[0001] This invention relates to anti-foam granules for use in detergent compositions and
to a process_for their preparation.
[0002] The low-foaming fabric washing powder market in Europe is now well developed and
a number of different anti-foam compounds have been used to suppress the inherent
tendency of powders containing anionic and nonionic surfactants to over-foam when
used in front-loading, drum type washing machines. For instance, mixtures of certain
alkyl phosphoric acids with hydrocarbon waxes, certain silicone oil/hydrophobic silica
mixtures and liquid hydrocarbons have all been used as an alternative to soap as anti-foam,
and a number of other proposals have been made and are published in the patent literature.
[0003] Amongst the latter publications is French patent No 2 416 946, which relates to compositions
containing a special mixture of liquid hydrocarbon with either a solid hydrocarbon
or a fatty acid ester and a hydrophobic silica. Specifically the anti-foam system
consists of:
A (1) 30-98% of a liquid hydrocarbon;
(2) 2-70% of an auxiliary substance selected from solid hydrocarbons (M Pt 35-100°C)
and long chain fatty acid esters of fatty alcohols, or mixtures thereof; and
B 0.1-25% of hydrophobic silica.
[0004] We too have been studying the use of mixtures of hydrophobic silica with hydrocarbons
of various descriptions and have discovered that if these materials are incorporated
into a granule based on a substrate which produces a mechanical action on addition
to water, then it is not necessary to use the proportions specified in French patent
No 2 416. 946, but it is possible to use mixtures containing much less of the liquid
component. There are a number of types of substrate which will produce a mechanical
action on the granule. For example gelatinised starch is a substrate which swells
rapidly on addition to water thereby breaking up the structure of the granule and
leading to extremely good dispersion of the hydrocarbon. Similarly sodium perborate
monohydrate is both extremely water-soluble and also evolves gas when immersed, both
properties being ones which tend to break up the granule.
[0005] Accordingly the present invention provides a detergent composition containing an
anionic detergent active compound and/or a nonionic surfactant and anti-foam granules
comprising hydrophobic silica and a mixture of liquid and solid hydrocarbons, characterised
in that the liquid hydrocarbon component constitutes less than 30% by weight of the
total hydrocarbon and in that the silica and the mixture of liquid and solid hydrocarbons
are sorbed on a core of a material producing a mechanical action on addition to water.
[0006] A second aspect of the invention provides two alternative processes for manufacturing
granules for use in the compositions. According to this aspect the invention provides
first a process for the production-of anti-foam granules which comprises:
(a) forming a molten mixture of the liquid and solid hydrocarbons together with the
hydrophobic silica;
(b) spraying the molten mixture onto agitated particles of the core material.
[0007] Secondly, it provides a process for the production of anti-foam granules which comprises:
(a) forming a molten mixture of the liquid and solid hydrocarbons together with the
hydrophobic silica;
'(b) admixing the molten mixture with particles of the core material; and
(c) grinding the resultant mass to granules.
[0008] Normally speaking, the compositions of the invention will contain both a nonionic
surfactant and an anionic detergent active compound. In general compositions which
contain both types of detergent produce lower amounts of foam than those which contain
only anionic surfactant and consequently lower amounts of anti-foam granule will be
required to control the foam.
[0009] Typical anionic detergent active compounds, which may be present in amounts of from
about 2 to 35% by weight of the finished compositions are sodium alkylbenzene sulphonates,
preferably the C
10-C
16 alkyl compounds, sodium primary and secondary alkyl sulphates, preferably the C
10-C
22 alkyl sulphates, sodium olefine sulphonates, preferably the C
10-C
18 sulphonates and sodium alkane sulphonates. Soaps of fatty acids may also be present,
preferably the sodium and potassium salts of C
10-C
22 fatty acids, both saturated and unsaturated. Where soap is the sole anionic surfactant
it may be present in an amount up to about 65% by weight of the finished composition,
down to about 0.2% by weight when other anionic surfactants are present. Typical soaps
which can be used are those formed from coconut oil, tallow, hydrogenated tallow,
hydrogenated rapeseed oil and natural oils containing high proportions of oleic acid
such as sunflower oil.
