Note: Within nine months from the publication of the mention of the grant of the European patent, any

person may give

notice to the European Patent Ofce of opposition to the European patent granted. Notice of opposition shall be led in
a written reasoned statement. It shall not be deemed to have been led until the opposition fee has been paid. (Art.
99(1) European Patent Convention).
Printed by Jouve, 75001 PARIS (FR)
Europisches Patentamt
European Patent Office
Office europen des brevets
(19)
E
P
1

3
0
5

3
8
7
B
1
*EP001305387B1*
(11) EP 1 305 387 B1
(12) EUROPEAN PATENT SPECIFICATION
(45) Date of publication and mention
of the grant of the patent:
19.01.2005 Bulletin 2005/03
(21) Application number: 01949433.5
(22) Date of filing: 25.06.2001
(51) Int Cl.
7
: C11D 3/40, C11D 3/04,
C11D 3/12
(86) International application number:
PCT/EP2001/007177
(87) International publication number:
WO 2002/010327 (07.02.2002 Gazette 2002/06)
(54) COLOURED SPECKLE COMPOSITION AND PARTICULATE LAUNDRY DETERGENT
COMPOSITIONS CONTAINING IT
GEFRBTE TEILCHENZUSAMMENSETZUNG SOWIE DIESE ENTHALTENDE
TEILCHENFRMIGE WASCHMITTEL
COMPOSITION COLOREE A MOUCHETURES ET COMPOSITIONS PARTICULAIRES DE
DETERGENT DE LESSIVE CONTENANT LADITE COMPOSITION
(84) Designated Contracting States:
AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU
MC NL PT SE TR
(30) Priority: 31.07.2000 GB 0018774
(43) Date of publication of application:
02.05.2003 Bulletin 2003/18
(73) Proprietors:
UNILEVER PLC
London EC4P 4BQ (GB)
Designated Contracting States:
CY GB IE
UNILEVER N.V.
3013 AL Rotterdam (NL)
Designated Contracting States:
AT BE CH LI DE DK ES FI FR GR IT LU MC NL PT
SE TR
(72) Inventors:
CARRIEL, Soledad Scarlet Ri, Lever Division
CEP-05120-900, Parque Anhanguera, SP (BR)
NUNZIO, del, Mario, Jovelino, c/o Mixing
Cevirnica
Sanra Branca KM02,Sao Paulo SP 12380-000
(BR)
SCHIOZER, Adriana Lopes
Sao Paulo 13271-000 (BR)
(74) Representative: Elliott, Peter William et al
Unilever PLC
Unilever Intellectual Property Group
Colworth House
Sharnbrook Bedford, MK44 1LQ (GB)
(56) References cited:
GB-A- 1 546 139 US-A- 3 850 833
US-A- 5 605 883
DATABASE WPI Section Ch, Week 197623
Derwent Publications Ltd., London, GB; Class
A97, AN 1976-42484X XP002032900 & JP 49
033905 A (DAINICHISEIKA COLOR & CHEM
MFG), 28 March 1974 (1974-03-28)
EP 1 305 387 B1
2
5
10
15
20
25
30
35
40
45
50
55
Description
TECHNICAL FIELD
[0001] The present invention relates to a coloured
particulate material and its use as speckles in particulate
laundry detergent compositions for use in laundering
fabrics by hand or machine.
BACKGROUND AND PRIOR ART
[0002] It is well known to include visually contrasting
particles, for example, coloured speckles or noodles, in
laundry detergent powders. These may be included as
a cue to the consumer, to indicate the presence of some
specific ingredient, for example, bleach, or may simply
be present to give the product an attractive appearance.
[0003] Problems that have been observed with previ-
ously proposed speckle compositions include poor dis-
solution, poor flow properties, and a tendency for the
colourant to stain fabrics in the wash.
[0004] Speckles based on various carrier materials
have been disclosed in the prior art.
[0005] GB 1 546 139 (Procter & Gamble) discloses
coloured speckles in which a colourant is carried on hy-
dratable alkaline inorganic salt, for example, sodium
tripolyphosphate, sodium carbonate or sodium tetrabo-
rate.
[0006] US 5 606 883 (Bernard et al) discloses col-
oured speckle agglomerates comprising zeolite, noni-
onic surfactant, colourant, binding agent and water.
[0007] EP 19413A (Unilever) discloses coloured
speckles based on a solid surfactant, for example, a
highly-ethoxylated nonionic surfactant.
[0008] EP 60728A (Unilever) discloses coloured
speckles prepared by spraying a detergent base powder
with an aqueous colourant solution which also contains
a hydratable salt, preferably a phosphate, carbonate or
sulphate.
[0009] GB 2 199 338A (Unilever) discloses coloured
speckles prepared by mixing a detergent base powder
with a dyestuff and treating with a binder which is pref-
erably a water-soluble polymer (e.g. acrylic/maleic co-
polymer) or a nonionic surfactant.
[0010] WO 99/51714A (Unilever) discloses coloured
speckles in which the principal carrier material is an al-
pha-hydroxy carboxylic acid, preferably citric acid.
[0011] Other materials that have been proposed as
bases for coloured speckles include soap, sodiummeta-
silicate, and clays.
[0012] WO 90 00006A (PPG Industries Inc) discloses
a particulate halogen bleaching composition, for exam-
ple, calcium hypochlorite, containing about 0.1 to 10
wt% of a colourant-treated particulate inorganic water-
soluble salt, for example, sodium chloride.
[0013] US 4 992 193 (Lever Brothers) discloses a
conventional detergent powder containing soap-based
noodles (but not speckles) which comprise 2-5 wt% in-
organic salt (sodium chloride is specifically disclosed)
and optionally up to 0.1 wt% dyestuff.
