Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
CA 02318511 2000-07-07
WO 99136493 PCTIUS98/00587
1
A DETERGENT GRANULE WITH IMPROVED DISSOLUTION
t° FIELD
The present invention relates to a detergent granule having improved
dissolution. The present invention further relates to a surfactant-containing
detergent granule having improved dissolution.
~5 BACKGROUND
There is a current trend for commercially available granular detergent
compositions to have higher bulk densities as weN as higher active ingredient
content. Such detergent compositions offer greater convenience to the
consumer and at the same time, reduce the amount of packaging materials
2o which will ul~mately be disposed of. But for such granular detergent
compositions, there are problems of poor dissolution resulting in residue
andlor
partially dissolved detergent clump/gel-like mass left on fabric, in the
washing
machine, or in a washing machine dispenser drawer. This residue can vary from
fine particles to masses as large as 10 to 100 millimeters in size, and is
very
25 undesirable for consumers.
Although not wanting to be limited by theory, several examples are
illustrated showing how poor dissolution may occur. For example, when
consumers fin;t put detergent composition and clothes in the washing machine
prior to the addition of water in the tub, significant residue is left in the
tub or on
so the clothes. This residue is formed as the machine is filling with water,
since the
CA 02318511 2000-07-07
WO 99136493 PCT/US98/00587
2
detergent is trapped in the clothes and there is no agitation of the tub
contents.
Under these conditions, hydration and dissolution occur on the surface of the
detergent, wherein the detergent forms a hydrated paste, or gel-like mass.
In another example, detergent compositions containing zeolite-built
s powders dispense poorly, especially when such compositions are placed in a
dispenser drawer of a washing machine andlor a detergent dosing device. This
poor dispensing may be caused by the formation of a gel-like mass, which have
high levels of surfactant, upon contact with water. The gel-like mass prevents
a
proportion of the detergent powder from being solubilized in the wash water,
~o which reduces the effectiveness of the detergent. These solubility problems
especially occur in conditions having low water pressures and/or lower washing
temperatures.
It is known that bleach activators in powder form do not remain stable
when incorporated in detergent compositions. Therefore, such particles are
used
~s as extrudates or otherwise formed into larger bleach activator particles or
bodies
in order to maintain the stability of the bleach activator particles. But
these large
particles have dissolution problems in the wash solution. As a result, water-
soluble disintegrants have been used in large bleach activator particles in
order
to have better dissolution of the bleach activators. In this technique, the
water-
2o soluble disintegrants are incorporated into the large bleach activator
particle.
Then, as moisture is exposed to the large particle, the water-soluble
disintegrants
solubilize in the wash solution, leaving gaps in the large particle, and
thereby
promote the rupturing of the large particle and release the activator
particles to
the water.
2s It is also known to use disintegrating aids in bleach activator particles
that
are not very water-soluble, but are water-swellable in the presence of water,
such
as upon contact with the wash solution. In this technique, larger particles
containing these water-swellabie disintegrants break up into small particles
due
to the swelling up of the disintegrants, thus releasing the activator into the
wash
3o solution.
CA 02318511 2002-09-26
3
It has now been surprisingly found that the use of substantially water-
insoluble disintegrants can improve the dissolution of detergent granules
containing high levels of surfactant. Particularly, it has been surprisingly
found
that the water-insoluble disintegrants improve the dissolution of residue
and/or
partially dissolved detergent clumplgel-like masses.
None of the existing art provides all of the advantages and benefits of the
present invention.
SUMMARY
The present invention, in one embodiment, relates to a detergent granule
with improved dissolution comprising, A. from about 10% to about 60% by weight
of a surfactant selected from the group consisting of nonionic surfactant,
linear
alkyl benzene sulfonate, and mixtures thereof; B. from 5% to 60% by weight of
a
builder; C. from about 0.1 % to about 10% by weight of water-insoluble
disintegrant impregnated within the detergent granule; and D. optionally,
other
detersive ingredients.
In another embodiment, there is provided a process for preparing a
detergent granule comprising A. from about 10% to about 60% by weight of a
surfactant selected from the group consisting of nonionic surfactant, linear
alkyl
benzene sulfonate, and mixtures thereof; B. from 5% to 60% by weight of a
builder; C. from about 0.1 % to about 10% by weight of water-insoluble
disintegrant impregnated within the detergent granule; and D. optionally,
other
detersive ingredients, said process comprising the steps of: A. forming a wet
detergent agglomerate by agglomerating a high active paste form of said
surfactant, said builder, and said other optional detersive ingredients in a
high
shear mixer followed by a medium shear mixer; B. drying the wet detergent
agglomerate to obtain a dried detergent agglomerate, wherein the dried
detergent agglomerate has a moisture content from about 1% to about 10%; and
C. impregnating a water-insoluble disintegrant within the dried detergent
agglomerate by further
CA 02318511 2002-09-26
3a
agglomerating the water-insoluble disintegrant, the dried detergent
agglomerate
and a non-aqueous binder in a medium shear mixer.
This invention also relates to processes for impregnating the water-
insoluble disintegrant within the detergent granule.
These and other features, aspects and advantages of the present
invention will become evident to those skilled in the art from a reading of
the
present disclosure.
DETAILED DESCRIPTION
It has now been found that a detergent granule having nonionic and/or
linear alkyl benzene sulfonate surfactants and a water-insoluble disintegrant
impregnated within the detergent granule have surprisingly improved
dissolution,
especially in cold water. While the specification concludes with claims
particularly pointing out and distinctly claiming the invention, it is
believed that
the present invention will be better understood from the following
description.
All percentages are by weight of the detergent granule unless specifically
stated otherwise.
CA 02318511 2002-09-26
4
All ratios are weight ratios unless specifically stated otherwise.
As used herein, "comprising" means that other steps and other ingredients
which do not affect the end result can be added. This term encompasses the
terms "consisting of and "consisting essentially of'.
s As used herein, "cold water" means water which is at a temperature of
below 30°C.
As used herein, "density" means bulk density unless specifically stated
otherwise.
It has now been found that a detergent granule having, by weight of the
granule, from about 10% to about 60°lo surfactant selected from the
group
consisting of nonionic surfactant, linear alkyl benzene sulfonate, and
mixtures
thereof, and from about 0.1 % to about 10% water-insoluble disintegrant
impregnated within the detergent granule can have surprisingly improved
dissolution. The detergent granule has particularly improved dissolution in
cold
water.
As used herein, detergent granule is a granular particle containing at a
2o minimum, a surfactant selected from the group consisting of nonionic
surfactant,
linear alkyl benzene sulfonate, and mixtures thereof, and a water-insoluble
disintegrant impregranted with the detergent granule. The detergent granule
can
optionally comprise other detersive ingredients. Detergent compositions, such
as
laundry detergent compositions, may comprise such detergent granules, in
2s addition to other optional detersive ingredients. The detergent granule
preferably
has a density from about 400 to about 1200 grams per liter, preferably from
about 450 to about 950 grams per liter. The detergent granule preferably has a
mean particle size of from about 200 microns to about 800 microns.