[0010] Typical nonionic surfactants, are ethoxylated primary and secondary alcohols of from
8 to 25 carbon atoms containing from 3 to 25 moles of ethylene oxide per mole of alcohol.
These materials may generally be present in an amount of from 1 to 25% by weight,
based on the weight of the finished composition.
[0011] Typical detergency builders which can be used are the water-soluble phosphates, carbonates,
percarbonates and aluminosilicates, particularly.the sodium and potassium salts of
these compounds. Organic builders may also be used, examples being sodium carboxymethyloxysuccinate,
sodium citrate, sodium polyacrylates and sodium nitrilotriacetate. Any of these compounds,
or any other builder compound, in any suitable mixture, may be used in amounts of
from 5 to 60% by weight of the finished composition. Other components which will normally
be present are bleaching agents, corrosion inhibitors, anti-redeposition agents, fluorescers,
stabilisers and substantial proportions of water.
[0012] The invention will be further illustrated by means of the following example:
Example
[0013] Six detergent powders having the following formulations were prepared by conventional
slurry-making, spray-drying and dry-dosing techniques.

[0014] The general experimental technique for assessment of. the efficacy of various anti-foam
granules in suppressing the foam produced by these powders is as follows:
First each powder was subjected to accelerated ageing by storing it in an E3 unlaminated
cardboard carton for 2 or 4 weeks at 37°C and 60% relative humidity.
[0015] 200 gms of the powder was placed in the powder dispenser of a Brandt 433 washing
machine containing 4 Kg of clean clothes. The clothes were then washed, using the
main wash cycle which heats up to 90°C, and using water of 30° French hardness. Foam
height was measured against an arbitrary scale attached to the window of the washing
machine.
[0016] The anti-foam granules for incorporation into powders were prepared by forming a
molten mixture of the liquid hydrocarbon, the solid hydrocarbon and silica and spraying
the mixture onto the sorbent in a pan granulator.
[0017] The formulations of the granules were as follows:

[0018] The above granules were incorporated into the powders as shown in the table and the
foam produced was assessed as described.
[0019] It can be seen that whilst initially the foam level is . moderate it decreases as
the temperature rises to a satisfactory level. On the other hand, some deactivation
after storage (accelerated test) is noticed; nevertheless, the foam control of the
granules remains quite satisfactory.
1. A detergent composition containing an anionic detergent active compound and/or
a nonionic surfactant and anti-foam granules comprising hydrophobic silica and a mixture
of liquid and solid hydrocarbons, characterised in that the liquid hydrocarbon component
constitutes less than 30% by weight of the total hydrocarbon and in that the silica
and the mixture of liquid and solid hydrocarbons are sorbed on a core of a material
producing a mechanical action on addition to water.
2. A detergent composition according to claim 1 wherein the material producing a mechanical
action on addition to water comprises gelatinised starch.
3. A detergent composition according to claim 1 or claim 2 wherein the material producing
a mechanical action on addition to water comprises sodium perborate monohydrate.
4. A detergent composition according to any one of the preceding claims wherein the
liquid hydrocarbon component comprises from 15-25% by weight of the total hydrocarbon.
5. A detergent composition according to any one of the preceding claims wherein the
balance of the hydrocarbon component is a petroleum jelly or a paraffin wax having
a drop-melting point of 50°C or higher.
6. A process for the production of anti-foam granules in accordance with claim 1 comprises:
(a) forming a molten mixture of the liquid and solid hydrocarbons together with the
hydrophobic silica and
(b) -spraying the molten mixture onto agitated . particles of the core material.
7. A process for the production of anti-foam granules in accordance with claim 1 which
comprises:
(a) forming a molten mixture of the liquid and solid hydrocarbons together with the
hydrophobic silica,
(b) admixing the molten mixture with particles of the core material; and
(c) grinding the resultant mass to granules.