[0014] US 3850833 (Colgate-Palmolive) discloses
coloured particles consisting of sodium chloride, potas-
sium chloride and/or sodium sulphate for incorporation
into a scouring cleanser composition.
SUMMARY OF THE INVENTION
[0015] The present inventors have now discovered
that coloured speckles for use in laundry detergent com-
positions may advantageously be based on sodium
chloride. Sodium chloride is stable, inert, highly water-
soluble, and compatible with all ingredients used in laun-
dry detergent compositions.
[0016] The speckles exhibit excellent dissolution be-
haviour and flow properties, and no staining of fabrics
in the wash is observed.
DEFINITION OF THE INVENTION
[0017] The present invention accordingly provides a
particulate laundry detergent composition comprising a
minor proportion of a coloured speckle composition hav-
ing a colour contrasting with that of the major proportion
of the composition, from5 to 60 wt%of detergent-active
material and from 10 to 080 wt% of detergency builder
characterised in that the coloured speckle composition
comprises a colourant and at least 90wt% sodium chlo-
ride.
[0018] The present invention also provides a coloured
particulate composition for use as a speckle composi-
tion in a particulate laundry detergent composition,
which coloured particulate composition comprises:
(a) from 90 to 99.5 wt%, preferably from 95 to 99
wt%, of sodium chloride,
(b) from 0.01 to 6 wt%, preferably from 0.02 to 0.5
wt%, of a colourant,
and at least one of:
(c1) from 0.1 to 10 wt%, preferably from 0.2 to 5
wt%, of silica,
(c2) from 0.1 to 10 wt%, preferably from 0.2 to 1
wt%, of a flow aid other than a silica,
(c3) from 0.01 to 3 wt%, preferably from 0.02 to 0.5
wt%, of an opaque white pigment and,
(c4) from 0.05 to 5 wt%, preferably from 0.1 to 1
wt%, of a binder.
1 2
EP 1 305 387 B1
3
5
10
15
20
25
30
35
40
45
50
55
DETAILED DESCRIPTION OF THE INVENTION
The Speckle Composition
[0019] Preferably the speckle composition contains
from90 to 99.5 wt%, more preferably from95 to 99 wt%,
of sodium chloride.
[0020] Also essential is a colourant. This may be a
pigment, or a water-dispersible dye. Preferred colours
are red and blue. A preferred pigment is Pigment Red
CI 12490. Suitable blue colourants are phthalocyanines.
The colourant is suitably present in an amount of from
0.01 to 6 wt%, preferably from 0.02 to 0.5 wt%, based
on the speckle composition.
[0021] Preferably an opaque white pigment is present
to give the speckle particles sufficient opacity. A suitable
material is titanium dioxide. The opaque white pigment
is suitably present in an amount of from 0.01 to 3 wt%,
preferably from 0.02 to 0.5 wt%.
[0022] According to a preferred embodiment of the in-
vention the speckle composition contains silica, to pro-
vide a protective outer coating on the speckles and to
improve flow. Silica is suitably present in an amount of
from 0.1 wt%, preferably from 0.2 to 5 wt%.
[0023] The speckle composition preferably also con-
tains a flow aid other than a silica. Suitable flow aids are
selected from silicates and aluminosilicates. The flow
aid is suitably present in an amount of from 0.1, prefer-
ably from 0.2 to 1 wt%.
[0024] Preferably the speckle composition also con-
tains a binder. Preferred binders are polymers, for ex-
ample, cellulosic materials, for example, sodium car-
boxymethyl cellulose, or acrylic polymers, for example,
acrylic/maleic copolymers such as Sokalan (Trade
Mark) CP5 ex BASF. Other organic film-forming materi-
als may be envisaged, for example, polyethylene gly-
cols or highly ethoxylated nonionic surfactants. An es-
pecially preferred binder is sodium carboxymethyl cel-
lulose. The binder is suitably present in an amount of
from 0.05 to 5 wt%, preferably from 0.1 to 1 wt%.
Preparation of the Speckle Composition
[0025] The speckle composition may be prepared by
any convenient method for treating the sodium chloride
with the colourant. Any suitable mixing apparatus may
be used. The mixer should have a stainless steel or oth-
er inert interior surface in view of the corrosive proper-
ties of sodium chloride.
[0026] In a preferred procedure, the sodium chloride
is dosed into a mixer, and a premix of the colourant, the
opaque white pigment and the binder then added. If sil-
ica is incorporated, a minor proportion of the silica is
preferably added with the sodium chloride, and the ma-
jor proportion added after addition of the colourant
premix. Flowaid is preferably added last. After thorough
mixing to ensure homogeneity, the composition is dried.
Detergent Compositions
[0027] The coloured speckle composition of the in-
vention is suitable for use in both white and coloured
detergent compositions, provided that there is sufficient
contrast between the colour of the major proportion of
the powder and the colour of the speckles.
[0028] Thus the detergent composition may comprise
a major proportion of white or light-coloured particles
and a minor proportion of the coloured speckle compo-
sition. Alternatively, the detergent composition may
comprise a major proportion of particles having a first
colour, for example, blue, and a minor proportion of the
coloured speckle composition having a second colour
contrasting with the first colour, for example, red.
[0029] The speckle composition is preferably present
in an amount of from 0.01 to 15 wt%, preferably from
0.1 to 10 wt%, more preferably from 1 to 10 wt% and
most preferably from 2 to 8 wt%.
[0030] Detergent compositions according to the in-
vention contain, as well as the speckle composition,
conventional detergent ingredients, notably detergent-
active materials (surfactants), and preferably also de-
tergency builders.
