[0001] This invention relates to detergent particularly but not exclusively for use in domestic
dishwashing although it may find industrial or alternative domestic applications.
[0002] Percentace compositions used in this specification are by weight unless indicated
otherwise.
[0003] According to the present invention a mobile liquid detergent comprises not more than
8% water and not less than 90% of active detergent, including an anionic surface active
agent, an ethanolamide derivative of coconut oil, and a non-ionic polyether.
[0004] An active detergent is a surface active agent, a 0.01% aqueous solution of which
exhibits a surface tension of not more than 45 dyne /cm (4.5 x 10
-2N
m-1).
[0005] Preferred detergents in accordance with this invention comprise not less than 92%
active detergent, not more than 1% polyethylene glycol and not more than 4% glycerin.
[0006] Detergents in accordance with this invention have an advantage that they do not contain
a large proportion of water, thereby facilitating economical transportation and packing.
Furthermore, use of inactive thickening agents such as sodium chloride in compositions
which have been diluted for use is unnecessary since detergent in accordance with
this invention thicken upon dilution with water alone.
[0007] A first preferred composition may be diluted to a 7% to 50% aqueous solution having
a viscosity not less than 200 centistokes and being capable of passing a dishwashing
and foam test as hereinafter defined. More preferred compositions may be diluted to
7% to 20% aqueous solutions having these properties.
[0008] A second preferred higher foaming composition may be diluted to a 15% to 45% aqueous
solution having a viscosity not less than 200 centistokes and being capable of passing
a dishwashing and foam test as hereinafter defined.
[0009] The non-ionic polyether may comprise an alkylphenyl polyether or a polyether derivative
of an alcohol. Preferred alcohol polyethers may be derived from
C13/
C15 or C17/C18 aliphatic alcohols or from mixtures of oleyl and cetyl alcohols.
[0010] Especially preferred compositions may be diluted to 8% to 10% of their strength to
produce solutions preferably having viscosities of 500 to 1000 centistokes, but solutions
showing viscosities up to 2000 centistokes may also be obtained.
[0011] The dishwashing and foam test is performed as follows. Sodium chloride (2.5%), gelatine
(2.5%), caramel (5%), instant potate (9.5%), fat (Trex or Tesco (Registered Trade
Mark) lard 68%), and water (12.5%) are warmed and mixed together. The mixture is placed
in a refrigerator for 24 hours and is removed from the refrigerator at least 30 minutes
before use. A portion (5g) of the mixture is applied to the surface of each plate
used in the test and the plates are then left to stand for 1 hour. The plates are
23cm in diameter and are white in colour.
[0012] A portion (0.5g) of the detergent solution is placed in one end of a polyethylene
bowl having internal dimensions of 33cm x 29cm and a depth of 13cm and which is inclined
at an angle of 25° to the horizontal.
[0013] Water (5t) at a temperature of 54°C is allowed to run onto the detergent through
an aperture 6mm in diameter located 40cm above the detergent. The bowl is arranged
horizontally when half of the water has been added and the remaining water is allowed
to pour into the opposite end of the bowl thereby providing a good foam covering the
entire water surface. A second bowl is filled with water for rinsing the plates. Two
soiled plates are immersed into the water and a stopclock is immediately started.
After 20 seconds the first plate is washed and rinsed. A third plate is then immersed
below the second plate and the second plate is then washed. A fourth plate is then
immersed below the third and the process is repeated until there is no foam remaining
on the surface of the water. The final temperature of the water must not be less than
45°C. The test is repeated ten times and the mean taken.
[0014] The detergent passes this test if eight or more plates can be washed before the foam
dissipates when using a diluted solution equivalent to a maximum concentration of
0.01% of the concentrated detergent.
[0015] The ethanolamide derivative of coconut oil may be a monoethanolamide or diethanolamide
derivative. These. may be formed by reacting coconut oil or the methyl ester thereof
with either monoethanolamine or diethanolamine in the presence of sodium methoxide.
The major constituent of coconut oil is the triglyceride of dodecanoic acid although
shorter and longer chain triglycerides are also present.
