about 65% to about
99% by weight of the composition of PEG. The first particles and second particles
may comprise from about 40% to about 99% by weight of the composition of PEG. The
first particles and second particles may comprise from about 45% to about 99% by weight
of the composition of PEG.
[0082] Alternatively, the first particles and second particles can comprise from about 40%
to about 90%, alternatively from about 45% to about 75%, alternatively from about
50% to about 70%, alternatively combinations thereof and any whole percentages or
ranges of whole percentages within any of the aforementioned ranges, of PEG by weight
of the respective particles.
[0083] The plurality of first particles and second particles can be substantially free from
particles having a mass less than 10 mg. This can be practical for limiting the ability
of the first particles and or second particles to become airborne.
[0084] Depending on the application, the first particles and second particles can comprise
from about 0.5% to about 5% by weight of the respective particles of a balancing agent
selected from the group consisting of glycerin, polypropylene glycol, isopropyl myristate,
dipropylene glycol, 1,2-propanediol, and PEG having a weight average molecular weight
less than 2,000, and mixtures thereof. The balancing agent can be practical for providing
particles having the same processing characteristics even though the particles have
different formulations. For instance, two different scent variants of a product may
have different levels of perfume. With use of a balancing agent, the PEG level can
be the same in each scent variant and the formulas can be balanced with the balancing
agent. This can make processing simpler in that the formulas for the scent variants
will have the same level of PEG and may have similar processing characteristics.
[0085] The first particles and second particles can comprise an antioxidant. The antioxidant
can help to promote stability of the color and or odor of the respective particles
over time between production and use. The first particles and or second particles
can comprise between about 0.01% to about 1% by weight antioxidant. The first particles
and or second particles can comprise between about 0.001% to about 2% by weight antioxidant.
The first particles and or second particles can comprise between about 0.01% to about
0.1% by weight antioxidant. The antioxidant can be butylated hydroxytoluene.
[0086] The first carrier and the second carrier can comprise a water soluble polymer. Water
soluble polymers can be relatively easily processed with other formulation components
that make up the first particles and second particles.
[0087] The first carrier and second carrier can be the same water soluble polymer or different
water soluble polymers. For first particles and second particles processed as a melt,
it can be convenient to have the first carrier and the second carrier be the same
material. This can be a convenient enabler for manufacturing the first particles and
the second particles on the same or similar manufacturing equipment using the same
or similar processing settings, such as temperature, line speed, liquid controls,
and the like.
[0088] Further, if the same or similar materials are used as the water soluble first carrier
and the water soluble second carrier, the dissolution behavior of the carriers in
the wash can be consistent amongst the first particles and second particles. For instance,
if the first particles comprise a water soluble first carrier that is PEG having a
particular distribution of molecular weights and the second particles comprise a water
soluble second carrier that is the same as the water soluble first carrier, the dissolution
behavior of the first particles and the second particles in the wash are expected
to be similar. If the first particles and the second particles are similarly sized
to one another, then the first particles and second particles are expected to dissolve
in the wash within similar amounts of time.
[0089] The water soluble first carrier and water soluble second carrier can comprise a monomer
present in both the first carrier and the second carrier. For instance, the first
carrier and the second carrier can comprise the same monomer, but the carriers may
have different molecular weight distributions. Different molecular weight distributions
can be used to control the amount of time it takes for the particles to dissolve in
the wash. Different molecular weight distributions may also be used to obtain advantages
or avoid difficulties during manufacturing.
[0090] The onset of melt of the first particles and the second particles can differ by less
than 40 °C. This difference being so small can be practical for manufacturing in that
it might be possible to manufacture the first particles and the second particles on
the same manufacturing equipment with little or no modification required in the equipment
setup being required as part of the change over process. Similarly, if the first particles
and second particles are manufactured on separate equipment, the process settings
can be the same or similar for both pieces of equipment. Furthermore, expertise that
is gained on manufacturing the first particles may be applied to manufacturing the
second particles, and vice versa. The onset of melt of the first particles and the
second particles can differ by less than 20 °C.
