Field of the invention
[0001] The present invention relates to a novel liquid bleaching composition and a method
for treating a textile, especially laundry fabrics, using the same. More in particular,
the invention relates to a liquid bleaching composition having favourable cleaning,
bleaching and foaming characteristics.
Background of the invention
[0002] The use of bleaching catalysts for stain removal has been developed over recent years.
The recent discovery that some catalysts are capable of bleaching effectively in the
absence of an added peroxyl source has recently become the focus of some interest,
as will be clear from e.g. WO-99/65905, WO-00/12667, WO-00/12808, WO-00/29537, and
WO-00/60045.
[0003] The shelf life of a product may be regarded as the period of time over which the
product may be stored whilst retaining its required quality. A satisfactory shelf
life is in many instances a crucial factor for the success of a commercial product.
A product with a short shelf life generally dictates that the product is made in small
batches and is rapidly sold to the customer. It is also a concern to the owners of
a brand with a short shelf life that the consumer uses the product within the shelf
life; otherwise the consumer may be inclined to change to a similar product of another
brand. In contrast, a similar product with a long shelf life may be made in larger
batches, held as stock for a longer period of time and the period of time that a consumer
stores the product is not of a great concern to the owners of the particular brand
concerned. Despite the shelf life being an important consideration, the product must
also be active during use.
[0004] It is an object of the present invention to provide a liquid bleaching composition
that has favourable storage properties whilst being active in use.
It is another object of the invention to provide a liquid bleaching composition that
shows good bleaching and cleaning performance, and additionally has moderate foaming
characteristics when in use.
It is a further object of the invention to provide a liquid bleaching composition
that is chemically and physically stable when in storage.
We have now surprisingly found that one or more of these objects can be achieved when
using an aqueous liquid bleaching composition according to the present invention.
Summary of the invention
[0005] Accordingly, in one aspect the present invention provides an aqueous liquid bleaching
composition having a pH-value of less than or equal to 7, and comprising surfactant
material, a bleach catalyst and an antifoam system containing fatty acid having an
iodine value lower than 1.0 and a neutralising agent selected from the group consisting
of a substituted amine with a C1 or C2 substitution and tetraalkyl ammoniumhydroxide
having a C1-C4 alkyl group.
Furthermore, in a second aspect the invention provides a method of bleaching a textile,
comprising the steps of:
(i) diluting from 0.5 to 20 g of a liquid bleaching composition according to the present
invention with 1 litre of water;
(ii) treating the textile with the diluted composition;
(iii) rinsing the textile with water; and
(iv) drying the textile.
[0006] The iodine value according to the present invention is a measure for the level of
saturation of the fatty acid: the lower the iodine value of the fatty acid, the higher
is the degree of saturation. In connection with the present invention, the iodine
value of a fatty acid is defined as the weight of halogens expressed as iodine absorbed
by 100 parts by weight of the fatty acid. It follows that a lower iodine value will
be measured if the level of saturation of the fatty acid is higher.
The iodine value is determined by the Wijs' method described by IFFO (ISO 3961:1996,
May 1998) in which the test sample is dissolved in a solvent and Wijs' reagent added.
After about one hour reaction time, potassium iodide and water are added to the mixture.
Iodine liberated by the process is titrated with sodium thiosulphate solution.
Detailed description of the invention.
[0007] It has been found that the aqueous liquid bleaching composition of the invention
shows both good cleaning and favourable bleaching performance. In addition, it was
observed that said composition has moderate foaming characteristics when in use. Furthermore,
liquid bleaching compositions according to the invention were found to have favourable
storage properties:
their bleaching and cleaning activities were maintained after prolonged periods of
storage.
Preferably, the aqueous liquid bleaching composition of the invention has a water
content of 40 to 90% by weight, more preferably 45 to 80% by weight.
Furthermore, the liquid composition of the invention is preferably isotropic and transparent.