CA 02318511 2000-07-07
WO 99/36493 PCT/US98/00587
As used herein, impregnated within, means that the water-insoluble
disintegrant is substantially ingrained into the interior and dispersed
throughout
the detergent granule.
As used herein, water-insoluble means substantially water-insoluble.
s Preferably, the solubility in water of the water-insoluble disintegrant is
not more
than about 25%, more preferably not more than about 10%.
It has been found that dissolution problems occur for detergent
compositions having a high level of particular surfactants. Specifically,
detergent
granules having a high level of either a nonionic surfactant, linear alkyl
benzene
~o sulfonate surfactant, or a combination of both, have been found to possess
dissolution problems, especially in cold water. Detergent granules having
other
surfactants, especially crystalline surfactants such as alkyl sulfates and
alkyl
alkoxy sulfates, also possess decreased dissolution when used in conjunction
with nonionic and/or linear alkyl benzene sulfonate surfactants.
It has been found that the dissolution of detergent granules containing
these surfactants can be improved by impregnating within the granule a water-
insoluble disintegrant. Without intending to be limited by theory, it is
believed
that for detergent granules containing high levels of surfactant, hydration
and
dissolution occur on the surface of the detergent granule, wherein the
detergent
2o granule forms a hydrated paste, or gel-like mass. The fomlaiion of a gel-
like
mass, which have high levels of surfactant, occur upon contact with water,
such
as when the detergent granule comes into contact with a wash solution. The gel-
like mass prevents a proportion of the detergent granule from being
solubilized in
the wash solution, which reduces the dissolution of the detergent granule.
23 For such detergent granules containing a high level of surfactant, it is
believed that a disintegrant impregnated within the granule absorbs water
through wicking action and expand once in contact with water. This expansion
inside of the granule can then cause the granule to break into smaller pieces,
increasing the surface area of the detergent granule. This increase in surface
3o area exposes more of the detergent granule to the water in the wash
solution,
CA 02318511 2000-07-07
WO 99136493 PCT/US98/00587
6
thereby improving the overall dissolution of the detergent granule, as well as
the
granular detergent composition as a whole.
The invention herein also includes a granular detergent composition
containing the detergent granule described herein, as well as processes for
s making the detergent granule.
Surfactant
The detergent granule contains a surfactant selected from the group
consisting of nonionic surfactant, linear alkyl benzene sulfonate, and
mixtures
~o thereof. The detergent granule can optionally contain other surfactants.
Other
surfactants, especially crystalline surfactants such as alkyl sulfates, alkyl
alkoxy
sulfates, and mixtures thereof, can also possess decreased dissolution when
used in conjunction with nonionic and/or linear alkyl benzene sulfonate
surfactants.
The detergent granule of the present invention contains, by weight of the
granule, from about 10% to about 60% surfactant, preferably from about 15% to
about 40% surfactant.
1. Nonionic surfactant
Polyethylene, polypropylene, and poiybutylene oxide condensates of alkyl
2o phenols are suitable for use as a nonionic surfactant in the present
invention,
with the polyethylene oxide condensates being preferred. These compounds
include the condensation products of alkyl phenols having an alkyl group
containing from about 8 to about 14 carbon atoms, preferably from about 8 to
about 14 carbon atoms, in either a straight-chain or branched-chain
configuration
25 with the alkyiene oxide. In a preferred embodiment, the ethylene oxide is
present
in an amount equal to from about 2 to about 25 moles, more preferably from
about 3 to about 15 moles, of ethylene oxide per mole of alkyl phenol.
Commercially available nonionic surfactants of this type include IgepaITM CO-
530, marketed by the GAF Corporation; and TritonTM X-45, X-114, X-100 and X-
CA 02318511 2002-09-26
7
102, all marketed by the Rohm 8~ Haas Company. These surfactants are
commonly referred to as alkylphenol alkoxylates (e.g., alkyl phenol
ethoxylates).
The condensation products of primary and secondary aliphatic alcohols
with from about 1 to about 25 moles of ethylene oxide are also suitable for
use
s as a nonionic surfactant in the present invention. The alkyl chain of the
aliphatic
alcohol can either be straight or branched, primary or secondary, and
generally
contains from about 8 to about 22 carbon atoms. Preferred are the condensation
products of alcohols having an alkyl group containing from about 8 to about 20
carbon atoms, preferably from about 10 to about 18 carbon atoms, with from
~o about 2 to about 10 moles of ethylene oxide per mole of alcohol. About 2 to
about 9 moles, preferably from about 2 to about 5 moles of ethylene oxide per
mole of alcohol are present in said condensation products. Examples of
commercially available nonionic surfactants of this type include TergitoITM 15-
S-
9 (the condensation product of C11-C15 linear alcohols with 9 moles ethylene
~s oxide), TergitoITM 24-L-6 NMW {the condensation product of C12-C14 Primary
alcohol with 6 moles ethylene oxide with a narrow molecular weight
distribution),
both marketed by Union Carbide Corporation; NeodoITM 45-9 (the condensation
product of C14-C15 linear alcohols with 9 moles of ethylene oxide), NeodoITM
23-3.(the condensation product of C12-C13 linear alcohols with 3.0 moles of
2a ethylene oxide), NeodoITM 45-7 (the condensation product of C14-C15 linear
alcohols with 7 moles of ethylene oxide), NeodoITM 45-5 (the condensation
product of C14-C15 linear alcohols with 5 moles of ethylene oxide) marketed by
Shell Chemical Company, KyroTM EOB (the condensation product of C13-C15
alcohols with 9 moles ethylene oxide), marketed by The Procter & Gamble
TM
2s Company, and Genapol LA 030 or 050 (the condensation product of C12-C14
alcohols with 3 or '5 moles of ethylene oxide) marketed by Hoechst. Preferred
range of HLB in these products is from 8-11 and most preferred from 8-10.
Also useful as a nonionic surfactant in the present invention are the
alkylpolysaccharides disclosed in U.S. Patent 4,565,647 to Llenado, issued
3o January 21, 1986, having a hydrophobic group containing from about 6 to
about
CA 02318511 2000-07-07
WO 99/36493 PCTNS98/00587
8
30 carbon atoms, preferably from about 10 to about 1fi carbon atoms and a
polysaccharide, e.g. a polyglucoside, hydrophilic group containing from about
1.3
to about 10, preferably from about 1.3 to about 3, most preferably from about
1.3
to about 2.7 saccharide units. Any reducing saccharide containing 5 or 6
carbon
s atoms can be used, e.g., glucose, galactose and galactosyl moieties can be
substituted for the glucosyi moieties (optionally the hydrophobic group is
attached at the 2-, 3-, 4-, etc. positions thus giving a glucose or galactose
as
opposed to a glucoside or galactoside). The intersaccharide bonds can be,
e.g.,
between the one position of the additional saccharide units and the 2-, 3-, 4-
,
~o andlor 6- positions on the preceding saccharide units. Also useful herein
are
glucose-derived amides.
