[0001] This invention relates to a process for manufacturing detergent powder containing
a photobleach.
[0002] Photobleaches are now being introduced into washing powders, particularly into those
sold in the sunnier countries of Europe and in South America. The most convenient
way of incorporating photobleaches such as zinc or aluminium phthalocyanine sulphonate
into detergent powders prepared by spray-drying would be to incorporate them into
the aqueous crutcher slurry, together with other components such as detergent active
compound and builders. However, when this method is used in practice, loss of photobleach
occurs, and the resulting powder has poor stability during storage.
[0003] According to this invention there is provided a process for the manufacture of a
particulate detergent fabric washing product which comprises forming a spray-dried
or granulated base powder and combining it with a photobleach compound, characterised
in that the combination is effected by spraying a solution or suspension of the photobleach
onto a powder comprising the base powder.
[0004] European patent application No 0 057 088 (Procter & Gamble Limited) discloses spraying
an aqueous solution of a photobleach and of an amorphous phosphate onto a mixture
of a storage-sensitive detergent and a hydratable salt. In contrast to the disclosure,
the present invention provides a generally applicable process for incorporation of
a photobleach into spray-dried or granulated powders without loss during processing
or subsequent storage.
[0005] One of the key properties of photobleaches is their ability to sorb onto the fibres
of an article. This property is extremely concentration dependent and is also sensitive
to modifications in molecular structure, which are believed to occur when photobleaches
are incorporated into a crutcher slurry. In order to make good what would amount to
a loss of the original photobleach, were it decided to process powder by including
photobleach in the slurry, it would be necessary to increase the initial concentration
to obtain the desired performance in the spray-dried product. That would be an extremely
expensive measure. Even that would not counteract the loss which occurs during storage
when photobleach is incorporated into a powder by a slurry-making and spray-drying
route.
[0006] It is preferred that the photobleach is a zinc or aluminium phthalocyanine sulphonate
and that it is sprayed onto the spray-dried or granulated base powder in aqueous solution
or suspension. While the solution or suspension may be of any desired concentration,
better control of the amount of photobleach incorporated into the powder is achieved
if it is very dilute, for example 0.001 to 0.2% by weight.
[0007] The solution or suspension may be sprayed onto the spray-dried or granulated powder
in any desired fashion, for example in an inclined pan granulator such as an Eirich
pan (trade mark), in a fluidised bed or rotating drum mixer, or onto the powder on
a moving belt, or in a curtain as it falls from one level in the plant to another.
[0008] The solution or suspension preferably contains an inorganic acid salt such as sodium
dihydrogen phosphate, sodium bicarbonate and sodium bisulphate, which has been discovered
to improve the physical properties of the sprayed powder.
[0009] The question of brightness or apparent whiteness is one which really only applies
to fabric washing, other indices being appropriate in the dishwashing field for example.
Consequently, this invention is only applicable to fabric washing products. However,
as implied above it is applicable to both spray-dried products prepared by hot- spray-drying
of an aqueous crutcher slurry, or to granulated products prepared by absorbing the
liquid components of the composition onto the solid ones to provide a balanced, free-flowing
particulate solid.
[0010] The major components of the fabric washing product in accordance with the invention
are one or more anionic and/or nonionic surfactants and one or more detergency builders,
together with a number of optional components.
[0011] 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
lO-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.
[0012] 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.
[0013] 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.
[0014] Typical detergency builders which can be used are the water-soluble phosphates, carbonates
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 and precursors therefore, such as tetraacetylethylene
diamine, corrosion inhibitors, anti-redeposition agents, fluorescers, stabilisers,
enzymes and substantial proportions of water.
[0015] The process of the invention will be illustrated in the following examples, Example
1 being a comparative example.
Example 1
[0016] Aluminium phthalocyanine sulphonate (AIPCS) was incorporated into a crutcher slurry
having the composition quoted below in the amounts shown in Table 1. The slurry was
then spray-dried to a powder and the content of AIPCS was determined by visible absorption
spectroscopy.

Example 2
[0017] A carefully measured quantity of AIPCS solution having a concentration of 0.299%
was sprayed onto spray-dried base powder from an Amicon (trade mark) pressure vessel
fitted with a Delavan Watson (trade mark) single fluid spray jet at an operating pressure
of 70 psig. The base powder (20 Kg) was agitated by being rotated in a 1 metre pan
granulator inclined at an angle of 50-54° to the horizontal and rotating at a speed
of 22 rpm.
[0018] The formulation of the base powder was

[0019] The content of AIPCS was determined as before and was found to be the same as the
theoretical value, within the experimental error.
Example 3
[0020] An aqueous solution containing AIPCS (0.08%) and sodium dihydrogen phosphate (25%)
was sprayed from an Amicon (trade mark) pressure vessel onto a falling curtain of
a spray-dried base powder having the composition shown in Example 2. The rate of flow
of the powder was 25.1 Kg/min and the AIPCS solution was sprayed at a rate of 1.6
Kg/min.
[0021] The AIPCS content was determined as before and was found to be the same as the theoretical
value, within the experimental error, that is to say, there was no measurable loss
of AIPCS during the processing.
[0022] Examples 2 and 3 demonstrate the advantage to be gained as regards reduced loss of
AIPCS during processing by operating the process of the invention, in comparison with
the process defined in Example 1.
Example 4
[0023] The detergent powders produced by the processes described in Examples 1, 2 and 3
were assessed for storage stability. They were sealed in non-laminated packs and stored
at 30°C and 80% relative humidity for 18 weeks. Initially, and at 6 week intervals
the content of AIPCS was analysed spectro-photometrically. The results are shown in
Table II.

[0024] It can be seen that the percentage loss of AIPCS is significantly lower when AIPCS
is added to the powder by spraying, as in Examples 2 and 3 rather than by incorporating
it in the crutcher slurry as in Example 1.
1. A process for the manufacture of a particulate detergent fabric washing product
which comprises forming a spray-dried or granulated base powder and combining it with
a photobleach compound, characterised in that the combination is effected by spraying
a solution or suspension of the photobleach onto a powder comprising the base powder.
2. A process in accordance with claim 1 wherein the solution or suspension is sprayed
onto the powder in a fluidised bed.
3. A process in accordance with claim 1 or claim 2 wherein the photobleach is a zinc
or aluminium phthalocyanine sulphonate.
4. A process in accordance with any one of the preceding claims wherein the concentration
of photobleach in the solution or suspension is from 0.001 to 0.2% by weight.
5. A process in accordance with any one of the preceding claims wherein the solution
or suspension also contains an inorganic salt.
6. A process in accordance with claim 5 wherein the inorganic salt comprises sodium
dihydrogen phosphate, sodium bicarbonate or sodium bisulphate.