Reason is that transparent liquid detergent compositions are generally regarded to
have a visually attractive appearance.
pH-value
[0008] The pH-value of the composition of the invention is less than or equal to 7, preferably
in the range of from 6 to 7, more preferably from 6.5 to 7. This range of pH-values
is needed for obtaining a chemically stable composition. More in particular, it was
found that the bleach catalyst can remain stable and does not dissociate when the
liquid composition of the invention is stored at a pH of less than or equal to 7.
Furthermore, when protease enzyme is present in the composition of the invention,
said relatively low pH-value range may also be beneficial for maintaining the activity
of the protease enzyme, depending on the type thereof.
[0009] However, for obtaining favourable bleaching and cleaning performance when the composition
of the invention is used for treating textile, it is preferred that the pH-value of
said composition is raised to the range of from 7.5 to 9 upon dilution with water.
Hence, it is preferred that said composition additionally contains a pH-changing means
capable of bringing about this increase of pH-value. Desirably, the pH-changing means
is capable of raising the pH-value to at least 8 upon dilution with water.
[0010] The pH-changing means is effectively provided by a pH-jump system containing a boron
compound, particularly borax decahydrate, and a polyol. The borate ion and certain
cis 1,2-polyols complex when present in the undiluted composition, so as to cause
a reduction in pH-value to a value of less than or equal to 7. Upon dilution, the
complex dissociates liberating free borate to raise the pH-value in the diluted solution
resulting in a pH-jump. Examples of polyols that exhibit the complexing mechanism
with borax include catechol, galactitol, fructose, sorbitol, and pinacol. For economic
reasons, sorbitol is the preferred polyol.
[0011] The desired ratio of the polyol to the boron compound needs to be considered since
it influences performance.
[0012] To achieve the desired pH-value during storage of less than or equal to 7, ratios
greater than 1:1 are preferred. The level of the boron compound, particularly borax,
incorporated in the composition of the invention also influences the performance.
Borax levels of at least 1% by weight are desired to ensure sufficient buffering.
Excessive amounts of borax (>10% by weight) give good buffering properties; however,
such levels lead to a pH-value of the undiluted composition that is higher than desired.
Generally, pH-jump systems in which the weight ratio of the polyol and boron compound
ranges from 1:1 to 10:1 are preferred for use in the present invention.
[0013] When applying a borax-sorbitol pH-jump system, said system preferably comprises at
least 2% by weight of Sorbitol and at least 1 % by weight of borax.
In practice, compositions containing, as a pH-jump system, a combination of 5% wt
borax and 20% wt sorbitol were found to yield the best results.
Such a pH-jump system is known from EP-A-381,262.
Salts of calcium and magnesium have been found to enhance the pH-jump effect by further
lowering the pH of the undiluted composition. Other di- and trivalent cations may
be used but Ca and Mg are preferred. Any anion may be used providing the resulting
Ca/Mg salt is sufficiently soluble. Chloride, although it could be used, is not preferred
because of oxidation problems.
[0014] Other types of pH-jump systems are based on the principle of insoluble alkaline salts
in the undiluted composition that dissolve on dilution to raise the solution pH. Examples
of such alkaline salts are sodium tripolyphosphate (STP), sodium carbonate, sodium
bicarbonate, sodium silicate, sodium pyro- and ortho-phosphate.
[0015] An alternative type of pH-jump system for use in a liquid detergent composition includes
a metal cation and an N-containing compound, as disclosed in US-A-5,484,555.
The antifoam
[0016] The antifoam system of the present invention contains one or more fatty acids having
an iodine value of lower than 1.0, preferably lower than 0.3, and a neutralising agent
therefor, as further specified below.
As mentioned above, the iodine value is a measure for the level of saturation of the
fatty acid; the lower the iodine value of the fatty acid, the higher is the degree
of saturation.
Preferably, the fatty acid has a degree of saturation of more than 95%, said degree
of saturation being most preferably 100%. Reason is that such saturated fatty acids
have been found to perform favourably for reducing and controlling foaming characteristics,
and to also lead to improved chemical stability of the bleach catalyst present in
the composition of the invention.