[0031] Heavy-duty laundry detergent compositions in
accordance with the invention may suitably comprise
from 5 to 60 wt% of detergent-active material, from 10
to 80 wt% of detergency builder, from 0.1 to 10 wt% of
the speckles, and optionally other detergent ingredients
to 100 wt%.
[0032] The detergent compositions will contain, as es-
sential ingredients, one or more detergent active com-
pounds (surfactants) which may be chosen from soap
and non-soap anionic, cationic, nonionic, amphoteric
and zwitterionic detergent active compounds, and mix-
tures thereof. Many suitable detergent active com-
pounds are available and are fully described in the liter-
ature, for example, in "Surface-Active Agents and De-
tergents", Volumes I and II, by Schwartz, Perry and
Berch.
[0033] The preferred detergent active compounds
that can be used are soaps and synthetic non-soap an-
ionic and nonionic compounds. Non-soap anionic sur-
factants are especially preferred.
[0034] Non-soap anionic surfactants are well-known
to those skilled in the art. Examples include alkylben-
zene sulphonates, particularly linear alkylbenzene sul-
phonates having an alkyl chain length of C
8
-C
15
; primary
and secondary alkylsulphates, particularly C
8
-C
15
pri-
mary alkyl sulphates; alkyl ether sulphates; olefin sul-
phonates; alkyl xylene sulphonates; dialkyl sulphosuc-
cinates; and fatty acid ester sulphonates. Sodium salts
are generally preferred. A preferred anionic surfactant
is linear alkylbenzene sulphonate.
[0035] Nonionic surfactants may optionally be
present. These include the primary and secondary al-
cohol ethoxylates, especially the C
8
-C
20
aliphatic alco-
hols ethoxylated with an average of from 1 to 20 moles
3 4
EP 1 305 387 B1
4
5
10
15
20
25
30
35
40
45
50
55
of ethylene oxide per mole of alcohol, and more espe-
cially the C
10
-C
15
primary and secondary aliphatic alco-
hols ethoxylated with an average of from 1 to 10 moles
of ethylene oxide per mole of alcohol. Non-ethoxylated
nonionic surfactants include alkylpolyglycosides, glyc-
erol monoethers, and polyhydroxyamides (glucamide).
[0036] Cationic surfactants may optionally be
present. These include quaternary ammonium salts of
the general formula R
1
R
2
R
3
R
4
N
+
X
-
wherein the R
groups are long or short hydrocarbyl chains, typically
alkyl, hydroxyalkyl or ethoxylated alkyl groups, and X is
a solubilising anion (for example, compounds in which
R
1
is a C
8
-C
22
alkyl group, preferably a C
8
-C
10
or
C
12
-C
14
alkyl group, R
2
is a methyl group, and R
3
and
R
4
, which may be the same or different, are methyl or
hydroxyethyl groups); and cationic esters (for example,
choline esters).
[0037] In an especially preferred cationic surfactant of
the general formula R
1
R
2
R
3
R
4
N
+
X
-
, R
1
represents a
C
8
-C
10
or C
12
-C
14
alkyl group, R
2
and R
3
represent me-
thyl groups, R
4
presents a hydroxyethyl group, and X
-
represents a halide or methosulphate ion.
[0038] Optionally, amphoteric surfactants, for exam-
ple, amine oxides, and zwitterionic surfactants, for ex-
ample, betaines, may also be present.
[0039] Preferably, the quantity of anionic surfactant is
in the range of from 5 to 50% by weight of the total com-
position. More preferably, the quantity of anionic sur-
factant is in the range of from 8 to 35 wt%, most prefer-
ably from 10 to 30 wt%
[0040] Nonionic surfactant, if present, is preferably
used in an amount within the range of from 1 to 20 wt%.
[0041] The total amount of surfactant present is pref-
erably within the range of from 5 to 60 wt%.
[0042] The compositions may suitably contain from
10 to 80 wt%, preferably from 15 to 70 wt%, of deter-
gency builder. Preferably, the quantity of builder is in the
range of from 15 to 50 wt%.
[0043] The detergent compositions may contain as
builder a crystalline aluminosilicate, preferably an alkali
metal aluminosilicate, more preferably a sodium alumi-
nosilicate (zeolite).
[0044] The zeolite used as a builder may be the com-
mercially available zeolite A (zeolite 4A) now widely
used in laundry detergent powders. Alternatively, the ze-
olite may be maximum aluminium zeolite P (zeolite
MAP) as described and claimed in EP 384 070B (Uni-
lever), and commercially available as Doucil (Trade
Mark) A24 from Crosfield Chemicals Ltd, UK.
[0045] Zeolite MAP is defined as an alkali metal alu-
minosilicate of zeolite P type having a silicon to alumin-
iumratio not exceeding 1.33, preferably within the range
of from 0.90 to 1.33, preferably within the range of from
0.90 to 1.20.
[0046] Especially preferred is zeolite MAP having a
silicon to aluminiumratio not exceeding 1.07, more pref-
erably about 1.00. The particle size of the zeolite is not
critical. Zeolite A or zeolite MAP of any suitable particle
size may be used.
[0047] Also preferred according to the present inven-
tion are phosphate builders, especially sodium
tripolyphosphate. This may be used in combination with
sodiumorthophosphate, and/or sodiumpyrophosphate.
[0048] Other inorganic builders that may be present
additionally or alternatively include sodium carbonate,
layered silicate, amorphous aluminosilicates.
[0049] Most preferably, the builder is selected from
sodium tripolyphosphate, zeolite, sodium carbonate,
and combinations thereof.