Preferred alkylpolyglycosides have the formula:
R2~(CnH2n0)t(9lYcosyl)x
wherein R2 is selected from the group consisting of alkyl, alkylphenyl,
~s hydroxyalkyl, hydroxyalkylphenyl, and mixtures thereof in which the alkyl
groups
contain from about 10 to about 18, preferably from about 12 to about 14,
carbon
atoms; n is 2 or 3, preferably 2; t is from 0 to about 10, preferably 0; and x
is from
about 1.3 to about 10, preferably from about 1.3 to about 3, most preferably
from
about 1.3 to about 2.7. The glycosyl is preferably derived from glucose. To
20 prepare these compounds, the alcohol or alkylpolyethoxy alcohol is formed
first
and then reacted with glucose, or a source of glucose, to form the glucoside
(attachment at the 1-position). The additional glycosyl units can then be
attached between their 1-position and the preceding glycosyl units 2-, 3-, 4-
and/or 6-position, preferably predominately the 2-position.
The condensation products of ethylene oxide with a hydrophobic base
formed by the condensation of propylene oxide with propylene glycol are also
suitable for use as a nonionic surfactant in the present invention. The
hydrophobic portion of these compounds will preferably have a molecular weight
of from about 1500 to about 1800 and will exhibit water insolubility. The
addition
so of poiyoxyethylene moieties to this hydrophobic portion tends to increase
the
CA 02318511 2000-07-07
WO 99/36493 PCT/US98/00587
9 .
water solubility of the molecule as a whole, and the liquid character of the
product is retained up to the point where the polyoxyethylene content is about
50% of the total weight of the condensation product, which corresponds to
condensation with up to about 40 moles of ethylene oxide. Examples of
s compounds of this type include certain commercially-available PluronicTM
surfactants, marketed by BASF.
Also suitable for use as a nonionic surfactant in the present invention are
the condensation products of ethylene oxide with the product resulting from
the
reaction of propylene oxide and ethylenediamine. The hydrophobic moiety of
~o these products consists of the reaction product of ethylenediamine and
excess
propylene oxide, and generally has a molecular weight of from about 2500 to
about 3000. This hydrophobic moiety is condensed with ethylene oxide to the
extent that the condensation product contains from about 40% to about 80% by
weight of polyoxyethyiene and has a molecular weight of from about 5,000 to
~s about 11,000. Examples of this type of nonionic surfactant include certain
commercially available TetronicTM compounds, marketed by BASF.
Especially preferred for use as the nonionic surfactant in the present
invention are polyethylene oxide condensates of alkyl phenols, condensation
products of primary and secondary aliphatic alcohols with from about 1 to
about
20 25 moles of ethylene oxide, alkylpolysaccharides, and mixtures thereof.
More
preferred are Cg-C14 alkyl phenol ethoxytates having from 3 to 15 ethoxy
groups
and Cg-C18 alcohol ethoxylates (preferably C1 p avg.) having from 2 to 10
ethoxy
groups, and mixtures thereof.
Also preferred nonionic surfactants are polyhydroxy fatty acid amide
2s surfactants of the formula:
R2-C-N-Z
II I
O R1
wherein R1 is H, or R1 is C1~ hydrocarbyl, 2-hydroxy ethyl, 2-hydroxy propyl
or
3o a mixture thereof, R2 is C5_31 hydrocarbyl, and Z is a
polyhydroxyhydrocarbyl
CA 02318511 2000-07-07
WO 99/36493 PCTNS98100587
-
having a linear hydrocarbyl chain with at least 3 hydroxyls directly connected
to
the chain, or an alkoxylated derivative thereof. Preferably, R1 is methyl, R2
is a
straight C11-15 alkyl or C16-18 alkyl or alkenyl chain such as coconut alkyl
or
mixtures thereof, and Z is derived from a reducing sugar such as glucose,
s fructose, maltose, lactose, in a reductive amination reaction.
When included herein, the amount of nonionic surfactant in the detergent
granule comprises, by weight of the granule, from about 0% to about 60%,
preferably from about 1 % to about 20% nonionic surfactant.
2. Linear Alkyl Benzene Sulfonate
The linear alkyl benzene sulfonate (LAS) suitable for use herein includes
the water soluble salts, for example, the alkali metal, magnesium, ammonium
and alkyloiammonium salts of organic sulfuric reaction products having in
their
molecular structure an alkyl group containing from about 10 to about 20 carbon
atoms and a sulfonic acid or sulfuric acid ester group. LAS and other carbon
is chain based compounds herein are abbreviated according to the average alkyl
group length. For example, LAS with an average chain length of 12 carbon
atoms is abbreviated as C12 LAS, even though it contains a distribution of LAS
molecules with alkyl groups of differing lengths. Preferred LAS useful herein
are
C10_1g LASs. Especially valuable herein are linear straight chain alkyl
benzene
sulfonates in which the average number of carbon atoms in the alkyl group is
from about 11 to 13, abbreviated as C11_13 LAS. The alkali metal salts,
particularly the sodium and potassium salts of these surfactants are
preferred.
Magnesium salt of LAS may also be useful in certain granule.
When included herein, the amount of LAS surfactant in the detergent
2s granule comprises, by weight of the granule, from about 0% to about 60%,
preferably from about 3% to about 30% LAS.
Water Insoluble Disintearant
The detergent granule of the present invention contains from about 0.1
to about 10%, preferably from about 0.5% to about 7%, more preferably from
3o about 1 % to about 5%, by weight of the detergent granule, a water-
insoluble
CA 02318511 2002-09-26
disintegrant impregnated within the granule. The water-insoluble disintegrant
useful herein is substantially water-insoluble, but can absorb water.
Accordingly, the water-insoluble disintegrant must be impregnated within
the detergent granule, because a disintegrant limited to the outside of the
s detergent granule can 'fail to cause it to break up.
Preferred water-insoluble disintegrants are described in the Handbook of
Pharmaceutical Excipients (1986). Examples of such suitable water-insoluble
disintegrants include starch: natural, modified or pre-gelatinized starch
(with less
than 25% water soluble portion), Veegum (highly refined isomorphous silicate),
~o crospovidone, cellulose, kaolin, crosslinked carboxy methyl cellulose
(e.g.,
TM TM
AcDiSol), microcrystalline cellulose (e.g., Avicei PH101 & PH102), crosslinked
TM
polyvinyl pyrrolidone (e.g., Kollidon Ct-), and mixtures thereof. More
preferred
disintegrants among these disintegrants include crosslinked carboxy methyl
ceNulose (e.g., AcDiSol), microcrystalline cellulose (e.g., Avicel PH101 &
PH102),
~s crossfinked polyvinyl pyrrofidone (e.g., Kollidon CL), and mixtures
thereof.