[0091] The water soluble first carrier and water soluble second carrier can disperse completely
in 25 °C water within a Dispersion Time of less than 60 minutes. The water soluble
first carrier and water soluble second carrier can disperse completely in 25 °C water
within a Dispersion Time of less than 20 minutes. The water soluble first carrier
and water soluble second carrier can disperse completely in 25 °C water within a Dispersion
Time of less than 10 minutes. The water soluble first carrier and water soluble second
carrier can disperse completely in 25 °C water within a Dispersion Time of less than
4 minutes. The water soluble first carrier and water soluble second carrier can disperse
completely in 25 °C water within a Dispersion Time of less than 2 minutes. The water
soluble first carrier and water soluble second carrier can disperse completely in
25 °C water within a Dispersion Time of less than 1 minute. The Dispersion Time is
determined according to the DISPERSION TEST METHOD described herein. For shorter wash
cycles, particles having a shorter Dispersion Time may preferable.
[0092] The first particles and second particles can have different Dispersion Times. For
instance, the first particles can have a Dispersion Time that is shorter or longer
than the Dispersion Time of the second particles. It can be practical to have the
first particles have a shorter Dispersion Time than the second particles. This can
provide early room bloom of perfume as the first particles disperse in the wash and
then significant release of silicone from the second particles to be deposited on
the fabric. If for certain wash conditions, cycles, silicone, and perfumes it is desirable
for the silicone to be released before the perfume, then the second particles can
have a shorter Dispersion Time than the first particles.
DYE
[0093] The first particles and or second particles may comprise dye. The dye may include
those dyes that are typically used in laundry detergent or fabric softeners. The fabric
treatment composition may comprise less than 0.1%, alternatively about 0.001% to about
0.1%, alternatively about 0.01% to about 0.02%, alternatively combinations thereof
and any hundredths of percent or ranges of hundredths of percent within any of the
aforementioned ranges, of dye by weight of the particles of fabric treatment composition.
Examples of suitable dyes include, but are not limited to, LIQUITINT PINK AM, AQUA
AS CYAN 15, and VIOLET FL, available from Milliken Chemical. Employing a dye can be
practical to help the user differentiate between particles having differing scents
and the first particles and second particles, by using different colored dyes for
the respective particles, if desired.
PERFUME
[0094] In addition to the first carrier, the first particles can further comprise 0.1% to
about 20% by weight perfume. The perfume can be unencapsulated perfume, encapsulated
perfume, perfume provided by a perfume delivery technology, or a perfume provided
in some other manner. Perfumes are generally described in
U.S. Patent 7,186,680 at column 10, line 56, to column 25, line 22. The particles can comprise unencapsulated
perfume and are essentially free of perfume carriers, such as a perfume encapsulate.
The particles can comprise perfume carrier materials (and perfume contained therein).
Examples of perfume carrier materials are described in
U.S. Patent 7,186,680, column 25, line 23, to column 31, line 7. Specific examples of perfume carrier materials
may include cyclodextrin and zeolites.
[0095] The particles can comprise about 0.1% to about 20%, alternatively about 1% to about
15%, alternatively about 2% to about 10%, alternatively combinations thereof and any
whole percentages within any of the aforementioned ranges, of perfume by weight of
the first particles. The first particles can comprise from about 0.1% by weight to
about 6% by weight of the first particles of perfume. The perfume can be unencapsulated
perfume and or encapsulated perfume.
[0096] The first particles can be free or substantially free of a perfume carrier. The first
particles may comprise about 0.1% to about 20%, alternatively about 1% to about 15%,
alternatively 2% to about 10%, alternatively combinations thereof and any whole percentages
within any of the aforementioned ranges, of unencapsulated perfume by weight of the
first particles.
[0097] The first particles can comprise unencapsulated perfume and encapsulated perfume.
The first particles may comprise about 0.1% to about 20%, alternatively about 1% to
about 15%, alternatively from about 2% to about 10%, alternatively combinations thereof
and any whole percentages or ranges of whole percentages within any of the aforementioned
ranges, of the unencapsulated perfume by weight of the first particles. Such levels
of unencapsulated perfume can be appropriate for any of the first particles disclosed
herein that have unencapsulated perfume.
[0098] The first particles can comprise unencapsulated perfume and encapsulated perfume
but be free or essentially free of other perfume carriers. The first particles can
comprise unencapsulated perfume and encapsulated perfume and be free of other perfume
carriers.