[0050] Organic builders may optionally be present.
These include polycarboxylate polymers such as poly-
acrylates and acrylic/maleic copolymers; polyaspar-
tates; monomeric polycarboxylates such as citrates,
gluconates, oxydisuccinates, glycerol mono-di- and tri-
succinates, carboxymethyloxysuccinates, carboxy-
methyloxymalonates, dipicolinates, hydroxyethyl imino-
diacetates, alkyl- and alkenylmalonates and succinates;
and sulphonated fatty acid salts.
[0051] Organic builders may be used in minor
amounts as supplements to inorganic builders such as
phosphates and zeolites. Especially preferred supple-
mentary organic builders are citrates, suitably used in
amounts of from 5 to 30 wt %, preferably from 10 to 25
wt %; and acrylic polymers, more especially acrylic/
maleic copolymers, suitably used in amounts of from0.5
to 15 wt %, preferably from 1 to 10 wt%.
[0052] Builders, both inorganic and organic, are pref-
erably present in alkali metal salt, especially sodium
salt, form.
[0053] Detergent compositions according to the in-
vention may also suitably contain a bleach system, al-
though non-bleaching formulations are also within the
scope of the invention.
[0054] The bleach system is preferably based on per-
oxy bleach compounds, for example, inorganic persalts
or organic peroxyacids, capable of yielding hydrogen
peroxide in aqueous solution. Suitable peroxy bleach
compounds include organic peroxides such as urea per-
oxide, and inorganic persalts such as the alkali metal
perborates, percarbonates, perphosphates, persilicates
and persulphates. Preferred inorganic persalts are so-
dium perborate monohydrate and tetrahydrate, and so-
dium percarbonate. The peroxy bleach compound is
suitably present in an amount of from 5 to 35 wt%, pref-
erably from 10 to 25 wt%.
[0055] The peroxy bleach compound may be used in
conjunction with a bleach activator (bleach precursor)
to improve bleaching action at low wash temperatures.
The bleach precursor is suitably present in an amount
of from 1 to 8 wt%, preferably from 2 to 5 wt%.
[0056] Preferred bleach precursors are peroxycar-
boxylic acid precursors, more especially peracetic acid
precursors and peroxybenzoic acid precursors; and per-
oxycarbonic acid precursors. An especially preferred
bleach precursor suitable for use in the present inven-
tion is N,N,N',N'-tetracetyl ethylenediamine (TAED).
5 6
EP 1 305 387 B1
5
5
10
15
20
25
30
35
40
45
50
55
[0057] A bleach stabiliser (heavy metal sequestrant)
may also be present. Suitable bleach stabilisers include
ethylenediamine tetraacetate (EDTA) and the polyphos-
phonates such as Dequest (Trade Mark) , EDTMP.
[0058] The detergent compositions may also contain
one or more enzymes. Suitable enzymes include the
proteases, amylases, cellulases, oxidases, peroxidases
and lipases usable for incorporation in detergent com-
positions.
[0059] Preferred proteolytic enzymes (proteases) are
catalytically active protein materials which degrade or
alter protein types of stains when present as in fabric
stains in a hydrolysis reaction. They may be of any suit-
able origin, such as vegetable, animal, bacterial or yeast
origin.
[0060] Proteolytic enzymes or proteases of various
qualities and origins and having activity in various pH
ranges of from 4-12 are available. Proteases of both
high and low isoelectric point are suitable.
[0061] Other enzymes that may suitably be present
include lipases, amylases, and cellulases including
high-activity cellulases such as Carezyme ex Novo.
[0062] In particulate detergent compositions, deter-
gency enzymes are commonly employed in granular
form in amounts of from about 0.1 to about 3.0 wt%.
However, any suitable physical form of enzyme may be
used in any effective amount.
[0063] Antiredeposition agents, for example, cellu-
lose esters and ethers, for example sodiumcarboxyme-
thyl cellulose, may also be present.
[0064] The compositions may also contain soil re-
lease polymers, for example sulphonated and unsul-
phonated PET/POET polymers, both end-capped and
non-end-capped, and polyethylene glycol/polyvinyl al-
cohol graft copolymers such as Sokolan (Trade Mark)
HP22.
[0065] Especially preferred soil release polymers are
the sulphonated non-end-capped polyesters described
and claimed in WO 95 32997A (Rhodia Chimie).
[0066] The detergent compositions may also include
one or more inorganic salts other than builder salts.
These may include, for example, sodium bicarbonate,
sodium silicate, sodium sulphate, magnesiumsulphate,
calciumsulphate, calciumchloride and sodiumchloride.
Preferred inorganic salts are sodium sulphate, sodium
chloride, and combinations thereof. The coloured
speckle composition is especially suitable for incorpo-
ration in detergent compositions which contain sodium
chloride in addition to that present in the speckle com-
position.
[0067] The detergent compositions may also contain
other inorganic materials, for example, calcite, silica,
amorphous aluminosilicate, or clays.
[0068] Other ingredients that may be present include
solvents, hydrotropes, fluorescers, dyes, photobleach-
es, foamboosters or foamcontrollers (antifoams) as ap-
propriate, fabric conditioning compounds, and per-
fumes.
[0069] An especially preferred detergent composition
according to the invention comprises:
(i) from 10 to 30 wt% of linear alkylbenzene sulpho-
nate,
(ii) from 5 to 60 wt% of detergency builder selected
from sodium tripolyphosphate, sodium carbonate,
zeolite and combinations thereof,
(iii) from 0 to 50 wt% of sodium chloride,
(iv) from 1 to 10 wt% of the coloured speckle com-
position,
(v) optionally other minor ingredients to 100 wt%,
preferably selected from sodium carboxymethyl
cellulose, sodiumsulphate, bentonite clay, fluoresc-
er, dye of a contrasting colour to that of the coloured
speckle composition, and perfume.