This water-insoluble disintegrant must be impregnated into the granule in
conditions where little, or preferably from about 1 °fo to about
10°~ water, more
preferably less than about 5% moisture or water is present at the time the
disintegrant is impregnated.
2o Other Detersive Ingredients
In addition to the above, the detergent granule of the invention may
optionally contain other detersive ingredients. The precise nature of these
additional components, and levels of incorporation thereof will depend on the
physical form of the composition, and the nature of the cleaning operation for
is which it is to be used.
The detergent granule of the invention may for example, be formulated as
hand o~ machine laundry detergent compositions including laundry additive
compositions and compositions suitable for use in the soaking and/or
pretreatment of stained fabrics. Furthermore, the detergent granule of the
3o invention can comprise other detersive ingredients.
CA 02318511 2000-07-07
WO 99136493 PCTNS98/00587
12
Other Surfactant
In addition to nonionic surfactant andlor linear alkyl benzene sulfonate
surfactant, other surfactants can optionally be included herein. It has been
s found that the dissolution of certain types of other surfactants, especially
crystalline surfactants, such as for example, alkyl sulfates, can also benefit
from
the invention described herein. The preferred ratio of LAS and/or nonionic
surfactant to a crystalline surfactant, is from about 10:1 to about 1:10.
Without
intending to be limited by theory, it is believed that the increased
dissolution of
~o the nonionic surfactant andlor the LAS surfactant produces a co-
solubilizafion
effect. As the dissolution of the nonionic surfactant and/or the LAS
surfactant
increases, this co-sotubilization effect increases the dissolution of other
surfactants. A preferred example of other surfactants include cationic
surfactant,
amphoteric surfactant, zwitterionic surfactant, and mixtures thereof. Other
is anionic surfactants besides LAS and crystalline surfactants are also
preferred.
Nonlimiting examples of other surfactants useful in the detergent
composition include, for example, branched-chain and random C10-C2p alkyl
sulfates ("AS"), the C10-C1g secondary (2,3) alkyl sulfates of the formula
CH3(CH2)x(CHOSOg M+) CH3 and CH3 (CH2)y(CHOS03-M+) CH2CH3 where
2o x and (y + 1 ) are integers of at least about 7, preferably at least about
9, and M is
a water-solubitizing cat'ron, especially sodium, unsaturated sulfates such as
oleyl
sulfate, the C10-C1g alkyl alkoxy sulfates ("AEXS'; especially EO 1-7 ethoxy
sulfates), C10-C1g alkyl alkoxy carboxylates (especially the EO 1-5
ethoxycarboxylates), the Cl~lg glycerol ethers, the C10-C1g alkyl
2s polyglycosides and their corresponding sulfated polyglycosides, and C12-C18
alpha-sulfonated fatty acid esters. If desired, the conventional nonionic and
amphoteric surfactants such as the C12-C1g alkyl ethoxylates ("AE") including
the so-called narrow peaked alkyl ethoxylates and Cg-C 12 alkyl phenol
alkoxytates (especially ethoxylates and mixed ethoxylpropoxy), C12-C18
3o betaines and sulfobetaines ("sultaines"), C10-C1g amine oxides, and the
like,
CA 02318511 2002-09-26
13
can also be included in the overall compositions. The C10-C1g N-alkyl
polyhydroxy fatty acid amides can also be used. Typical examples include the
C12-C1g N-methyiglucamides. See WO 92106154 to Cook, et al., published
April 16,1992. Other sugar-derived surfactants include the N-alkoxy
polyhydroxy
s fatty acid amides, such as C1p-C1g N-(3-methoxypropyl) glucamide. The N-
propyi through N-hexyl C12-C18 glucamides can be used for low sudsing. C10-
C20 conventional soaps may also be used. If high sudsing is desired, the
branched-chain C10-C16 soaps may be used. Other conventional useful
surfactants are listed in standard texts.
1o Other suitable anionic surfactants to be used are alkyl ester sulfonate
surfactants including linear esters of Cg-C2p carboxylic acids (i.e., fatty
acids)
which are sulfonated with gaseous S03 according to "The Journal of the
American Oil Chemists Society", 52 (1975), pp. 323-329. Suitable starting
materials would include natural fatty substances as derived from tallow, palm
oil,
~s etc.
Further examples are described in "Surface Active Agents and
Detergents" (Vol. ! and !l by Schwartz, Perry and Berch). A variety of such
surfactants are also generally disclosed in U.S. Patent 3,929,678, issued
December 30, 1975 to Laughlin, et al. at Column 23, line 58 through Column 29,
20 line 23.
Potassium Ions
The detergent granule or a granular detergent composition containing the
detergent granule may also contain from about 0.05% to about 50%, preferably
from about 0.5% to about 30%, more preferably from about 1 °~ to about
20%, by
2s weight, of potassium ions.
The potassium ions useful herein can be provided from, for example, a
potassium salt.
A preferred example of such a potassium salt can be selected from the
group consisting of a potassium salt of alkali builders (e.g., potassium salts
of
CA 02318511 2002-09-26
14
carbonates, potassium salts of silicates), a potassium salt of mid-chain
branched
surfactants, and mixtures thereof.
Of the potassium salts, inorganic potassium salts are preferred, and are
more preferably selected from the group consisting of potassium chloride
(KCI),
s potassium carbonate (K2C03), potassium sulfate (K2S04), tetrapotassium
pyrophosphate (K4P207), tripotassium pyrophosphate (HK3P20~), dipotassium
pyrophosphate (H2KZPT0~), and monopotassium pyrophosphate (H3KPz0~),
pentapotassium tripolyphosphate (K5P30~°), tetrapotassium
tripolyphosphate
(HK4P30~°), tripotassium tripolyphosphate (HZK3P30to), dipotassium
~o tripolyphosphate (H3KZP30~°), and monopotassium tripolyphosphate
(H4KP30~o);
potassium hydroxide (KOH); potassium silicate; potassium citrate, potassium
longer alkyl chain, mid-chain branched surfactant compounds, linear potassium
alkylbenzene sulfonate, potassium alkyl sulfate, potassium
alkylpolyethoxylate,
and mixtures thereof. These are commercially available. Inorganic potassium
~s salts may be dehydrated (preferably) or hydrated. Of the hydrates, those
which
are stable up to about 120°F (48.9°C) are preferred. Potassium
carbonate is
most preferred.
Also suitable for use herein are salts of film forming polymers as described
in U.S. Pat. No. 4,379,080 to Murphy, issued Apr. 5, 1983, column 8, line 44
to
2o column 10, line 37, which are either partially or wholly neutralized
with potassium. Particularly preferred are the potassium salts of
copolymers of acrylamide and acrylate having a molecular weight between about
4,000 and 20,000.