[0099] The first particles can comprise encapsulated perfume. Encapsulated perfume can be
perfume oil enclosed within a shell wall. The shell wall can have an average shell
thickness less than the maximum dimension of the perfume core. The encapsulated perfume
can be a friable perfume encapsulate. A friable perfume encapsulate is a encapsulated
perfume in which the shell has low water solubility or is not water soluble. The perfume
encapsulate can be a moisture activated perfume encapsulate. The perfume encapsulate
can comprise a melamine/formaldehyde shell. Perfume encapsulates may be obtained from
Encapsys, or International Flavor & Fragrances, or other suitable source. The perfume
encapsulate shell can be coated with polymer to enhance the ability of the perfume
encapsulate to adhere to fabric. This can be desirable if the first particles are
designed to be a fabric treatment composition. The perfume encapsulate can be those
described in
U.S. Patent Publication 2008/0305982.
[0100] The first particles can comprise about 0.1% to about 20%, alternatively about 0.1%
to about 10%, alternatively about 1% to about 15%, alternatively 2% to about 10%,
alternatively combinations thereof and any whole percentages within any of the aforementioned
ranges, of encapsulated perfume by weight of the first particles.
[0101] The first particles can comprise perfume encapsulate but be free of or essentially
free of unencapsulated perfume. The first particles may comprise about 0.1% to about
20%, alternatively about 1% to about 15%, alternatively about 2% to about 10%, alternatively
combinations thereof and any whole percentages within any of the aforementioned ranges,
of encapsulated perfume by weight of the first particles.
METHOD OF MAKING PARTICLES
[0102] An apparatus 100 for forming first and second particles is shown in Fig. 3. The raw
material or raw materials are provided to a mixer. The mixer has sufficient capacity
to retain the volume of raw materials provided thereto for a sufficient residence
time to permit the desired level of mixing and or reaction of the raw materials. The
material leaving the mixer is the precursor material 50. The precursor material 50
can be a molten product. The mixer can be a dynamic mixer. A dynamic mixer is a mixer
to which energy is applied to mix the contents in the mixer. The mixer can comprise
one or more impellers to mix the contents in the mixer.
[0103] Between the mixer and the distributor, the precursor material 50 can be transported
through the feed pipe. The feed pipe can be in fluid communication with the mixer.
An intermediate mixer can be provided in fluid communication with the feed pipe between
the mixer and the distributor. The intermediate mixer can be a static mixer in fluid
communication with the feed pipe between the mixer and the distributor. The intermediate
mixer, which can be a static mixer, can be downstream of the mixer. Stated otherwise,
the mixer can be upstream of the intermediate mixer or static mixer if employed. The
intermediate mixer can be a static mixer. The intermediate mixer can be a rotor-stator
mixer. The intermediate mixer can be a colloid mill. The intermediate mixer can be
a driven in-line fluid disperser. The intermediate mixer can be an Ultra Turrax disperser,
Dispax-reactor disperser, Colloid Mil MK, or Cone Mill MKO, available from IKA, Wilmington,
North Carolina, United States of America. The intermediate mixer can be a perforated
disc mill, toothed colloid mill, or DIL Inline Homogenizer, available from FrymaKoruma,
Rheinfelden, Switzerland.
[0104] The distributor can be provided with a plurality of apertures 10. The precursor material
50 can be passed through the apertures 10. After passing through the apertures 10,
the precursor material 50 can be deposited on a moving conveyor 20 that is provided
beneath the distributor 40. The conveyor 20 can be moveable in translation relative
to the distributor 30.
[0105] The precursor material 50 can be cooled on the moving conveyor 20 to form a plurality
of solid particles 30. The cooling can be provided by ambient cooling. Optionally
the cooling can be provided by spraying the under-side of the conveyor 20 with ambient
temperature water or chilled water.
[0106] Once the particles 30 (first or second) are sufficiently coherent, the particles
30 (first or second) can be transferred from the conveyor 20 to processing equipment
downstream of the conveyor 20 for further processing and or packaging.
[0107] First and second particles comprising a carrier that is a water soluble polymer can
be made, by way of non-limiting example, by forming particles from a melt of the composition
that ultimately forms the particles. The rotoforming process can be practical to make
first and second particles comprising polyethylene glycol as the carrier material.
Other process for forming first and second particles can be suitable as well.
[0108] The process for forming first and second particles can comprise the step of providing
a precursor material. The precursor material can be a melt of the composition that
ultimately forms the first or second particles. The precursor material can be passed
through apertures in a distributor that is provided. The distributor can have a plurality
of apertures. A moving conveyor can be provided beneath the distributor. The precursor
material can be deposited on the moving conveyor. The deposited precursor material
can be cooled to form the plurality of first or second particles. The cooling can
be ambient cooling or cooling in which heat is removed from the deposited precursor
material to form the plurality of first or second particles.