[0070] The detergent compositions of the invention
may be in powder or tablet form.
[0071] Powders of low to moderate bulk density may
be prepared by spray-drying a slurry, and optionally
postdosing (dry-mixing) further ingredients. "Concen-
trated" or "compact" powders may be prepared by mix-
ing and granulating processes, for example, using a
high-speed mixer/granulator, or other non-tower proc-
esses. In both types of powder, the speckle composition
may be incorporated by postdosing (dry mixing).
[0072] The detergent composition of the invention
may alternatively be in tablet form. Tablets may be pre-
pared by compacting powders, especially "concentrat-
ed" or "compact" powders, prepared as described
above. The speckle composition is then included in the
powder prior to compaction.
EXAMPLES
[0073] The invention will now be illustrated in further
detail by means of the following Examples, in which
parts and percentages are by weight unless otherwise
stated.
Example 1: Pink Speckle Composition
[0074] A speckle composition was prepared to the fol-
lowing formulation:
Ingredient Weight %
Sodium chloride 98.50
Silica 1.00
Sodium carboxymethyl cellulose 0.16
Zeolite 0.35
7 8
EP 1 305 387 B1
6
5
10
15
20
25
30
35
40
45
50
55
[0075] The composition was prepared as follows. The
ingredients were introduced into a stainless steel mixer
in the following order:
1. Sodium chloride
2. Silica (0.33 wt%)
3. Pigment solution (titaniumdioxide, red colourant,
sodium carboxymethyl cellulose)
4. Silica (rest)
5. Zeolite
[0076] The ingredients were mixed for a period of time
sufficient to ensure homogeneity, and the resulting par-
ticulate material then dried.
[0077] The speckles were of an attractive pink colour.
Comparative Examples A to C
[0078] Speckles using the same colourant were pre-
pared using the following materials instead of sodium
chloride:
Detergent Compositions
[0079] The speckle compositions of Example 1 and
Comparative Examples A, B and C were introduced, at
a level of 4 wt%, into samples of a laundry detergent
powder having the following formulation:
(continued)
Ingredient Weight %
Titanium dioxide, dispersed CI 77891 0.05
Pigment Red CI 12490 0.09
Comparative Example Carrier material
A Soap
B Sodium metasilicate
C Sodium carbonate
Ingredient Weight %
Linear alkylbenzene sulphonate 14.700
Sodium tripolyphosphate 1.024
Zeolite (100%) 4.863
Sodium carbonate 24.200
Speckle composition (1, A, B or C) 4.000
Sodium chloride 45.7486
Sodium sulphate 0.0205
Bentonite clay 2.6621
Fluorescers (Tinopal* CBS-X, DMS) 0.1822
[0080] The pink speckles of Example 1 had a strong
visual impact giving the product an attractive appear-
ance. On storage no loss of colour from the speckles
was observed.
Dissolution and Staining Test
[0081] The detergent compositions and speckle com-
positions were tested for dissolution and for fabric stain-
ing.
[0082] Dissolution was measured by a conductivity
method.
[0083] Staining was measured using hand bowl wash
methodology. The fabrics used were knitted cotton, and
polyester (67%) /cotton (33%).
[0084] Three different handwash methods were used:
(i) the powder was dissolved in water in a bowl and
the fabrics then added,
(ii) the fabrics were placed in the water in the bowl
and the powder then added,
(iii) the fabrics were thoroughly wetted and a con-
centrated paste (powder and a little water) applied
directly.
[0085] In methods (i) and (ii), the detergent composi-
tions were used at a concentration in the wash liquor of
3.5 g/l.
[0086] The fabrics were allowed to soak for 1 hour and
for 2 hours, and the fabrics were then washed and
rinsed.
The speckle compositions were also placed directly on-
to wet fabrics for 1 hour and 2 hours of soak.
[0087] The results were as follows:
[0088] Only the sodium-chloride-based speckles of
Example 1 gave good dissolution without any fabric
staining. No staining was observed even under the most
stressed conditions.
(continued)
Ingredient Weight %
Sodium carboxymethyl cellulose 0.1184
Blue dye 0.0124
Perfume 0.2700
Water and minor ingredients balance
Example 1 A B C
Dissolution Good Poor Good Good
Staining No No Yes Yes
9 10
EP 1 305 387 B1
7
5
10
15
20
25
30
35
40
45
50
55
Claims
1. A particulate laundry detergent composition com-
prising a minor proportion of a coloured speckle
composition having a colour contrasting with that of
the major proportion of the composition, from 5 to
60 wt% of detergent-active material and from 10 to
80 wt%of detergency builder characterised in that
the coloured speckle composition comprises at
least 90 wt% sodium chloride.
2. A detergent composition as claimed in claim 1,
characterised in that the coloured speckle compo-
sition comprises:
(a) from 90 to 99.5 wt%, preferably from 95 to
99 wt%, of sodium chloride,
(b) from 0.01 to 6 wt%, preferably from 0.02 to
0.5 wt%, of a colourant,
(c) optionally from 0.1 to 10 wt%, preferably
from 0.2 to 5 wt%, of silica,
(d) optionally from 0.1 to 10 wt%, preferably
from 0.2 to 1 wt%, of a flow aid other than a
silica,
(e) optionally from 0.01 to 3 wt%, preferably
from 0.02 to 0.5 wt%, of an opaque white pig-
ment,
(f) optionally from 0.05 to 5 wt%, preferably
from 0.1 to 1 wt%, of a binder.