Filler Salts
2s In conventional detergent compositions, the filler salts are preferably
present in substantial amounts, typically 17-35% by weight of the total
composition. As one embodiment, the "compact" form of the composition herein
is best reflected by high density (e.g. 500g/liter to 950g/liter) and, in
terms of
granule, by a reduced amount of inorganic filler salt. Inorganic filler salts
are
3o conventional optional ingredients of detergent granules in powder form. In
the
CA 02318511 2000-07-07
WO 99136493 PCTNS98/00587
composition, the filler salt is preferably present in amounts not exceeding
25% of
the total composition, preferably not exceeding 15%, most preferably not
exceeding 5% by weight of the composition.
The inorganic filler salts, such as meant in the present compositions are
s selected from the alkali and alkaline-earth-metal salts of sulfates and
chlorides.
A preferred filler salt is sodium sulfate.
Enzyrmes
The present invention can comprise one or more enzymes which provide
cleaning performance and/or fabric care benefits.
~o Said enzymes include enzymes selected from, hemicellulases,
peroxidases, proteases, gluco-amylases, cellulases, amylases, xylanases,
lipases, esterases, cutinases, pectinases, reductases, oxidases,
phenoloxidases,
lipoxygenases, tigninases, pullulanases, tannases, pentosanases, malanases, f3-
glucanases, arabinosidases chondroitinase, lactase or mixtures thereof.
~s Sleachina Agent
Bleach systems that can be included in the present invention include
bleaching agents such as anhydrous sodium perborate monohydrate, anhydrous
sodium perborate tetrahydrate and percarbonate with a particle size of from
about 400 to about 800 microns in diameter. These bleaching agent
2o components can include one or more oxygen bleaching agents and, depending
upon the bleaching agent chosen, one or more bleach activators. When present
oxygen bleaching compounds will typically be present at levels of from about 1
to about 25°x.
The bleaching agent component for use herein can be any of the
2s bleaching agents useful for detergent compositions including oxygen
bleaches as
well as others known in the art. The bleaching agent suitable for the present
invention can be an activated or non-activated bleaching agent.
One category of oxygen bleaching agent that can be used encompasses
percarboxylic acid bleaching agents and salts thereof. Suitable examples of
this
30 lass of agents include magnesium monoperoxyphthalate hexahydrate, the
CA 02318511 2002-09-26
magnesium salt of meta-chloro perbenzoic acid, 4-nonylamino-4-
oxoperoxybytyric acid and diperoxydodecanedioic acid. Such bleaching agents
are disclosed in U.S. Patent 4,483,781 to Hartman, issued November 20, 1984,
U.S. Patent 4,634,551 to Burns et al., issued January 6, 1987, European Patent
Application 0,133,354 to Banks et al., published February 20, 1985, and
U.S. Patent 4,412,934 to Chung and Spadini, issued November 1, 1983. Highly
preferred oxygen bleaches also iriclude 6-nonylamino-6-oxoperoxycaproic acid
(NAPAA) as described in U.S. Patent 4,634,551 to Hardy and Ingram, issued
January 6, 1987.
~o The hydrogen peroxide releasing agents can be used in combination with
bleach activators such as tetraacetylethylenediamine (TAED),
nonanoyloxybenzene-sulfonate (NOBS, described in US 4,412,934 to Chung and
Spadini, issued November 1, 1983), 3,5,-trimethylhexanoloxybenzenesulfonate
(ISONOBS, described in EP 120,591) or pentaacetylglucose (PAG), which are
~s perhydroiyzed to form a peracid as the active bleaching species, leading to
improved bleaching effect. Also suitable activators are acylated citrate
esters.
Bleaching agents other than oxygen bleaching agents are also known in
the art and can be utilized herein. One type of non-oxygen bleaching agent of
particular interest includes photoactivated bleaching agents such as the
2o sulfonated zinc and/or aluminum phthafocyanines. These materials can be
deposited upon the substrate during the washing process. Upon irradiation with
fight, in the presence of oxygen, such as by hanging clothes out to dry in the
daylight, the sulfonated zinc phthalocyanine is activated and, consequently,
the
substrate is bleached. Preferred zinc phthalocyanine and a photoactivated
2s bleaching process are described in U.S. Patent 4,033,718, issued July 5,
1977 to
Holcombe, et al. Typically, detergent compositions will contain about
0.025°lo to
about 1.25%, by weight, of sulfonated zinc phthalocyanine.
Builder System
The present invention may further comprise a builder system.
CA 02318511 2000-07-07
W O 99/36493 PCTIUS98I00581
17
Any conventional builder system is suitable for use herein including
aiuminosilicate materials, silicates, polycarboxylates and fatty acids,
materials
such as ethylenediamine tetraacetate, diethylene triamine
pentamethyleneacetate, metal ion sequestrants such as
s aminopolyphosphonates, particularly ethylenediamine tetramethylene
phosphonic acid and diethylene triamine pentamethylenephosphonic acid.
Though less preferred for obvious environmental reasons, phosphate builders
can also be used herein where permitted.
Suitable builders can be an inorganic ion exchange material, commonly an
~o inorganic hydrated aluminosilicate material, more particularly a hydrated
synthetic zeolite such as hydrated zeoNte A, X, B, HS or MAP. Another suitable
inorganic builder material is layered silicate, e.g. SKS-6 (Hoechst). SKS-6 is
a
crystalline layered silicate consisting of sodium silicate (Na2Si205).
Poiycarboxylates builder systems can also be useful herein, such as, for
example
~s those disclosed in Belgian Patent Nos. 831,368, 821,369 and 821,370.
Polycarboxylates containing four carboxy groups include oxydisuccinates
disclosed in British Patent No. 1,261,829, 1,1,2,2-ethane tetracarboxylates,
1,1,3,3-propane tetracarboxylates and 1,1,2,3-propane tetracarboxylates.
Polycarboxylates containing sulfo substituents include the sulfosuccinate
2o derivatives disclosed in GB Patent Nos. 1,398,421 and 1,398,422 and in U.S.
Patent No. 3,936,448, and the sulfonated pyrolysed citrates described in GB
Patent No. 1,082,179, while polycarboxylates containing phosphone substituents
are disclosed in GB Patent No. 1,439,000.
Alicyclic and heterocyclic polycarboxylates include cyclopentane-
2s cis,cis,cis-tetracarboxyiates, cyclopentadienide pentacarboxylates, 2,3,4,5-
tetrahydro-furan - cis, cis, cis-tetracarboxylates, 2,5-tetrahydro-furan -cis -
dicarboxylates, 2,2,5,5-tetrahydrofuran - tetracarboxylates, 1,2,3,4,5,6-
hexane -
hexacar-boxylates and carboxymethyl derivatives of polyhydric alcohols such as
sorbitol, mannitol and xylitol. Aromatic poly-carboxylates include mellitic
acid,
CA 02318511 2000-07-07
WO 99/36493 PCTNS98100587
18
pyromeHitic acid and the phthalic acid derivatives disclosed in GB Patent No.
1,425,343.
Of the above, the preferred polycarboxylates are hydroxycarboxylates
containing up to three carboxy groups per molecule, more particularly
citrates.
s Preferred builder systems for use in the present compositions include a
mixture of a water-insoluble aluminosiiicate builder such as zeolite A or of a
layered silicate (SKS-6), and a water-soluble carboxylate chelating agent such
as
citric acid.