[0109] It can be desirable to provide the precursor material at as low a temperature as
possible that permits suitable first and second particles to be formed. The precursor
material can be provided at a temperature less than 70 °C. The precursor material
can be provided at a temperature between the onset of melt of the precursor material
and about 70 °C.
[0110] Rotoforming can be a practical process for forming first and second particles from
a melt. One suitable rotoforming device is a Sandvik ROTOFORM 3000 having a 750 mm
wide 10 m long belt. The distributor of a rotoforming device is a rotating cylinder.
The cylinder can have 2 mm diameter apertures set at a 10 mm pitch in the cross machine
direction and 9.35 mm pitch in the machine direction. The cylinder can be set at approximately
3 mm above the belt. The belt speed and rotational speed of the cylinder can be set
at about 10 m/min.
[0111] The precursor material can be provided from a mixer. The precursor material can be
pumped from the mixer through a plate and frame heat exchanger set to control the
outlet temperature.
[0112] The precursor material can be prepared in a batch or continuous mixer. Molten carrier
material can be provided and the other constituents of the particle can be mixed with
the molten carrier.
[0113] First and second particles can also be made using other approaches. For instance,
granulation or press agglomeration can be appropriate. In granulation, the precursor
material is compacted and homogenized by rotating mixing tools and granulated to form
first and second particles. For precursor materials that are substantially free of
water, a wide variety of sizes of first and second particles can be made.
[0114] In press agglomeration, the precursor material is compacted and plasticized under
pressure and under the effect of shear forces, homogenized and then discharged from
the press agglomeration machine via a forming/shaping process. Press agglomeration
techniques include extrusion, roller compacting, pelleting, and tableting.
[0115] The precursor material can be delivered to a planetary roll extruder or twin screw
extruder having co-rotating or contra-rotating screws. The barrel and the extrusion
granulation head can be heated to the desired extrusion temperature. The precursor
material can be compacted under pressure, plasticized, extruded in the form of strands
through a multiple-bore extrusion die in the extruder head, and sized using a cutting
blade. The bore diameter of the extrusion header can be selected to provide for appropriately
sized first and second particles. The extruded first and second particles can be shaped
using a spheronizer to provide for particles that have a spherical shape.
[0116] Optionally, the extrusion and compression steps may be carried out in a low-pressure
extruder, such as a flat die pelleting press, for example as available from Amandus
Kahl, Reinbek, Germany. Optionally, the extrusion and compression steps may be carried
out in a low pressure extruder, such as a BEXTRUDER, available from Hosokawa Alpine
Aktiengesellschaft, Augsburg, Germany.
[0117] The first and second particles can be made using roller compacting. In roller compacting
the precursor material is introduced between two rollers and rolled under pressure
between the two rollers to form a sheet of compactate. The rollers provide a high
linear pressure on the precursor material. The rollers can be heated or cooled as
desired, depending on the processing characteristics of the precursor material. The
sheet of compactate is broken up into small pieces by cutting. The small pieces can
be further shaped, for example by using a spheronizer.
MEAN PARTICLE SIZE TEST METHOD
[0118] The mean particle size of the silicone in the composition of the present invention
is determined as follows.
[0119] A Horiba Laser Scattering Particle Size and Distribution Analyzer, model LA-930 (Horiba
Instruments, Inc., Irvine, CA, USA) with accompanying software (LA-930 Software, Version
3.73) is used to measure the volume-weighted diameter of silicone particles resulting
from the dissolution of the test composition (i.e. composition) in water. A cuvette-type,
static quartz fraction cell (10 mL capacity) is used for all measurements. The fraction
cell is placed in a Horiba fraction cell holder model LY-203 (available from Horiba
Instruments, Inc., Irvine, CA, USA).
[0120] Within the instrument software, the selected graph conditions are: Density Distribution
Graph is Standard; Axis Selection is Log X- Lin Y; Cumulative Distribution Graph is
On; Size Class is Passing (Undersize); and Axis Type is Bar. Within the instrument
software, the selected display conditions include: Form of Distribution is Standard;
and Distribution Base is Volume. The Relative Refractive Index (RRI) value to be selected
in the software is determined by the identity of the predominant silicone present
(on a wt% basis) in the composition being tested. The RRI code selected is 106a/000i
for silicone material e.g., polydimethylsiloxane or Magnasoft Plus (available from
Momentive Performance Materials Inc., Waterford, NY, USA).