[0016] Preferably the anionic detergent is a salt of dodecylbenzenesulphonic acid or a mixture
of salts of alkylbenzenesulphonic acids of which a major constituent is dodecylbenzenesulphonic
acid. Suitable mixtures may be either broad cut or narrow cut, that is there may be
greater or lesser variation in the lengths of the alkyl chains. Narrow cut mixtures
are preferred. The dodecylbenzenesulphonate is soft. There should be no propylene
tetramer present.
[0017] Alternatively or in addition the anionic detergent may comprise an alkyl sulphate,
or an alkyl ether sulphate. These sulphates are advantageous for production of detergents
with good foaming properties. Alkyl sulphates may be derived from linear alk-l-ene
having 12 to 18 carbon atoms for example sodium lauryl sulphate. Preferred alcohol
sulphates may be derived from products of the OXO or Ziegler processes. Preferred
ether sulphates are derived from ethylene oxide and may comprise a major proportion
having the general formula:- .

wherein n is 13 or 15, m is 2 or 3 and X is Na, K, NH
4 or an ethanolamine.
[0018] Preferred detergents in accordance with the invention incorporates an alkylphenyl
polyether such as OH terminated polyether. The latter may be formed by reacting an
alkyl phenol with ethylene oxide. Preferred polyethers incorporate nonyl or octyl
alkyl chains or mixtures including major proportions of such chains. Preferred polyethers
may comprise mixtures of polyether chains with major proportions of chains having
6 or 9 (CH
2CH
20) units or, more preferably, major proportions of both 6 and 9 (CH
2CH
20) unit containing chains. A greater proportion of chains having 6 (CH
2CH
20) units to chains having 9 (CH
2CH
20) units is particularly preferred. Smaller proportions of polyethers with larger
ether chain lengths may be incorporated for example having 12 (CH
ZCH
20) units.
[0019] Preferred detergents in accordance with this invention incorporate a base. Preferred
bases include monoethanolamine, diethanolamine, triethanolamine or potassium or sodium
hydroxides. Monoethanolamine and triethanolamine are particularly preferred.
[0020] Detergents in accordance with this invention may be selected from a wide range of
compositions in which the proportions of the ingredients are chosen so that 7% aqueous
solutions of the detergent exhibit a viscosity of at least 200 centistokes and have
adequate cleaning properties in accordance with the plate washing test.
[0021] The cleaning capabilities and foam end point of detergents in accordance with this
invention are dependent on a number of factors.
[0022] The ratio of anionic detergent to nonionic detergent is important, an excess of non-ionic
detergent being preferred.
[0023] The ratio of anionic detergent to insoluble polyethers is also important, a greater
proportion of anionic detergent having been found to increase the solubility of the
polyether constituent.
[0024] Preferably the detergent incorporates not more than 30% of anionic detergent estimated
as the free acid. More preferably there is between 15% and 25% of dodecylbenzenesulphonic
acid present in detergents which do not contain alkyl or ether sulphates. If the latter
compounds are present the preferred proportion of dodecylbenzenesulphonic acid is
8% to 25%. The proportion of alkyl or ether sulphate is preferably 10% to 30% based
on the weight of the commercially available solutions, the latter containing approximately
70% of the pure compounds.
[0025] The proportion of the ethanolamide derivative of coconut oil has an important effect
of the viscosity of the detergent. The derivative also serves to stabilise the foam.
Preferably there is 10% to 40% of coconut oil ethanolamide present. More preferably
there is 15% to 33% of the ethanolamide, a range of 20% to 30% being especially preferred.
[0026] It has been found that incorporation of alkylphenyl polyethers having a side chain
incorporating a small number of (CH
2CH
20) groups is a key factor effecting the viscosity of detergents in accordance with
the invention. However, such polyethers alone may be insoluble in water. Preferably
the cloud point of the insoluble polyether is less than zero. Mixtures incorporating
nonylphenyl polyether are particularly preferred ingredients, a wide range of ether
chain lengths being advantageous.