A suitable chelant for inclusion in the detergent compositions in
1o accordance with the invention is ethylenediamine-N,N'-disuccinic acid
(EDDS) or
the alkali metal, alkaline earth metal, ammonium, or substituted ammonium
salts
thereof, or mixtures thereof. Preferred EDDS compounds are the free acid form
and the sodium or magnesium salt thereof. Examples of such preferred sodium
salts of EDDS include Na2EDDS and Na4EDDS. Examples of such preferred
~s magnesium salts of EDDS include MgEDDS and Mg2EDDS. The magnesium
salts are the most preferred for inclusion in compositions in accordance with
the
invention.
Preferred builder systems include a mixture of a water-insoluble
aluminosilicate builder such as zeolite A, and a water-soluble carboxylate
2o chelating agent such as citric acid.
Other builder materials that can form part of the builder system for use in
non-liquid compositions include inorganic materials such as alkali metal
carbonates, bicarbonates, silicates, and organic materials such as the organic
phosphonates, amino polyalkylene phosphonates and amino polycarboxylates.
2s Other suitable water-soluble organic salts are the homo- or co-polymeric
acids or their salts, in which the polycarboxylic acid comprises at least two
carboxyl radicals separated from each other by not more than two carbon atoms.
Polymers of this type are disclosed in GB-A-1,596,756. Examples of such
salts are polyacrylates of MW 2,000-10,000 and their copolymers with malefic
CA 02318511 2000-07-07
WO 99136493 PCTIUS98100587
19
anhydride, such copolymers having a molecular weight of from about 4,000 to
about 80,000, especially from about 5,000 to about 20,000.
Detergency builder systems are normally included in amounts of from 5%
to 60% by weight of the composition preferably from 10% to 50% and most
s usually from 20% to 40% by weight.
Softening Agents
Fabric softening agents can also be incorporated into laundry detergent
compositions in accordance with the present invention. These agents may be
inorganic or organic in type. Inorganic softening agents are exemplified by
the
~o smectite clays disclosed in GB-A-1 400 898 and in U.S. Patent 5,019,292.
Organic fabric softening agents include the water insoluble tertiary amines as
disclosed in GB-A1 514 27fi and EP-BO 011 340 and their combination with
mono C,Z-C,4 quaternary ammonium salts are disclosed in EP-B-0 026 527 and
EP-B-0 026 528 and di-long-chain amides as disclosed in EP-B-0 242 919. Other
~s useful organic ingredients of fabric softening systems include high
molecular
weight polyethylene oxide materials as disclosed in EP-A-0 299 575 and 0 313
146.
Levels of smectite clay are normally in the range from 2% to 20%, more
preferably from 5% to 15% by weight, with the material being added as a dry
2o mixed component to the remainder of the formulation.
Die Transfer Inhibitors
The detergent composition of the present invention can also include
compounds, such as polymers, for inhibiting dye transfer from one fabric to
another of solubiiized and suspended dyes encountered during fabric laundering
2s operations involving colored fabrics.
Especially suitable polymeric dye transfer inhibiting agents are polyamine
N-oxide polymers, copolymers of N-vinyipyrrolidone and N-vinyiimidazole,
polyvinylpyrrottdone polymers, polyvinyloxazolidones and polyvinylimidazoles
or
mixtures thereof.
CA 02318511 2000-07-07
WO 99136493 PCTNS98/00587
Other components used in detergent compositions may be employed,
such as soil-suspending agents, soil-release agents, optical brighteners,
abrasives, bactericides, tarnish inhibitors, coloring agents, suds
suppressers,
enzyme stabilizers, and/or encapsulated or non-encapsulated perfumes.
5
Process
The following describes four preferred types of processes. The following
examples further describe and demonstrate the preferred embodiments within
the scope of the present invention. The examples are given solely for the
~o purpose of illustration, and are not to be construed as limitations of the
present
invention since many variations thereof are possible without departing from
its
spirit and scope.
Example 1
~5 The example 1 process is characterized by the following steps:
A. forming a detergent particle by spray-drying an aqueous detergent
slurry comprising a surfactant selected from the group consisting of
nonionic surfactant, linear alkyl benzene sulfonate, and mixtures
thereof; and
2o B. impregnating a water-insoluble disintegrant within the detergent
particle by compacting the aqueous detergent slurry and the water-
insoluble disintegrant.
In the above step A, the aqueous detergent slurry may further include
carbonate, builder such as zeolite A, polymers, cationic surfactant, sodium
z5 silicate andlor water. In the above step A, a spray drying tower is
preferably
used for spray drying. In the above step B, the compacting is conducted by
using a mixer (e.g. using KM mixer of Littleford Inc.). In the above step B,
the
compacting impregnates the water-insoluble disintegrant within the detergent
granule, and includes (1) granulation and densification process in a
medium/high
3o shear batch mixerlgranuiator, or (2) continuous granulation and
densification
CA 02318511 2000-07-07
PCTIUS98/00587
w0 99136493
21
process (e.g. using Lodige~ CB mixer and for Lodige~ KM mixer), (3) use of a
fluid bed process, (4) use of a compaction process (e.g., roll compaction)
andlor
(5) use of an extrusion process. Once formed, the medium to high density
detergent granules thus obtained can be coated by nonionic surfactant andlor
s builder or a flow aid such as zeolite A, and/or can be subsequently mixed
with
additives such as enzymes, bleach, perfume and crystalline layered silicate,
etc.
Example 2
The example 2 process is characterized by the step of impregnating a
1o water-insoluble disintegrant within a detergent agglomerate simultaneously
during a dry-neutralization process, wherein a linear alkyl benzene sulfonic
acid
is neutralized in the presence of an alkaline material. Preferably, the
detergent
granule is prepared by cooling the detergent agglomerate in the cooler.
In the example 2 process, it is the use of a mixer under a dry-
~s neutralization condition which impregnates the water-insoluble disintegrant
within
the detergent granule. The mixer useful herein can be, for example, a high
speed mixeNdensifier, or a variable-speed speed mixerldens~er. Alternatively,
two or more mixersldensifiers can be used, for example, where a high speed
mixer (e.g., a Lodige~ CB mixer) is first used, and then a moderate speed
mixer
20 (e.g., Lodige~ KM mixer) is used. The cooler useful herein can be, for
example,
a fluid bed cooler in which the detergent agglomerates are cooled and fines
are
removed. It is preferred that the detergent agglomerate has a density of from
about 600 to about 950 grams per liter and a mean particle size of from about
250 microns to about 400 microns in diameter. It is preferred that the
detergent
2s granule have a density of from about 550 to about 850 grams per liter and a
mean particle size of from about 400 microns to about 500 microns in diameter.