[0121] Prior to collecting measurements, the initial alignment for the instrument is set
for Coarse alignment of the laser beam, and then the alignment is set for Fine alignment
with filtered distilled (DI) water loaded in the background reference fraction cell.
The filtered DI water background sample is then subtracted by selecting "blank" in
the software. Neither the test composition sample, nor the DI water background sample
is stirred during the blanking or measurement processes.
[0122] Compositions are prepared for testing by being dissolved in filtered distilled (DI)
water. Initially, a dispersion with a final concentration of 0.08% (wt/wt) of the
test composition in water is prepared and assessed. This initial sample dispersion
is prepared by adding 0.08 g of the test composition into 100 g of the filtered DI
water at 23°C ± 2°C contained within a flat-bottom glass jar of approximately 200
mL volume. The mixture is then stirred at a rate of approximately 200 rpm until dissolution
of the sample is deemed to be complete, as determined when visual inspection reveals
that no solid material remains, or when no further dissolution is observable over
a time span of 15 minutes. This preparation results in a sample dispersion of water-immiscible
particles in filtered DI water, and is the initial sample dispersion to be assessed
in the instrument.
[0123] A 10 mL aliquot of the sample dispersion is used to rinse the fraction cell of the
instrument, and another 10 mL aliquot of the dispersion is loaded into the fraction
cell for testing. The initial sample dispersion created is tested in accordance with
the instructions and instrument parameters provided above, in order to assess the
Laser T% and Lamp T% values reported by the instrument for that sample concentration.
These T% values are used to determine if the concentration of the test composition
in the initial sample dispersion is suitable for conducting particle size measurements.
The goal is to create a sample dispersion whose concentration produces values for
both the Laser T% and Lamp T% parameters which fall within the range of 70% to 95%,
as this indicates that the dispersion is of a suitable concentration to measure particle
diameter. Frequently, the T% values will fall within the suitable range when the total
final concentration of the particle-forming material(s) in the dispersion is in range
of 0.01% to 0.1% (wt/wt). The T% values reported by the instrument are used to adjust
the concentration of the test composition in the dispersion, such that a concentration
is identified which is suitable for conducting particle size measurements. This is
achieved by creating new test dispersions made at final concentrations either higher
or lower than 0.08% accordingly, as needed in order to achieve T% values within the
required range. Once a suitable concentration for the dispersion has been determined,
new preparations at that concentration are created according to the mixing conditions
specified above, for the purpose of conducting the silicone particle diameter measurements
in accordance with the instructions and instrument parameters specified.
[0124] Each composition being tested is prepared and measured in at least three replicate
dispersions at a suitable concentration. Each replicate sample is weighed and dissolved
separately, and each replicate dispersion is measured after performing a rinse step
with that preparation. Since a prepared dispersion may not be stable, all testing
of samples from a dispersion is conducted within the 15 min time period immediately
after the dissolution is deemed complete and the stirring has ceased. From each of
the three dispersions, two 10 mL aliquots are measured. Each aliquot is measured repeatedly
via three analysis runs, such that particle size data is generated three times for
each aliquot. This results in six particle size analysis runs for each of the three
replicate dispersions. After each particle size measurement analysis run, the instrument
software displays a volume-weighted plot of Frequency (%) versus Diameter (µm) as
well as the value of the mean volume-weighted particle diameter. The mean volume-weighted
particle diameter values measured from all analysis runs of all replicate dispersions,
are recorded and averaged, to yield the mean volume-weighted particle size diameter
reported as the mean particle size of the silicone of the test composition.
DISPERSION TEST METHOD
[0125] The rate of dispersion of the carrier portion of the particles (first particles or
second particles) of the consumer product composition is determined according to the
following test method.
[0126] A magnetic stir bar and 200 mL of deionized water (DI water) are placed into a 250
mL capacity glass beaker located on top of a stir plate set at a stir speed of 150
rpm. The temperature of the DI water is maintained between 23 °C and 25 °C. A single
sample of the particles (first particles or second particles) of the composition (e.g.
a single particle) is added into the beaker of stirred DI water, and a timer is started
immediately at the same time. The sample (e.g. particle) is then observed visually
by eye under well-lit laboratory conditions without the aid of laboratory magnification
devices, to monitor and assess the appearance and size of the sample (e.g. particle)
with regard to its dispersion and disintegration. This visual assessment may require
the use of a flash light or other bright light source to ensure accurate observations.