[0027] Optimum cleansing capacity has been achieved with alkylphenyl polyethers incorporating
six or nine (CH
2CH
20) groups of mixtures thereof. Nonylphenyl polyethers are particularly efficacious
in control of the viscosity of the diluted detergent. Nonylphenyl polyethers having
a low solubility in water, notably those comprising six (CH
2CH
20) groups are particularly preferred as a major proportion of total polyethers in
the detergent. Preferred detergents incorporate between 25% and 55% .of nonylphenyl
polyether. More preferably there is between 40% and 55% of the polyether. Detergents
in accordance with this invention often incorporate a blend of nonylphenyl polyethers.
For example a detergent which can be diluted to from 8-20% solutions having a viscosity
not less than 300 cp may comprise 1-5% of nonylphenyl polyether incorporating 12 (CH
2CH
20) units, 25-45% of nonylphenyl polyether incorporating 6 (CH
2CH
20) units and 2-10% of nonylphenyl polyethers having 8 or 9 (CH
2CH
20) units. The actual percentages of these three components are chosen so that the
total percentage of polyether falls within the aforementioned range of 25-55%. A particular
efficacious range for the three aforementioned polyethers is 1-3% with 12 (CH
2CH
20) units, 30-45% with 6 (CH
2CH
20) units and 5-10% with 8 or 9 (CH
2CH
20) units.
[0028] Bases having a low molecular weight are preferred, monoethanolamine having been found
to provide more viscous detergents than diethanolamine. Use of triethanolamine has
the advantage of maintaining a constant pH in the detergent. Ethanolamines may be
used in conjunction with sodium or potassium hydroxides, the ratio of alkalai metal
hydroxide to ethanolamine being important.
[0029] Preferably there is 5% to 12% of mono-,di- and triethanolamine present, approximately
1.0 - 1.5x the stoichiometric amount based on the sulphonate and sulphate present
being desirable. The amount of mono,di or triethanolamine is preferably selected so
that a 10% aqueous solution of the detergent has a pH of 6.8 to 9, more preferably
of 7.5 to 8.5. A relatively larger proportion of diethanolamine or triethanolamine
is required if this reagent is used in place of ethanolamine since the mono derivative
is the most active.
[0030] Detergent in accordance with this invention may be diluted to form aqueous solutions
of more than 7% strength, for example 8%, 10%, 20%, 25% and 40%.
[0031] The typical viscosities of various solutions are set out below:-

[0032] A particularly preferred detergent comprises ingredients not exceeding a total of
100% and comprising, 7% to 30% of dodecylbenzenesulphonic acid, 10% to 30% of a solution
equivalent to a 70% solution of anionic detergent of the formula:

wherein n is 13 or 15 and m is 3; 25% to 50% of nonylphenyl polyether; 5% to 40% of
coconut oil diethanolamide and residual percentages of ethanolamine and triethanolamine.
[0033] More preferably the detergent may comprise: 7% to 15% of dodecylbenzeresulphonic
acid; 15% to 25% of the said solution of anionic detergent; 20% to 35% of coconut
oil diethanolamide; 1% to 4% of ethanolamine and 2% to 5% of triethanolamine.
[0034] The total percentage of nonylphenyl polyether and coconut oil diethanolamide is preferably
50% to 65%. The total percentage of dodecylbenzenesulphonic acid and the said anionic
detergent is preferably 20% to 35%. Tie percentage of coconut oil diethanolamide is
preferably 15% to 35%. This detergent yields self-thickening 10-25% aqueous solutions.
Such detergents having a total percentage of polyether and coconut oil diethanolamide
less than 50% form self thickening 15% to 45% aqueous solutions.
[0035] The invention is further described by means of the following Examples and with reference
to Table 1 and Figures 1 to 7 of the accompanying drawings which illustrate detergent
formulations in accordance with the invention.
[0036] Table 1 shows the compositions and properties of preferred detergents including the
viscosities of 7%, 8%, 10% and 20% aqueous solutions;
Fig. 1 shows a 3 dimensional representation of detergent compositions in accordance
with the invention;
Fig. 2 is a plan view of the diagram shown in Figure 1;
Figs. 3 to 7 show sections taken through the diagram shown in Figures 1 and 2.