Good anti-foaming results were obtained when the fatty acid is a mixture of lauric
acid, myristic acid, palmitic acid, stearic acid, arachidic acid, and behenic acid.
[0017] Preferably, the level of the fatty acid of the invention is at most 8%, more preferably
at most 4% by weight, most preferably at most 2% by weight based on the full liquid
composition of the invention.
[0018] For obtaining favourable solubility of the saturated fatty acid in the liquid composition
of the present invention, a neutralising agent selected from the group consisting
of a substituted amine with a C
1 or C
2 substitution and a tetraalkyl ammonium hydroxide having a C
1-C
4 alkyl group is present in said composition.
[0019] For ensuring that the composition has both good physical stability (as a result of
the favourable solubility of the fatty acid) and good pH-jump characteristics when
a pH-jump system is present, the neutralising agent is preferably a substituted amine
selected from the group consisting of triethanol amine, triethyl amine and dimethyl
ethanolamine.
The bleach catalyst
[0020] The bleach catalyst per se may be selected from a wide range of transition metal
complexes of organic molecules (ligands). In typical washing compositions the level
of the organic substance is such that the in-use level is from 0.05 µM to 50 mM, with
preferred in-use levels for domestic laundry operations falling in the range 1 to
100 µM. Higher levels may be desired and applied in industrial textile bleaching processes.
A mixture of different catalysts may be employed in the bleaching composition.
[0021] Suitable organic molecules (ligands) for forming complexes and complexes thereof
are found, for example in: GB 9906474.3; GB 9907714.1; GB 98309168.7, GB 98309169.5;
GB 9027415.0 and GB 9907713.3; DE 19755493; EP 999050; WO-A-9534628; EP-A-458379;
EP 0909809; United States Patent 4,728,455; WO-A-98/39098; WO-A-98/39406, WO 9748787,
WO 0029537; WO 0052124, and WO0060045 the complexes and organic molecule (ligand)
precursors of which are herein incorporated by reference. An example of a preferred
catalyst is a transition metal complex of MeN4Py ligand (N,N-bis(pyridin- 2-yl-methyl)-1,1-bis(pyridin-2-yl)-1-aminoethane).
[0022] The ligand forms a complex with one or more transition metals, in the latter case
for example as a dinuclear complex. Suitable transition metals include for example:
manganese in oxidation states II-V, iron II-V, copper I-III, cobalt I-III, titanium
II-IV, tungsten IV-VI, vanadium II-V and molybdenum II-VI.
[0023] An example of a preferred catalyst is a monomer ligand or transition metal catalyst
thereof of a ligand having the formula (I):
wherein each R is independently selected from: hydrogen, F, Cl, Br, hydroxyl, C1-C4-alkylO-,
-NH-CO-H, -NH-CO-C1-C4-alkyl, - NH2, -NH-C1-C4-alkyl, and C1-C4-alkyl;
R1 and R2 are independently selected from:
C1-C4-alkyl,
C6-C10-aryl, and,
a group containing a heteroatom capable of coordinating to a transition metal, wherein
at least one of R1 and R2 is the group containing the heteroatom;
R3 and R4 are independently selected from hydrogen, C1-C8 alkyl, C1-C8-alkyl-O-C1-C8-alkyl,
C1-C8-alkyl-O-C6-C10-aryl, C6-C10-aryl, C1-C8-hydroxyalkyl, and -(CH2)nC(O)OR5
wherein R5 is independently selected from: hydrogen, C1-C4-alkyl, n is from 0 to 4,
and mixtures thereof; and,
X is selected from C=O, -[C(R6)2]y- wherein Y is from 0 to 3 each R6 is independently selected from hydrogen, hydroxyl,
C1-C4-alkoxy and C1-C4-alkyl.