3. A detergent composition as claimed in any preced-
ing claim, characterised in that it comprises from
0.01 to 15 wt%, preferably from0.1 to 10 wt%, more
preferably from1 to 10 wt%, of the coloured speckle
composition.
4. A detergent composition as claimed in any preced-
ing claim, characterised in that it further compris-
es sodium chloride additional to that present in the
coloured speckle composition.
5. A detergent composition as claimed in any preced-
ing claim, characterised in that it comprises a ma-
jor proportion of white or light-coloured particles and
a minor proportion of the coloured speckle compo-
sition.
6. A detergent composition as claimed in any one of
claims 1 to 4, characterised in that it comprises a
major proportion of particles having a first colour
and a minor proportion of the coloured speckle com-
position having a second colour contrasting with the
first colour.
7. A detergent composition as claimed in claim 6,
characterised in that the major proportion of par-
ticles is blue and the coloured speckle composition
is red.
8. A detergent composition as claimed in any preced-
ing claim, characterised in that it comprises from
0.1 to 10 wt% of the coloured speckle composition,
and optionally other detergent ingredients to 100
wt%.
9. A detergent composition as claimed in claim 8,
characterised in that it comprises:
(i) from10 to 30 wt%of linear alkylbenzene sul-
phonate,
(ii) from 5 to 60 wt% of detergency builder se-
lected from sodium tripolyphosphate, sodium
carbonate, zeolite and combinations thereof,
(iii) from 0 to 50 wt% of sodium chloride,
(iv) from 1 to 10 wt% of the coloured speckle
composition,
(v) optionally other minor ingredients to 100
wt%, preferably selected from sodium car-
boxymethyl cellulose, sodium sulphate, ben-
tonite clay, fluorescer, dye of a contrasting col-
our to that of the coloured speckle composition,
and perfume.
10. A detergent composition as claimed in any preced-
ing claim, characterised in that it is in powder or
tablet form.
11. A coloured particulate composition for use as a
speckle composition in a particulate laundry deter-
gent composition, characterised in that the col-
oured particulate composition comprises:
(a) from 90 to 99.5 wt%, preferably from 95 to
99 wt%, of sodium chloride,
(b) from 0.01 to 6 wt%, preferably from 0.02 to
0.5 wt%, of a colourant,
and at least one of:
(c1) from 0.1 to 10 wt%, preferably from 0.2 to
5 wt%, of silica,
(c2) from 0.1 to 10 wt%, preferably from 0.2 to
1 wt%, of a flow aid other than a silica,
(c3) from 0.01 to 3 wt%, preferably from 0.02 to
0.5 wt%, of an opaque white pigment,
11 12
EP 1 305 387 B1
8
5
10
15
20
25
30
35
40
45
50
55
(c4) from 0.05 to 5 wt%, preferably from 0.1 to
1 wt%, of a binder.
12. A coloured particulate composition as claimed in
claim 11, characterised in that it comprises a flow
aid (c2) selected from silicates, aluminosilicates
and mixtures thereof.
13. A coloured particulate composition as claimed in
claim 11 or claim 12, characterised in that the col-
ourant (b) is a red or blue pigment.
14. A coloured particulate composition as claimed in
any one of claims 11 to 13, characterised in that
it comprises titanium dioxide as an opaque white
pigment (c3).
15. A coloured particulate composition as claimed in
any one of claims 11 to 14, characterised in that
it comprises a polymeric binder (c4).
16. A coloured particulate composition as claimed in
claim15, characterised in that the polymeric bind-
er (c4) is sodium carboxymethyl cellulose.
Patentansprche
1. Teilchenfrmige Wschewaschmittelzusammen-
setzung, umfassend einen geringen Anteil einer ge-
frbten Sprenkelzusammensetzung mit einer Far-
be, die mit jener des Hauptanteils der Zusammen-
setzung im Kontrast steht, von 5 bis 60 Gewichts-
prozent des waschaktiven Materials und 10 bis 80
Gewichtsprozent Waschmittelbuilder, dadurch ge-
kennzeichnet, dass die gefrbte Sprenkelzusam-
mensetzung mindestens 90 Gewichtsprozent Natri-
umchlorid umfasst.
2. Waschmittelzusammensetzung nach Anspruch 1,
dadurch gekennzeichnet, dass die gefrbte
Sprenkelzusammensetzung umfasst:
(a) 90 bis 99,5 Gewichtsprozent, vorzugsweise
95 bis 99 Gewichtsprozent, Natriumchlorid,
(b) 0,01 bis 6 Gewichtsprozent, vorzugsweise
0,02 bis 0,5 Gewichtsprozent, eines Frbemit-
tels,
(c) gegebenenfalls 0,1 bis 10 Gewichtsprozent,
vorzugsweise 0,2 bis 5 Gewichtsprozent, Sili-
ziumdioxid,
(d) gegebenenfalls 0,1 bis 10 Gewichtsprozent,
vorzugsweise 0,2 bis 1 Gewichtsprozent, einer
Fliehilfe, die von einem Siliziumdioxid ver-
schieden ist,
(e) gegebenenfalls 0,01 bis 3 Gewichtsprozent,
vorzugsweise 0,02 bis 0,5 Gewichtsprozent, ei-
nes opaken weien Pigments,
(f) gegebenenfalls 0,05 bis 5 Gewichtsprozent,
vorzugsweise 0,1 bis 1 Gewichtsprozent, eines
Bindemittels.