EXAMPLE 1
[0037] A detergent was prepared from a nonylphenyl polyether incorporating six (CH
2CH
20) units in the side chain (36%), dodecylbenzenesulphonic acid (30%) monoethanolamine
(9%), coconut oil diethanolamide (25%)
.
[0038] A 7,% aqueous solution of the detergent had a viscosity of 300 cs an 8% solution
was found to have a viscosity of 1000 cs and a 10% solution was found to be thixotropic
and to have a viscosity of 2000 cs on a Ford Cup No.4. 5gm of the 10% solution was
found to clean 9 plates according to the plate test.
EXAMPLE 2
[0039] A detergent was prepared from nonylphenyl polyether incorporating six (CH
2CH
20) units (18%), dodecylbenzenesulphonic acid (20%) monoethanolamine (7%), coconut
oil diethanolamide (37%) and nonylphenyl polyether incorporating
9 (
CH2CH20) units (18%). An 8% aqueous solution of the detergent was found to have a viscosity
of 210 cs and a 10% solution was found to have a viscosity of 2000 cs. 5 g of the
10% solution was found to clean 12 plates.
EXAMPLE 3
[0040] A detergent was prepared from nonylphenyl polyether containing six (CH
2CH
20) units (20%) dodecylbenzenesulphonic acid (20%), monoethanolamide (7%), coconut
oil diethanolamide (33%) and nonylphenyl polyether containing nine (CH
2CH
20) units (20%). An 8% aqueous solution of the detergent was found to have a viscosity
of 200 cs and a 10% solution was found to have a viscosity of 2000 cs. The detergent
(5g of 10% solution) was found to clean 13 plates.
EXAMPLE 4
[0041] A detergent was prepared from coconut oil diethanolamide (33%) nonylphenylpolyether
containing 9 (CH
2CH
20) units (5%), nonylphenylpolyether containing 6 (CH
2CH
20) units (35%), dodecylbenzenesulphonic acid (21%) and monoethanolamine (6%). A (10%)
aqueous solution of the detergent was found to have a viscosity of 1600 cs and 7%
aqueous solution was found to have a viscosity of 700 cs. The detergent (5g of 10%
solution) was found to clean 10 plates.
EXAMPLE 5
[0042] A detergent was prepared from coconut oil diethanolamide (32.8%) nonylphenylpolyether
containing 9 (CH
2CH
20) groups (10.8%), nonylphenylpolyether containing 6 (CH
2CH
20) groups (29.5%), narrow cut dodecylbenzenesulphonic acid (20.9%) and monoethanolamine
(5.9%). The viscosity of aqueous solutions of this detergent is shown in Figure 12.
EXAMPLE 6
[0043] A detergent was prepared from coconut oil diethanolamide (25-94%), nonylphenypolyether
containing 12 (CH
2CH
20) groups (0.89%), nonylphenylpolyether containing 8 (CH
2CH
20) groups (4.47%), nonylphenylpolyether containing 6 (CH
2CH
20) groups (30-41%) a sodium sulphated C13/C15 alcohol with 3 (CH
2C
H20) groups (Synperonic 3S70 a 70% commercial solution manufactured by ICI, 24.15%),
dodecylbenzenesulphonic acid (8.68%), monoethanolamine (0.54%),triethanolamine (4.47%)
and preservative (0.45%; Ketrol T,Cochrane and Keane Chemicals).
[0044] The resultant detergent yielded viscous, high foaming solutions upon dilution to
a strength of 10%,15% or 20%.
EXAMPLE 7
[0045] A detergent was prepared from coconut oil diethanolamide (20%), nonylphenylpolyether
containing 9 (CH
2CH
20) groups (2%), nonylphenylpolyether containing 6 (CH
2CH
20) groups (43%), Synperonic 3S70 (20%), dodecylbenzenesulphonic acid (10%), monoethanolamine
(1%) and triethanolamine (4%). The resultant detergent yielded viscous detergents
upon dilution to a strength of 9% to 10%.