[0024] With regard to the above formula (I) it is also particularly preferred that R1 and
R2 may also be independently selected from: C1 to C22-optionally substituted alkyl,
and an optionally substituted tertiary amine of the form -C2-C4-alkyl-NR7R8, in which
R7 and R8 are independently selected from the group consisting of straight chain,
branched or cyclo C1-C12 alkyl, benzyl, the -C2-C4-alkyl- of the -C2-C4-alkyl-NR7R8
may be substituted by 1 to 4 C1-C2-alkyl, or may form part of a C3 to C6 alkyl ring,
and in whichR7 and R8 may together form a saturated ring containing one or more other
heteroatoms.
[0025] Another preferred class of ligands are macropolycyclic rigid ligands of the formula:

wherein m and n are 0 or integers from 1 to 2, p is an integer from 1 to 6, preferably
m and n are both 0 or both 1 (preferably both 1), or m is 0 and n is at least 1; and
p is 1; and A is a nonhydrogen moiety preferably having no aromatic content; more
particularly each A can vary independently and is preferably selected from methyl,
ethyl, propyl, isopropyl, butyl, isobutyl, tert-butyl, C5-C20 alkyl, and one, but
not both, of the A moieties is benzyl, and combinations thereof.
[0026] Preferably, the macropolycyclic ligand is of the formula:

wherein "R
1" is independently selected from H, and linear or branched, substituted or unsubstituted
C1-C20 alkyl, alkylaryl, alkenyl or alkynyl; and all nitrogen atoms in the macropolycyclic
rings are coordinated with the transition metal.
[0027] Of the macropolycyclic ligands 5,12-dimethyl-1,5,8,12-tetraaza-bicyclo[6.6.2]hexadecane
is preferred. This ligand is most preferred as its manganese complex [Mn(Bcyclam)Cl
2] and may be synthesised according to WO9839098.
[0028] The transition metal complex preferably is of the general formula (AI):
[M
aL
kX
n]Y
m
in which:
M represents a metal selected from Mn(II)-(III)-(IV)-(V), Cu (I)-(II)-(III), Fe (II)-(III)-(IV)-(V),
Co(I) - (II) - (III), Ti(II)-(III)-(IV), V(II)-(III)-(IV)-(V), Mo(II)-(III)-(IV)-(V)-(VI)
and W(IV)-(V)-(VI), preferably from Fe(II)-(III)-(IV)-(V);
L represents the ligand, preferably N,N-bis(pyridin-2-yl-methyl)-1,1-bis(pyridin-2-yl)-1-aminoethane,
or its protonated or deprotonated analogue;
X represents a coordinating species selected from any mono, bi or tri charged anions
and any neutral molecules able to coordinate the metal in a mono, bi or tridentate
manner;
Y represents any non-coordinated counter ion;
a represents an integer from 1 to 10;
k represents an integer from 1 to 10;
n represents zero or an integer from 1 to 10;
m represents zero or an integer from 1 to 20.
Surfactant material
[0029] The liquid bleaching composition of the invention also contains surfactant material,
preferably at a concentration of 0.1 to 50% by weight, based on the total composition.
This surfactant system may in turn comprise 0 - 95 % by weight of one or more anionic
surfactants and 5 to 100 % by weight of one or more nonionic surfactants. The surfactant
system may additionally contain amphoteric or zwitterionic detergent compounds. The
liquid bleaching composition according to the invention will generally be used as
a dilution in water of about 0.05 to 2%.
[0030] In general, the nonionic and anionic surfactants of the surfactant system may be
chosen from the surfactants described "Surface Active Agents" Vol. 1, by Schwartz
& Perry, Interscience 1949, Vol. 2 by Schwartz, Perry & Berch, Interscience 1958,
in the current edition of "McCutcheon's Emulsifiers and Detergents" published by Manufacturing
Confectioners Company or in "Tenside-Taschenbuch", H. Stache, 2nd Edn., Carl Hauser
Verlag, 1981.