3. Waschmittelzusammensetzung nach einem voran-
gehenden Anspruch, dadurch gekennzeichnet,
dass sie 0,01 bis 15 Gewichtsprozent, vorzugswei-
se 0,1 bis 10 Gewichtsprozent, bevorzugter 1 bis
10 Gewichtsprozent, der gefrbten Sprenkelzu-
sammensetzung umfasst.
4. Waschmittelzusammensetzung nach einem voran-
gehenden Anspruch, dadurch gekennzeichnet,
dass sie weiterhin Natriumchlorid, zustzlich zu je-
nem, das in der gefrbten Sprenkelzusammenset-
zung vorliegt, umfasst.
5. Waschmittelzusammensetzung nach einem voran-
gehenden Anspruch, dadurch gekennzeichnet,
dass sie einen Hauptanteil von weien oder hell ge-
frbten Teilchen und einen geringen Anteil der ge-
frbten Sprenkelzusammensetzung umfasst.
6. Waschmittelzusammensetzung nach einem der
Ansprche 1 bis 4, dadurch gekennzeichnet,
dass sie einen Hauptanteil von Teilchen mit einer
ersten Farbe und einen geringen Anteil der gefrb-
ten Sprenkelzusammensetzung mit einer zweiten
Farbe, die mit der ersten Farbe in Kontrast steht,
umfasst.
7. Waschmittelzusammensetzung nach Anspruch 6,
dadurch gekennzeichnet, dass der Hauptanteil
der Teilchen blau ist und die gefrbte Sprenkelzu-
sammensetzung rot ist.
8. Waschmittelzusammensetzung nach einem voran-
gehenden Anspruch, dadurch gekennzeichnet,
dass sie 0,1 bis 10 Gewichtsprozent der gefrbten
Sprenkelzusammensetzung und gegebenenfalls
andere Waschmittelbestandteile auf 100 Gewichts-
prozent umfasst.
9. Waschmittelzusammensetzung nach Anspruch 8,
dadurch gekennzeichnet, dass sie umfasst:
(i) 10 bis 30 Gewichtsprozent lineares Al-
kylbenzolsulfonat,
(ii) 5 bis 60 Gewichtsprozent Waschmittelbuil-
der, ausgewhlt aus Natriumtripolyphosphat,
Natriumcarbonat, Zeolith und Kombinationen
davon,
(iii) 0 bis 50 Gewichtsprozent Natriumchlorid,
(iv) 1 bis 10 Gewichtsprozent der gefrbten
Sprenkelzusammensetzung,
(v) gegebenenfalls andere geringe Bestandtei-
le auf 100 Gewichtsprozent, vorzugsweise aus-
gewhlt aus Natriumcarboxymethylcellulose,
13 14
EP 1 305 387 B1
9
5
10
15
20
25
30
35
40
45
50
55
Natriumsulfat, Bentonitton, Fluoreszenzmittel,
Farbstoff von einer zu jener der gefrbten
Sprenkelzusammensetzung im Kontrast ste-
henden Farbe und Parfm.
10. Waschmittelzusammensetzung nach einem voran-
gehenden Anspruch, dadurch gekennzeichnet,
dass sie in Pulver- oder Tablettenform vorliegt.
11. Gefrbte Teilchenzusammensetzung zur Verwen-
dung als eine Sprenkelzusammensetzung in einer
teilchenfrmigen Wschewaschmittelzusammen-
setzung, dadurch gekennzeichnet, dass die ge-
frbte teilchenfrmige Zusammensetzung umfasst:
(a) 90 bis 99,5 Gewichtsprozent, vorzugsweise
95 bis 99 Gewichtsprozent, Natriumchlorid,
(b) 0,01 bis 6 Gewichtsprozent, vorzugsweise
0,02 bis 0,5 Gewichtsprozent, eines Frbemit-
tels,
und mindestens eines von:
(c1) 0,1 bis 10 Gewichtsprozent, vorzugsweise
0,2 bis 5 Gewichtsprozent, Siliziumdioxid,
(c2) 0,1 bis 10 Gewichtsprozent, vorzugsweise
0,2 bis 1 Gewichtsprozent, einer Fliehilfe, die
von einem Siliziumdioxid verschieden ist,
(c3) 0,01 bis 3 Gewichtsprozent, vorzugsweise
0,02 bis 0,5 Gewichtsprozent, eines opaken
weien Pigments,
(c4) 0,05 bis 5 Gewichtsprozent, vorzugsweise
0,1 bis 1 Gewichtsprozent, eines Bindemittels.
12. Gefrbte teilchenfrmige Zusammensetzung nach
Anspruch 11, dadurch gekennzeichnet, dass sie
eine Fliehilfe (c2), ausgewhlt aus Silikaten, Alu-
minosilikaten und Gemischen davon, umfasst.
13. Gefrbte teilchenfrmige Zusammensetzung nach
Anspruch 11 oder Anspruch 12, dadurch gekenn-
zeichnet, dass das Frbemittel (b) ein rotes oder
blaues Pigment ist.
14. Gefrbte teilchenfrmige Zusammensetzung nach
einem der Ansprche 11 bis 13, dadurch gekenn-
zeichnet, dass sie Titandioxid als ein opaques wei-
es Pigment (c3) umfasst.
15. Gefrbte teilchenfrmige Zusammensetzung nach
einem der Ansprche 11 bis 14, dadurch gekenn-
zeichnet, dass sie ein polymeres Bindemittel (c4)
umfasst.
16. Gefrbte teilchenfrmige Zusammensetzung nach
Anspruch 15, dadurch gekennzeichnet, dass das
polymere Bindemittel (c4) Natriumcarboxymethyl-
cellulose ist.