In the example 2 process, a non-liquid other surfactant can be further
included with the builder and the water-insoluble disintegrant. Preferred
optional
detersive ingredients include enzymes, brighteners, NOBS, perborate, CMC,
CA 02318511 2000-07-07
WO 99136493 PCTNS98100587
22
DTPA, perfume and soil-release agents, and can be dry blended with the cooled
detergent agglomerates.
Example 3
s The example 3 process is characterized by the following steps:
A. providing a nonionic surfactant, an alkaline material, a builder, and
a water-insoluble disintegrant;
B. providing a mixer and a cooler;
C. obtaining a detergent agglomerate by agglomerating the nonionic
~o surfactants, alkaline material, builder, and water-insoluble
disintegrant within the mixer; and
D. preparing a detergent granule by cooling the detergent agglomerate
in the cooler.
In the example 3 process, it is the use of a mixer under agglomeration
~s conditions which impregnates the water insoluble disintegrant within the
detergent granule. This nonionic agglomerate can either be used as an
intermediate in a granular composition, or mixed with other detersive
ingredients.
All other characteristics and equipment of the example 3 process are the same
as in the example 2 process detailed above.
2o The disintegrant may also be added in the medium shear mixer (e.g.
loedige~ KM mixer) and a non-aqueous binder like polyvinyl alcohol (PVA) or
polyethylene glycol (PEG) may be used to reaggiomerate the disintegrant with
the mix coming out of the high shear mixer ( e.g. t-oedige~ CB mixer).
2s x m 1e 4
The example 4 process is characterized by the following steps:
A. forming a wet detergent agglomerate by agglomerating a high
active paste form of a surfactant, an alkaline material, a builder,
and other optional detersive ingredients in a high shear mixer
followed by a medium shear mixer;
CA 02318511 2000-07-07
WO 99/36493 PCTNS98/00587
23
B. drying the wet detergent agglomerate to obtain a dried detergent
agglomerate, wherein the dried detergent agglomerate has a
moisture content from about 1 % to about 10%, preferably less than
about 5%; and
s C. impregnating a water-insoluble disintegrant within the dried
detergent agglomerate by further agglomerating the water-insoluble
disintegrant, the dried detergent agglomerate and a non-aqueous
binder in a medium shear mixer.
Specifically, a high active paste form of surfactant (70-80% active AS,
~o AES,LAS paste) is agglomerated with sodium carbonate, builders (Zeolite A
/STPP ) and other inorganic and organic solids present in the formulation in a
continuous high shear mixer (e.g. Lodige~ CB mixer) followed by further
agglomeration in a medium shear mixer ( e.g. Lodige~ KM mixer). The wet
agglomerate is then preferably dried in a fluid bed drier to reduce the
moisture
~s content, preferably from about 1 % to about 10% and more preferably less
than
about 5%. The dried agglomerate is then mixed with the disintegrant in a
medium shear mixer (e.g. Lodige~ KM mixer) and reagglomerated using a non-
aqueous binder ( e.g. PVA I PEG ). Other detergent additives are then mixed
with the anal agglomerate containing the disintegrant to make the finished
zo pnxiuct.
In the following examples, the abbreviated component identifications have
the following meanings:
CA 02318511 2000-07-07
WO 99/36493
24
PCTNS98100587
NaLAS Sodium linear C12 alkyl benzene sulfonate
KLAS Potassium linear C12 alkyl benzene sulfonate
AS Alkyl Sulfate
AEXS Alkyl Ethoxy Sulfate (X represents ethoxy
number)
NaCX_YAS Sodium CX - CY alkyl sulfate
KCX_yAS Potassium CX - CY alkyl sulfate
25EY A C12_C15 predominantly linear primary alcohol
condensed with an average of Y moles of
ethylene
oxide
NaSKS-6 Crystalline layered silicate of formula
S-Na2Si205
Phosphate or STPP Sodium tripolyphosphate
MAIAA Copolymer of 4:1-1:4 maleidacryiic acid,
average
molecular weight about 4,000-80,000
NOES Nonanoyloxy benzene sulfonate in the form
of the
sodium salt
pg4 Anhydrous sodium perborate tetrahydrate.
TAED Tetraacetyl ethylene diamine
CMC Sodium carboxymethyl cellulose
SRp Soil Release Agents
DTPA Diethylene triamine yenta acetate
Example 5
An aqueous slung comprising anionic surfactants such as NaLAS and Na
s C".,SAS; cationic surfactants such as corn-alkyl methyl bis (hydroxyethyl)
ammonium chloride; polymer builder such as MAIAA; Zeolite A as builder;
carbonate; silicate andlor sulfate is prepared and spray-dried in a spray-
drier to
obtain a low density detergent granule. The low density tower detergent
granule
is then mixed with a water-insoluble disintegrant such as microcrystalline
CA 02318511 2000-07-07
WO 99/36493 PGTNS98/00587
cellulose, crosslinked carboxymethyl cellulose or crosslinked polyvinyl
pyrrolidone in a mixer (e.g. KM mixer by Littleford, Inc.). The mixture is
then
compacted in a roN compactor to impregnate the water-insoluble disintegrant
within the mixture. The roll compactor also increases the density of the
mixture
5 to form high density "chips." The high density (about 1200-1300 g11) chips
from
the compactor are then ground to the desired particle size distribution in a
cage
mill or a hammer mill to obtain a high density detergent granule (about 700-
750g/l). The high density detergent granule is then coated with nonionic
surfactants (e.g., 25E9 and Zeolite A) and precipitated silica as flow aids.
Other
~o additives such as NaSKS-6, enzymes, brighteners, NOBS, perborate,
percarbonate, perfume and SRP are dry-added to these high density granules
and mixed to make the finished detergent granule. Compositions A through D
are shown below and are made according to Example 5.
i
CA 02318511 2000-07-07
WO 99/36493 PCT/US98/00587
26
Composition A B C
NaLAS 24.00 22.00 22.00 22.00
NaC,4.,sAS 4.00 4.00 4.00 4.00
25E9 3.50 3.50 3.50 3.50
Cationics 0.50 1.20 1.20 1.20
NaSKS-6 7.50 6.00 6.00 6.00
Zeolite A 12.00 11.00 11.00 11.00
Silicate 12.00 12.50 12.50 12.50
7.00 14.00 14.00 14.00
Carbonate 15.00 11.00 11.00 11.00
Sulfate 3.00 0.00 0.00 0.00
microcrystalline cellulose0.00 0.00 4.00 p
(Avicel)
crosslinked carboxymethyl2.00 4.00 0.00 0
cellulose (AcDiSol)
crosslinked polyvinyl 0.00 0.00 0.00 4
pyrrolidone (Kollidon
CL)
E~~s 0.20 1.95 1.95 1.95
Brighteners 0.30 0.30 0.30 0.30
NOES 3.75 3.00 3.00 3.00
Perborate 3.50 0.00 0.00 0.00
Percarbonate 0.00 3.00 3.00 3.00
Perfume 0.06 0.08 0.08 0.08
S~ 0.7 0.7 0.7 0.7
CA 02318511 2000-07-07
WO 99/36493 PCTNS98/00587
27
Example 6
In this process example the surfactant system is changed to either a
mixture of Na and K surfactants or only K surfactants. All other steps are
same
as Example 5.
s Compositions E though H shown below are made according to Example 6.