[0031] Suitable nonionic detergent compounds which may be used include, in particular, the
reaction products of compounds having a hydrophobic group and a reactive hydrogen
atom, for example, aliphatic alcohols, acids, amides or alkyl phenols with alkylene
oxides, especially ethylene oxide either alone or with propylene oxide. Specific nonionic
detergent compounds are C
6-C
22 alkyl phenol-ethylene oxide condensates, generally 5 to 25 EO, i.e. 5 to 25 units
of ethylene oxide per molecule, and the condensation products of aliphatic C
8-C
18 primary or secondary linear or branched alcohols with ethylene oxide, generally 5
to 40 EO.
Also applicable are surfactants such as those described in EP-A-328 177 (Unilever),
which show resistance to salting-out, the alkyl polyglycoside surfactants described
in EP-A-070 074, and alkyl monoglycosides.
[0032] Suitable anionic detergent compounds which may be used are usually water-soluble
alkali metal salts of organic sulphates and sulphonates having alkyl radicals containing
from about 8 to about 22 carbon atoms, the term alkyl being used to include the alkyl
portion of higher acyl radicals. Examples of suitable synthetic anionic detergent
compounds are sodium and potassium alkyl sulphates, especially those obtained by sulphating
higher C
8-C
18 alcohols, produced for example from tallow or coconut oil, sodium and potassium alkyl
C
9-C
20 benzene sulphonates, particularly sodium linear secondary alkyl C
10-C
15 benzene sulphonates; and sodium alkyl glyceryl ether sulphates, especially those
ethers of the higher alcohols derived from tallow or coconut oil and synthetic alcohols
derived from petroleum. The preferred anionic detergent compounds are sodium C
11-C
15 alkyl benzene sulphonates, sodium C
12-C
18 alkyl sulphates and sodium linear alcohol ethoxy sulphates.
[0033] Preferred surfactant systems are mixtures of anionic with nonionic detergent active
materials, in particular the groups and examples of anionic and nonionic surfactants
pointed out in EP-A-346 995 (Unilever). Especially preferred is a surfactant system
that is a mixture of a sodium C
11-C
15 alkyl benzene sulphonate, a C
12-C
15 primary alcohol 3-9 EO ethoxylate and a sodium linear alcohol ethoxy sulphate.
[0034] The nonionic detergent is preferably present in amounts greater than 10%, e.g. 25-90%
by weight of the surfactant system. Anionic surfactants can be present for example
in amounts in the range from about 5% to about 40% by weight of the surfactant system.
Other components
[0035] The liquid bleaching composition of the invention may additionally comprise builders,
solvents, enzymes, perfumes, sequestrants, polymers, fluorescers and dyes.
The use and amount of these components are such that the bleaching and cleaning performance
of the composition is favourable depending on economic and environmental factors.
[0036] One skilled in the art will appreciate that some adventitious peroxyl species may
be in the composition nevertheless it is most preferred that the bleaching composition
of the present invention has less that 1%, preferably less than 0.1%, most preferably
less than 0.01%, of a peroxyl species present.
These adventitious peroxyl are predominantly alkyl hydroperoxides formed by autoxidation
of the surfactants.
[0037] The composition may additionally contain enzymes as found in WO 01/00768 A1 page
15, line 25 to page 19, line 29, the contents of which are herein incorporated by
reference.
[0038] Builders, polymers and other enzymes as optional ingredients may also be present,
as found in WO-00/60045.
[0039] Suitable detergency builders as optional ingredients may also be present, as found
in WO-00/34427.
[0040] In the context of the present invention, bleaching should be understood as relating
generally to the de-colourisation of stains or of other materials attached to or associated
with a substrate. However, it is envisaged that the present invention can be applied
where a requirement is the removal and/or neutralisation by an oxidative bleaching
reaction of malodours or other undesirable components attached to or otherwise associated
with a substrate. Furthermore, in the context of the present invention bleaching is
to be understood as being restricted to any bleaching mechanism or process that does
not require the presence of light or activation by light.