Revendications
1. Composition dtergente particulaire de lessive
comprenant une proportion mineure de composi-
tion de grains de couleur ayant une couleur contras-
tant avec celle de la proportion principale de la com-
position, de 5 60 % en poids de matriau dter-
gent actif et de 10 80 % en poids d'dificateur de
dtergence, caractrise en ce que la composi-
tion de grains de couleur comprend au moins 90 %
en poids de chlorure de sodium.
2. Composition dtergente selon la revendication 1,
caractrise en ce que la composition de grains
de couleur comprend :
(a) de 90 99,5 % en poids, de prfrence de
95 99 % en poids de chlorure de sodium ;
(b) de 0,01 6 % en poids, de prfrence de
0,02 0,5 % en poids d'un colorant ;
(c) optionnellement de 0,1 10 % en poids, de
prfrence de 0,2 5 % en poids de silice ;
(d) optionnellement de 0,1 10 % en poids, de
prfrence de 0,2 1 % en poids d'un aide
l'coulement autre que la silice ;
(e) optionnellement de 0,01 3 % en poids, de
prfrence de 0,02 0,5 % en poids d'un pig-
ment blanc opaque ;
(f) optionnellement, de 0,05 5 % en poids, de
prfrence de 0,1 1 % en poids d'un liant.
3. Composition dtergente selon l'une quelconque
des revendications prcdentes, caractrise en
ce qu'elle comprend de 0,01 15 % en poids, de
prfrence de 0,1 10 % en poids, plus prfren-
tiellement de 1 10 % en poids, de la composition
de grains de couleur.
4. Composition dtergente selon l'une quelconque
des revendications prcdentes, caractrise en
ce qu'elle comprend en outre du chlorure de so-
dium en plus de celui prsent dans la composition
de grains de couleur.
5. Composition dtergente selon l'une quelconque
des revendications prcdentes, caractrise en
ce qu'elle comprend une proportion principale de
particules blanches ou de couleur claire et une pro-
portion mineure de la composition de grains de cou-
leur.
6. Composition dtergente selon l'une quelconque
des revendications 1 4, caractrise en ce qu'el-
le comprend une proportion principale de particules
ayant une premire couleur et une proportion mi-
neure de la composition de grains de couleur ayant
une seconde couleur qui contraste avec celle de la
premire couleur.
15 16
EP 1 305 387 B1
10
5
10
15
20
25
30
35
40
45
50
55
7. Composition dtergente selon la revendication 6,
caractrise en ce que la partie principale des par-
ticules est bleue et que la composition de grains de
couleur est rouge.
8. Composition dtergente selon l'une quelconque
des revendications prcdentes, caractrise en
ce qu'elle comprend de 0,1 10 % en poids de la
composition de grains de couleur et optionnelle-
ment d'autres ingrdients dtergents hauteur de
100 % en poids.
9. Composition dtergente selon la revendication 8,
caractrise en ce qu'elle comprend :
(i) de 10 30 % en poids d'alkyl benzne sul-
fonate linaire ;
(ii) de 5 60 % en poids d'un dificateur de d-
tergence slectionn partir du tripolyphos-
phate de sodium, du carbonate de sodium, de
la zolite et des combinaisons de ceux-ci ;
(iii) de 0 50 % en poids de chlorure de
sodium ;
(iv) de 1 10 % de la composition de grains de
couleur;
(v) optionnellement, d'autres ingrdients mi-
neurs, hauteur de 100 %, qui sont de prf-
rence slectionns partir de la carboxymthyl
cellulose de sodium, du sulfate de sodium, de
l'argile bentonite, des agents de fluorescence,
des teintures d'une couleur qui contraste avec
celle de la composition de grains de couleur, et
du parfum.
10. Composition dtergente selon l'une quelconque
des revendications prcdentes, caractrise en
ce qu'elle se prsente sous la forme d'une poudre
ou d'une pastille.
11. Composition particulaire colore destine tre uti-
lise en tant que composition de grains de couleur
dans une composition dtergente de lessive, ca-
ractrise en ce que la composition particulaire
colore comprend :
(a) de 99 99,5 % en poids, de prfrence de
95 99 % en poids de chlorure de sodium ;
(b) de 0,01 6 % en poids, de prfrence de
0,02 0,5 % en poids d'un colorant,
et au moins l'un des composants suivants :
(c1) de 0,1 10 % en poids, de prfrence de
0,2 5 % en poids de silice ;
(c2) de 0,1 10 % en poids, de prfrence de
0,2 1 % en poids d'un aide l'coulement
autre qu'une silice ;
(c3) de 0,01 3 % en poids, de prfrence de
0,02 0,5 % en poids d'un pigment blanc
opaque ;
(c4) de 0,05 5 % en poids, de prfrence de
0,1 1 % en poids d'un liant.
12. Composition particulaire colore selon la revendi-
cation 11, caractrise en ce qu'elle comprend un
composant d'aide l'coulement (c2) slectionn
partir des silicates, des aluminosilicates et des m-
langes de ceux-ci.
13. Composition particulaire colore selon la revendi-
cation 11 ou la revendication 12, caractrise en
ce que le colorant (b) est un pigment rouge ou bleu.
14. Composition particulaire color selon l'une quel-
conque des revendications 11 13, caractrise
en ce qu'elle comprend du dioxyde de titane en tant
que pigment blanc opaque (c3).
15. Composition particulaire colore selon l'une quel-
conque des revendications 11 14, caractrise
en ce qu'elle comprend un liant polymre (c4).
16. Composition particulaire colore selon la revendi-
cation 15, caractrise en ce que le liant polymre
(c4) est de la carboxymthyl cellulose de sodium.
17 18