In addition, citric acid rxzonohydrate is added in compositions G and H.
Composition E F G H
NalAS 11.00 0.00 22.00 0.00
KLAS 11.00 22.00 0.00 22.00
NaC".,sAS 4.00 0.00 4.00 4.00
KC,,~,SAS 0.00 4.00 0.00 0.00
25E9 3.50 3.50 3.00 3.00
Cationics 1.20 1.20 1.20 1.20
NaSKS-6 8.00 6.00 5.00 5.00
Zeolite A 11.00 11.00 10.00 10.00
Silicate 12.50 12.50 10.00 10.00
14.00 14.00 14.00 14.00
Carbonate 11.00 11.00 13.00 13.00
crosslinked 3.00 3.00 3.00 3.00
carboxymethyl
cellulose (AcDiSol)
citric acid 0.00 0.00 3.00 3.00
monohydrate
Enrymes 2.00 2.00 2.00 2.00
Brighteners 0.30 0.30 0.30 0.30
NOBS 3.00 3.00 3.00 3.00
Perborate 3.00 0.00 0.00 0.00
CA 02318511 2000-07-07
WO 99136493 PCT/US98100587
28
Percarbonate 0.00 3.00 3.00 3.00
SRA 0.70 0.70 0.70 0.70
Perfume 0.08 0.08 0.08 0.08
Example 7
200 kglhr of linear alkyl benzene sulfonic acid (96% active) is dispersed by
the tools of a CB 30 mixer (Lodige~ CB mixer) along with 360 kglhr of STPP,
200 kg/hr of ground sodium carbonate or light soda ash, and 10-100 kglhr of a
water-insoluble disintegrant such as microcrystalline cellulose, crosslinked-
carboxymethyl cellulose or crosslinked polyvinyl pyrrolidone. This action
impregnates the water-insoluble disintegrant within the mixture. 10-20 kglhr
of
cationic solution (40% active) is also dispersed thereto. In compositions 10
8~ 11,
~o dried flakes of Na C,2-C,BAS andlor AE3S is added along with the builders
and
carbonate. The suffonic acid is neutralized in this step with the carbonate.
The
partially agglomerated mixture from the CB 30 mixer is fed into a KM 600 mixer
(Lodige~ KM mixer) for further agglomeration. In this step 40-100 kg/hr of
Zeolite A is added as a flow aid. Mean residence time in this mixer is 3-6
~s minutes and the mixer speed is 100-150 rpm. The agglomerate mixture is then
cooled in a fluid bed cooler and fines are stripped off in this step and
recycled to
the CB 30 mixer. Other performance ingredients such as enzymes, brighteners,
NOBS, perborate, CMC, DTPA, perfume and soil release agents are dry blended
with the agglomerate.
2o Compositions I through K shown below are made according to Example 7.
CA 02318511 2000-07-07
WO 99136493 PCTNS98/00587
29
Composition 1 J K
NaI.AS 20.00 20.00 3.50
AE3S 0.00 1.00 1.00
NaC,2-C,eAS 0.00 0.00 20.00
25E9 1.20 1.20 0.00
Cationics 0.30 0.60 0.60
STPP 30.00 36.00 25.00
Zeolite A 0.00 6.00 5.00
Silicate 5.00 4.00 6.00
~
acrylic acid polymer 1.00 0.00 0.00
MAIAA 0.00 0.90 1.00
polyethylene amine 0.30 0.00 0.00
Carbonate 10.00 16.00 25.00
Sulfate 25.00 0.00 0.00
microcrystalline 0.00 3.00 0.00
oelluiose(Avicel)
crosslinked carboxymethyl3.00 0.00 0.00
cellulose (AcDiSol)
crossfinked polyvinyl 0.00 0.00 2.00
pyrrolidone (Kollidon
CL)
Eniyrr~es 1.05 1.00 0.30
Brighteners 0.40 0.40 0.20
NOBS 0.00 2.00 2.00
Perborate 0.00 2.50 2.50
CMC 0.40 0.40 0.40
DTPA 0.00 0.90 0.90
Perfume 0.25 0.25 0.50
CA 02318511 2000-07-07
WO 99136493 PCTNS98/00587
SRA 0.00 0.20 0.20
Example 8
Nonionic surfactant such as C25AE5 (180 kglhr) and glucose amide paste
(85 kglhr) are dispersed by the tools of a CB 30 mixer (Lodige~ CB mixer)
along
s with 400 kg/hr of Zeolite A, 80 kglhr of ground sodium carbonate or light
soda
ash, and 100 kglhr of a water-insoluble disintegrant (such as microcrystalline
cellulose, crosslinked carboxymethyl cellulose or crosslinked polyvinyl
pyrrolidone). The partially agglomerated mixture from the CB 30 mixer is fed
into
a KM 600 mixer (Lodige~ KM mixer) for further agglomeration. In this step 100
~o kg/hr of Zeolite A is added as flow aid. The agglomerate mixture is then
cooled
in a fluid bed cooler where fines are stripped off in this step to be recycled
into
the CB 30 mixer. This nonionic agglomerate can be used as an intermediate
product to be dry added to other agglomerates or granules containing other
surfactants, builders etc. Composition L is an example of this approach.
~s Alternatively, this agglomerate can be mixed with other performance
ingredients
like enzymes, brighteners, NOBS, perborate, CMC, DTPA, perfume and soil
release agents to make the finished product. Composition M is an example of
this.
Compositions L and M are shown below are made according to Example
20 8, described above. The nonionic agglomerate of Compositions L and M
contain
the following, by weight of the nonionic agglomerate:
C25AE5 18.00
Glucose Amide 6.00
Zeolite A 50.00
25 Carbonate 8.00
AcDiSol (water-insoluble disintegrant) 10.00
Moisture 4.00
Miscellaneous 4.00
CA 02318511 2000-07-07
WO 99/36493 PCTNS98100587
31
Composition L M
NaLAS 1.00 0.00
s NaAE3S 2.00 0.00
NaAS 7.00 0.00
Nonionic agglomerate 20.00 80.00
Sulfate 6.00 0.00
NaSKS-6 11.00 0.00
~o Zeolite A ~ 11.00 0.00
Carbonate 7.00 10.00
Citric acid monohydrate 3.00 0.00
Polycarboxylate 3.00 0.00
Percarbonate 18.00 3.00
~s TAED 5.00 0.00
NOBS 0.00 3.00
Enzymes 1.00 1.00
Brighteners 0.25 0.30
0.20 0.30
2o CMC 0.35 0.00
Suds Suppresser 0.35 0.00
Perfume 0.45 0.10
Moisture 3.40 2.00