[0041] The present invention extends to both isotropic and complex liquid compositions,
a brief discussion of which follows. Isotropic liquid compositions are clearly preferred
Some isotropic formulations are termed 'micro-emulsion' liquids that are clear and
thermodynamically stable over a specified temperature range. The 'micro-emulsion'
formulation may be water in oil, or oil in water emulsions. Some liquid formulations
are macro-emulsions that are not clear and isotropic. Emulsions are considered meta-stable.
Liquid formulations of the present invention may also contain for example; monoethoxy
quats; AQAs and bis-AQAs; cationic amides; cationic esters; amino/diamino quats; glucamide;
amine oxides; ethoxylated polyethyleneimines; enhancement polymers of the form linear
amine based polymers, e.g. bishexamethylenetriamine; polyamines e.g. TETA, TEPA or
PEI polymers.
[0042] The liquid may be contained within a sachet as found in WO-02/068577. The sachet
is a container within the context of the present invention.
[0043] The liquid composition preferably also contains one or more antioxidants as described
in WO-02/072747 and WO-02/072746.
[0044] The invention will now be illustrated by way of the following non-limiting examples,
in which all parts and percentages are by weight unless otherwise indicated.
EXAMPLES 1, A
[0045] The following liquid detergent formulations were prepared:
| Example |
1 |
A |
| Ingredient |
%(wt) |
% (wt) |
| LAS acid |
6.0 |
6.0 |
| SLES 3 EO |
6.0 |
6.0 |
| NI 7EO |
6.0 |
6.0 |
| Proxel GXL |
0.016 |
0.016 |
| Sorbitol |
3.3 |
3.3 |
| Borax.10H2O |
2.3 |
2.3 |
| MPG |
4.7 |
4.7 |
| Neutralising agent |
0.75 |
0.75 |
| Prifac 5908 |
1.0/5.0 |
- |
| Prifac 7908 |
- |
1.0/5.0 |
| Protease enzyme |
0.4 |
0.4 |
| Bleach catalyst |
0.03 |
0.03 |
| Water |
balance to 100 |
|
Wherein:
LAS acid = C10-C14 alkyl benzene sulphonic acid;
SLES = sodium lauryl ether sulphate (with on average 3 ethylene oxide groups);
NI 7EO = C12-C13 fatty alcohol ethoxylated with an average of 7 ethylene oxide groups;
MPG = monopropylene glycol;
Prifac 5908 = palmkernel fatty acid having an iodine value lower than 1.0;
Prifac 7908 = palmkernel fatty acid having an iodine value higher than 1.0;
Proxel GXL = biocide (20% active).
[0046] As a bleach catalyst, the following chemical compound was used in the examples: 9.9-dihydroxy-2,4-di-(2-pyridyl)-3-methyl-7-(pyridin-2-ylmethyl)-3,7-diaza-bicyclo[3.3.1]nonane-1,5-dicarboxylate
Iron(II) dichloride. This bleach catalyst was prepared as described in Heidi Borzel,
Peter Comba, Karl S. Hagen, Yaroslaw D. Lampeka, Achim Lienke, Gerald Linti, Michael
Merz, Hans Pritzkow, Lyudmyla V. Tsymbal in Inorganica Chimica Acta 337 (2002), 407-419.
WO-02/48301 provides synthetic details of similar compounds.
[0047] As a neutralising agent, triethanolamine (TEA)was used.
The level of the neutralising agent in the liquid formulations of examples 1 and A
was sufficient to bring the pH to 7.
The method of preparation of these formulations was as follows: first all ingredients
except the borax-sorbitol complex were mixed so as to bring the pH-value at 7, and
subsequently said complex was added to the thus-formed mixture.
It can be derived from the above that the formulations of example 1 are according
to the present invention and that the formulations of (comparative) example A are
outside the scope of the invention.