[0127] The visual assessment is conducted every 10 seconds over the 60 minute time period
after the addition of the sample to the water. If the dispersion of the sample results
in the sample becoming visually undetectable as a discrete object(s), then the time
point at which this first occurs is noted. If the dispersion of the sample results
in a stable visual appearance after which no additional dispersion or disintegration
is observed, then the time point at which this stable appearance first occurs is noted.
A value of 60 min is assigned if the sample is still visible at the 60 minutes time
point and it appeared to still be undergoing dispersion or disintegration immediately
prior to the 60 min time point. For each material being tested, the assessment is
repeated ten times to result in ten replicate measurements. The time values noted
for the ten replicates are averaged, and this average value is reported as the Dispersion
Time value determined for that test material.
ONSET OF MELT TEST METHOD
[0128] Onset of melt is determined using the onset of melt test method as follows.
Differential Scanning Calorimetry (DSC) is used to quantify the temperature at which
the onset of melt occurs for the peak melt transition of any given composition of
particles to be tested. The melt temperature measurements are made using a high quality
DSC instrument with accompanying software and nitrogen purge capability, such as TA
Instruments' model Discovery DSC (TA Instruments Inc. / Waters Corporation, New Castle,
Delaware, U.S.A.). A calibration check is conducted using an Indium standard sample.
The DSC instrument is considered suitable to conduct the test if the onset of melt
temperature measured for the Indium standard sample is within the range of 156.3 -
157.3 °C.
[0129] A plurality of particles of the test composition are examined in order to identify
individual particles which comprise a first class of particle versus those which comprise
a second class of particle, and those that comprise any additional number of classes
which may be present. The process of examining a plurality of particles to achieve
such class identifications may include many approaches, including the examination
and comparison of individual particles by visual inspection, examination and comparison
of individual particles based on chemical makeup, and by chemical testing to determine
the presence or absence of silicone or perfumes in the interior of individual particles.
Test compositions are to be tested on a per class basis (i.e., by physically separating
individual particles according to their class, thus creating internally uniform samples
wherein each sample comprises a single class of particle). These samples are used
to test particles from each class separately from particles of other classes. The
results measured for each class of particle are reported separately (i.e. on a per
class basis).
[0130] For each class of particle present in the test composition, a uniform test sample
is prepared by obtaining at least 5g of particles of that class, which are then pulverised
via milling into powder form using an analytical milling device, such as the IKA basic
analytical mill model A11 B S1 (IKA-Werke GmbH & Co. KG, Staufen im Breisgau, Germany).
The milled sample is subsequently sieved through a clean stainless steel sieve with
sieve mesh size openings of nominally 1mm in diameter (e.g. number 18 mesh size).
For each sample to be tested, at least two replicate samples are independently milled
and measured. A sample of the milled material weighing approximately 5 mg is placed
into the bottom of a hermetic aluminium DSC sample pan, and the sample is spread out
to cover the base of the pan. A hermetic aluminium lid is placed on the sample pan,
and the lid is sealed with a sample encapsulating press to prevent evaporation or
weight loss during the measurement process. The DSC measurements are conducted relative
to a reference standard. An empty aluminium DSC sample pan used as the reference standard,
in order to measure the delta in heat adsorption of the sample-containing pan versus
the empty reference pan.
[0131] The DSC instrument is set up to analyze samples using the following cycle configuration
selections: Sample Purge Gas is nitrogen set at 50 mL/min; Sampling Interval is set
at 0.1 s/point; Equilibrate is set at -20.00 °C; Isothermal Hold is set at 1 min.
Data is collected during a single heating cycle using the settings: Ramp is set at
10.00 °C/min to 90.00 °C; and Isothermal Hold is set at 90.00 °C for 1 min. A sealed
sample pan containing a replicate test sample is carefully loaded into the instrument,
as is an empty reference pan. The DSC analysis cycle specified above is conducted
and the output data is assessed. The data acquired during the DSC heating cycle is
typically plotted with Temperature on the X-axis (in °C) and Heat Flow normalized
to sample weight (in W/g) on the Y-axis, such that melting points appear as downward
(endothermic) peaks since they absorb energy.
[0132] A melt transition onset temperature is the temperature at which a deflection is first
observed from the baseline previously established for the melt temperature of interest.