EXAMPLE 8
[0046] A detergent was prepared from coconut oil diethanolamide (25%), nonylphenylpolyether
containing 6 (
CH2CH20) groups (25%), Synperonic 3S70 (20%), dodecylbenzenesulphonic acid (20%), monoethanolamine
(2%) and triethanolamine (8%).
[0047] The resultant detergent produced viscous detergents when diluted to strengths of
15%, 20%, 25%, 30% and 40%.
[0048] A number of abbreviations are used in the following description and in the Table
and Figures to which the description relates. These are set out below:-
diethanolamine derivative of coconut oil = CD nonylphenylpolyether containing six
(CH2CH20) units = N6
nonylphenylpolyether containing 9 (CH2CH20) units = N9
nonylphenylpolyether containing twelve (CH2CH20) units = N12
dodecylbenzenesulphonic acid = "acid" monoethanolamine = MEO
[0049] Table 1 shows the composition and properties of preferred detergents. The compositions
of the detergents indicated by the reference numbers 18, 20, 26, 28 and 29 may be
determined from Figure 7. Figure 1 is a three-dimensional diagram showing the proportions
of N6, N9, CD and dodecylbenzenesulphonic acid which may be present in detergents
in accordance with the invention. Figure 2 is a plan view of the latter diagram. Figures
3 to 7 are sections through the diagram shown in Figures 1 and 2 showing variation
of the ingredients N6, N9 and CD at constant proportions of dodecylbenzenesulphonic
acid.
[0050] Figure 3 illustrates the variation at D of Figure 2 of a total of 40% of N9, N6 and
CD in detergents containing constant proportions of 40% Acid, 11% MEO and a residual
9% CD. The shaded area shows the preferred compositions.
[0051] Figure 4 shows the variation at D of Figure 2 of a total of 40% of N9, N6 and CD
in detergents containing constant proportions of 40% Acid, 11% MEO and a residual
9% CD. The shaded area shows the preferred compositions.
[0052] Figure 5 shows the variation at B of Figure 2 of a total of 60% of N9, N6 and CD
in detergents containing constant proportions of 30% Acid, 9% MEO and a residual 1%
CD. The shaded area shows preferred compositions.
[0053] Figure 6 shows the variations at A of Figure 2 of a total of 70% of N9, N6 and CD
in detergents containing constant properties of 20% Acid, 7% MEO and a residual 3%
CD. The first shaded area shows preferred compositions including diethanolamide prepared
from coconut oil or from the methyl ester thereof. The second shaded area shows additional
preferred compositions including diethanolamide prepared from coconut oil only.
[0054] Figure 7 is a section of Figure 2 taken close to Figure 6 and showing variation of
a total of 70% of N6, N9 and CD., in compositions containing constant proportions
of 21% Acid. 6% MEO and a residual 3% of CD. The two shaded areas show preferred and
especially preferred compositions.
[0055] Detergents including 65% or more of dodecylbenzenesulphonic acid have been found
to form gels or to be unstable. Detergents comprising less than 17% of the acid have
been found to have poor cleaning capacity and to exhibit low foam stability. Compositions
containing 10 - 25% of ether sulphate need only contain 8% to 15% of the acid.
[0056] The ingredients NP6, NP9 and NP12 are manufactured under the Registered Trade Mark
SYNPERONIC by ICI although alternative brands may also be used. Coconut oil derivatives
which are useful in accordance with the invention may be obtained under the Registered
Trade Mark ETHYLAN, manufactured by Diamond Shamrock Process Chemicals Limited. Coconut
oil may also be obtained from Rewo Chemicals Limited and Baxenden Chemicals Limited.
Dodecylbenzenesulphonic acid may be obtained from Shell, BP, CFC or Henkel. Ethanolamine
should preferably be the last ingredient which is added when making detergents in
accordance with this invention.

1. A mobile liquid detergent characterised in
comprising not more than 8% water, and not less than 90% of active detergent, including
an anionic surface active agent, an ethanolamide derivative of coconut oil and a non-ionic
polyether.
2. A detergent as claimed in claim 1, characterised in
comprising not less that 92% of active detergent, not more than 1% polyethylene glycol
and not more than 4% glycerin.