[0048] Samples of all of these liquid formulations were stored in glass vials for two weeks
at a pH of 7 and a temperature of 37°C.
Method of determining the bleach catalyst activity
[0049] The residual bleaching activity of all above liquid formulations were determined
at 40°C in a H
2O
2-containing NaH
2PO
4.H
2O pH 7 buffer and Acid Blue 45 (CAS No. 2861-02-1) as substrate, using the following
protocol.
[0050] Samples of 70 mg liquid were diluted in 10.00 ml MilliQ water. We added 45 µl of
this solution to an assay of 230 µL containing 20mM H
2O
2, 75 µM Acid blue 45 and 54 mM NaH
2PO
4.H
2O pH 7 buffer.
[0051] The changes in absorbance at 600 nm were measured for 5 min. at 40°C using a spectrophotometer.
The absolute changes in absorbance were correlated to activities obtained with freshly
prepared calibration samples. The measured activities expressed as µMol/l are shown
in Table 1.
Table 1:
| The residual bleaching activity (expressed in µMol/l), as function of fatty acid type
and level in the tested liquid formulation after storage thereof for 2 weeks at 37°C
and a pH of 7. |
| Fatty acid type |
1% in formulation |
5% in formulation |
| Prifac 5908 |
2.07 |
1.43 |
| Prifac 7908 |
1.40 |
0.23 |
[0052] The results in Table 1 clearly show a bleach activity advantage in using a type of
fatty acid according to the present invention (prifac 5908). This effect is significant
at both levels tested but it is most pronounced at a fatty acid level of 5% by weight.
EXAMPLE 2
[0053] In this example, various liquid detergent formulations having generally the same
composition as the formulation of example 1 but differing with regard to the type
of neutralising agent, were used. In these compositions, the following compounds were
used as neutralising agent: triethanolamine (TEA), monoethanolamine (MEA), triethylamine,
dimethyl ethanolamine, tetramethyl ammoniumhydroxide, tetraethyl ammoniumhydroxide,
and tetrabutyl ammoniumhydroxide.
[0054] In these compositions, the level of the neutralising agent was sufficient to bring
the pH to around 7.
[0055] Samples of these liquid formulations were stored in glass vial for two weeks at a
pH of 7 and a temperature of 5°C.
During this storage period the physical stability was regularly visually inspected.
It was particularly tested if precipitation and/or phase separation could be observed.
At the end of the storage period, the pH-values of the formulations were measured.
Subsequently, the formulations were diluted with water to obtain 0.7%wt solutions.
The pH-values of the thus-formed solutions in water was also measured.
The results of all these measurements are shown in Table 2.
Table 2:
| pH-values and physical stability's as a function of the type of neutralising agent
in the tested liquid composition. |
| Neutralising Agent |
pH-value before Dilution |
pH-value of 0.7% solution |
Physical Stability |
| TEA |
6.7 |
7.7 |
yes |
| MEA |
6.7 |
8.4 |
1 week |
| Triethylamine |
6.9 |
8.3 |
yes |
| Dimethyl Ethanolamine |
6.9 |
8.5 |
yes |
| Tetramethyl ammonium hydroxide |
6.7 |
8.2 |
1 week |
| Tetraethyl ammonium hydroxide |
6.7 |
8.1 |
1 week |
| Tetrabutyl Ammonium Hydroxide |
6.9 |
8.2 |
1 week |
[0056] It can be noticed that the physical stability of the MEA and ammoniumhydroxide containing
formulations is such that phase separation was observed after 1 week of storage at
5°C.
The formulations containing the other types of neutralising agent were all found to
be fully stable during/after storage.
[0057] It can also be seen that the action of the pH-jump system present in the tested formulations
upon dilution with water was somewhat hampered when using TEA as neutralising agent
as compared to the formulations with the other types of neutralising agents. When
applying TEA the pH-value was raised to 7.7 upon dilution, whereas the pH-value increased
to levels above 8 with the other types of neutralising agent.