The Peak Melt temperature is the specific temperature that requires the largest observed
differential energy to transition the sample from a solid phase to a melt phase, during
the specified DSC heating cycle. For the purpose of this invention, the Onset of Melt
temperature is defined as the melt transition onset temperature for the Peak Melt
temperature. Additional general information on the DSC technique may be found in the
industry standard method ASTM D3418-03 - Transition Temperatures of Polymers by DSC.
[0133] Using the DSC instrument software, two points are manually defined as the "Start
and Stop Integration" baseline limits. The two points selected are on flat regions
of the baseline to the left and right sides, respectively, of the melt transition
peak detected. This defined area is then used to determine the peak temperature (T)
which can be used to report the Peak Melt Temperature. The Onset of Melt temperature
for the Peak Melt temperature is then identified by the instrument software.
[0134] For each class of particle in a test composition, the Onset of Melt temperature reported
is the average result (in °C) from the replicate samples of that class of particle.
EXAMPLES/COMBINATIONS
[0135] The following are nonlimiting examples of compositions that can be formulated to
deliver a scent and fabric softness benefit through the wash. In the following examples,
the amounts of the formulation components within the particles are percent by weight
with respect to the particular particle (first particle or second particle). The weight
fraction of the composition that combines first particles and second particles is
percent by weight of the composition.
| |
Example A |
Example B |
Example C |
| |
First Particles |
Second Particles |
First Particles |
Second Particles |
First Particles |
Second Particles |
| PLURIOL 9000A |
87.3 |
68 |
90 |
75 |
90 |
70 |
| SiliconeB |
- |
32 |
- |
25 |
- |
30 |
| Encapsulated PerfumeC |
1.1 |
- |
0.8 |
- |
2 |
- |
| Unencapsulated Perfume |
7.5 |
- |
4.8 |
- |
6.0 |
- |
| DyeD |
0.012 |
- |
0.012 |
- |
0.012 |
- |
| Dipropylene Glycol |
1.1 |
- |
1.1 |
- |
1.1 |
- |
| Minors |
Remainder for the above to total 100% |
- |
Remainder for the above to total 100% |
- |
Remainder for the above to total 100% |
- |
| Weight Fraction of Composition |
65 |
35 |
50 |
50 |
35 |
65 |
A. Available from BASF
B. Dow Corning(R) XX-8766 Amino Polymer
C. Encapsulated perfume available from Encapsys
D. LIQUITINT BLUE BL available from Millikin Chemical |
[0136] Further examples and combinations can be as follows:
- A. A composition comprising:
- (i) a plurality of first particles comprising:
about 30% to about 98% by weight of said first particles a water soluble first carrier,
wherein said first particles have a first particles onset of melt from about 25 °C
to about 120 °C; and
perfume carried by said first carrier; and
- (ii) a plurality of second particles comprising:
about 30% to about 98% by weight of said second particles a water soluble second carrier,
wherein said second particles have a second particles onset of melt from about 25
°C to about 120 °C; and
silicone carried by said second carrier;
wherein said first particles and said second particles are in a package.
- B. The composition according to Paragraph A, wherein said first carrier and said second
carrier comprise a water soluble polymer.
- C. The composition according to Paragraph A or B, wherein said first particles onset
of melt and said second particles onset of melt differ by less than 40 °C.
- D. The composition according to any one of Paragraphs A to C, wherein said first carrier
and said second carrier comprise a monomer present in both said first carrier and
said second carrier.
- E. The composition according to any one of Paragraphs A to D, wherein said first carrier
and second carrier are selected from the group consisting of polyvinyl alcohol, modified
polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl alcohol/polyvinyl pyrrolidone,
polyvinyl alcohol/polyvinyl amine, partially hydrolyzed polyvinyl acetate, polyalkylene
oxide, polyethylene glycol, acrylamide, acrylic acid, cellulose, alkyl cellulosics,
methyl cellulose, ethyl cellulose, propyl cellulose, cellulose ethers, cellulose esters,
cellulose amides, polyvinyl acetates, polycarboxylic acids and salts, polyaminoacids
or peptides, polyamides, polyacrylamide, copolymers of maleic/acrylic acids, polysaccharides,
starch, modified starch, gelatin, alginates, xyloglucans, hemicellulosic polysaccharides,
xylan, glucuronoxylan, arabinoxylan, mannan, glucomannan, galactoglucomannan, natural
gums, pectin, xanthan, carrageenan, locus bean, arabic, tragacanth, polyacrylates,
sulfonated polyacrylates, water-soluble acrylate copolymers, alkylhydroxy cellulosics,
methylcellulose, carboxymethylcellulose sodium, modified carboxy-methylcellulose,
dextrin, ethylcellulose, propylcellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose,
maltodextrin, polymethacrylates, polyvinyl alcohol copolymers, hydroxypropyl methyl
cellulose, and mixtures thereof.