3. A detergent as claimed in claim 1 or 2, characterised in that
7% to 50% aqueous solutions of the detergent have a viscosity not less than 200 centistokes
and are capable of passing a dishwashing test as herein defined.
4. A detergent composition as claimed in claim 3, characterised in
forming 8% to 10% aqueous solutions having viscosities of 500 to 1000 centistokes.
5. A detergent as claimed in claim 3, characterised in that
15% to 45% aqueous solutions have a viscosity not less than 200 centistokes.
6. A detergent as claimed in any preceding claim characterised in
comprising a polyether selected from an alkylphenyl polyether or a polyether derived
from aliphatic alcohol selected from: alcohols having 13 to 15 carbon atoms; alcohols
having 17 or 18 carbon atoms or a mixture of oleyl and cetyl alcohols.
7. A detergent as claimed in any preceding claim characterised in that
the anionic detergent comprises dodecylbenzenesulphonic acid or a salt thereof.
8. A detergent as claimed in any preceding claim, characterised in comprising an anionic
detergent selected from an alkyl sulphate or an anionic detergent represented by the
formula:

wherein n is 12 or 15, m is 2 or 3 and X is Na, K, NH
4 or an ethanolamine.
9. A detergent as daimed in any of claims 6 to 8 characterised in
comprising a polyether represented by the formula:

wherein r and s are integers.
10. A detergent as claimed in claim 9, characterised in that r is 8 or 9 and s is
6 to 12.
11. A detergent as claimed in claim 10, characterised in that
a major proportion of the polyethers have r equal to 8 or 9 and s equal to 6 or 9
and comprise a greater proportion of polyethers having s = 6 than having s = 9.
12. A detergent as claimed in any preceding claim, characterised in
comprising 5% to 12% monoethanolamine or triethanolamine.
13. A detergent as claimed in any preceding claim, characterised in
comprising a greater percentage of anionic detergent than polyether.
14. A detergent as claimed in any of claims 1 to 7, or claims 12 or 13 when not appendent
on claims 8 to 11 characterised in
comprising 15% to 25% of dodecylbenzenesulphonic acid.
15. A detergent as claimed in any of claims 8 to 11
characterised in
comprising 8% to 25% of dodecylbenzenesulphonic acid and an amount equivalent to 10%
to 30% of a 70% solution of an alkyl or ether sulphate.
16. A detergent as claimed in any preceding claim, characterised in
comprising 15% to 33% of said ethanolamide.
17. A detergent as claimed in claim 30 or 31, characterised in
comprising 1% to 5% of polyether wherein r is 9 and s is 12, 25% to 45% of polyether
wherein r is 9 and s is 6 and 2% to 10% of polyether wherein r is 9 and s is 8 or
9.
18. A detergent as claimed in claim 17, characterised in
comprising 1% to 3% of polyether wherein r is 9 and s is 12, 30% to 45% of polyether
wherein r is 9 and s is 6 and 5% to 10% of polyether wherein r is 9 and s is 8 or
9.
19. A detergent as claimed in any preceding claim characterised in
comprising ingredients selected from: 7% to 30% of a solution equivalent to a 70%
solution of an anionic detergent of the formula:

wherein n is 13 or 15, m is 3, X is Na, K, NH
4 or an ethanolamine, 25% to 50% of nonylphenyl polyether; 5% to 40% of coconut oil
diethanolamide and residual proportions of ethanolamine and triethanolamine.
20. A detergent as claimed in claim 19, characterised in
comprising ingredients selected from: 7% to 15% of dodecylbenzenesulphonic acid; 15%
to 25% of the said solution of anionic detergent; 30% to 45% of nonylphenyl polyether;20%
to 35% of coconut oil diethanolamide; 1% to 4% of ethanolamine, and 2% to 5% of triethanolamine.
21. A detergent as claimed in claim 19 or 20, characterised in
comprising a total of 50% to 65% of nonylphenyl polyether and coconut oil diethanolamide.
22. A detergent as claimed in any of claims 20 or 21, characterised in
comprising a total of 20% to 35% of dodecylbenzenesulphonic acid and the said anionic
detergent.