- F. The composition according to any one of Paragraphs A to E, wherein said perfume
is dispersed in said first carrier.
- G. The composition according to any one of Paragraphs A to F, wherein said silicone
is dispersed in said second carrier.
- H. The composition according to any one of Paragraphs A to G, where said perfume is
encapsulated within a shell wall.
- I. The composition according to any one of Paragraphs A to H, wherein said silicone
is present in said second particles in droplets.
- J. The composition according to any one of Paragraphs A to I, wherein said silicone
is present in said second particles in droplets having a mean particle size of from
about 2 µm to about 2000 µm.
- K. The composition according to any one of Paragraphs A to J, wherein said composition
comprises from about 10% to about 90% by weight said first particles and from about
10% to about 90% by weight said second particles.
- L. The composition according to any one of Paragraphs A to K, wherein said first carrier
and said second carrier are different materials.
- M. The composition according to any one of Paragraphs A to K, where said first carrier
and said second carrier are the same material.
- N. The composition according to any one of Paragraphs A to M, where said first particles
and said second particles mixed together have a coefficient of uniformity of less
than 2.
- O. The composition according to any one of Paragraphs A to N, wherein said first particles
have a first particles D50 and said second particles have a second particles D50,
wherein said second particles D50 is within about 20% of said first particles D50.
- P. The composition according to any one of Paragraphs A to O, wherein said first particles
comprise about 0.1% to about 20% by weight of said first particles of perfume.
- Q. The composition according to any one of Paragraphs A to P, wherein said first particles
comprise more perfume by weight percent than said second particles.
- R. The composition according to any one of Paragraphs A to Q, wherein said composition
comprises less than 5% by weight surfactant.
- S. The composition according to any one of Paragraphs A to R, wherein said first particles
comprise less than 3% by weight of said first particles silicone.
- T. The composition according to any one of Paragraphs A to S, wherein said second
particles comprise from about 3% to about 50% by weight of said second particles silicone.
- U. The composition according to any one of Paragraphs A to T, wherein said first particles
are together in a single chamber of said package.
- V. The composition according to any one of Paragraphs A to U, wherein said composition
comprises about 65% by weight said first particles and about 35% by weight said second
particles.
- W. A process for laundering articles of fabric with the composition of any one of
Paragraphs A to V comprising the steps of:
dispensing into a washing machine said composition according to Paragraph A into a
washing machine; a first composition comprising first particles and second particles,
wherein said first particles comprise a water soluble first carrier and perfume and
said second particles comprise a water soluble second carrier and silicone;
dispensing into said washing machine a detergent composition comprising a surfactant,
wherein said composition and said detergent composition are from different packages;
placing one or more articles of fabric into said washing machine; and
washing said fabric with said composition and said detergent composition.
[0137] The dimensions and values disclosed herein are not to be understood as being strictly
limited to the exact numerical values recited. Instead, unless otherwise specified,
each such dimension is intended to mean both the recited value and a functionally
equivalent range surrounding that value. For example, a dimension disclosed as "40
mm" is intended to mean "about 40 mm."
[0138] Every document cited herein, including any cross referenced or related patent or
application and any patent application or patent to which this application claims
priority or benefit thereof, is hereby incorporated herein by reference in its entirety
unless expressly excluded or otherwise limited. The citation of any document is not
an admission that it is prior art with respect to any invention disclosed or claimed
herein or that it alone, or in any combination with any other reference or references,
teaches, suggests or discloses any such invention. Further, to the extent that any
meaning or definition of a term in this document conflicts with any meaning or definition
of the same term in a document incorporated by reference, the meaning or definition
assigned to that term in this document shall govern.
[0139] While particular embodiments of the present invention have been illustrated and described,
it would be obvious to those skilled in the art that various other changes and modifications
can be made without departing from the spirit and scope of the invention. It is therefore
intended to cover in the appended claims all such changes and modifications that are
within the scope of this invention.