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Патент USA US3075932

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3,075,922
United States Patent 0 ”
Patented Jan. 29, 1953
l
2
commercial heavy-duty detergents in powder form, par-'
.
3,075,922
PREPARATION OF LIQUID DETERGENT
COMPUSITIONS
Harold Eugene Wixon, Jersey City, N.J., assignor to
ticularly with respect to soil redeposition power.
In the formulation of such product, the ingredients
should be selected and proportioned in accordance with
Colgate-Palmolive Company, New York, N.Y., a cor
the described method so as to form a suspension having
poration of Delaware
the foregoing qualities. As indicated the suspension is
pourable and is free-?owing upon light shaking of the
.
No Drawing. Filed Aug. 1, 1957, Ser. No. 675,562
6 Claims. (Cl. 252—138)
container at room temperature. The viscosity of the sus
pension may be varied accordingly but the product should
The present invention relates to the preparation of a 10 have an apparent viscosity from about 50 to about 7,000
centipoises, and preferably about 500 to about 6,000 cen
mixture of a water-soluble carboxyalkylcellulose salt and
tipoises for optimum results. The above references to
a water-soluble polyphosphate salt, as hereinafter de
viscosity and any others set forth in this application are
scribed and claimed.
determined by a Brook?eld viscometer, Model HAF,
The present application is a continuation-in—part of 15 using a No. 1, 2 or 3 spindle (depending upon the vis
abandoned applications Serial No. 532,734 and 532,735,
cosity) at '10 rpm. and at room temperature, i.e. 20°_
heavy-duty detergent liquid composition comprising ‘a
?led September 6, 1955, ‘and Serial No. 581,299, ?led
April 30, 1956.
C. vThe suspension may be employed in any suitable
In the detergent art, it is known to prepare detergent
compositions in powdered form, such as obtained by the
spray-drying of a slurry of a detergent composition.
These powdered products may comprise an organic de
tergent, and inorganic salts such as sodium tripolyphos
plastic in the form of bottles, cans, drums or bags.
phate, pyrophosphate, sulfate and silicate, etc. Various
organic materials including sodium carboxymethylcellu
lose have been incorporated also.
container or packaging material such as metal, glass or
The proportions of the materials in the ?nal product
are variable to some degree.
The amount of the car
iboxyalkylcellulose salt is a minor proportion such as
about 0.2 to 5 parts, and preferably about 0.5 to 3 parts
‘by weight and the polyphosphate content will be about 5
to 45 parts, and preferably about 10 to 30 parts, by
weight of the composition as formulated. The organic
The preparation of a detergent composition in the form t detergent is about 5 to 30 parts, and preferably about
of a stable, homogeneous liquid suspension comprising
10 to 25 parts, by weight. The above proportions are
polyphosphate salts and carboxyalkylcellulose salt involves
vbased upon 100 parts by weight of the ?nished formu
particular consideration of variances in manufacturing 30 lation. In general, the ratio of ‘organic detergent to poly
procedure in conjunction with the nature of the ingredi
:phosphate salt will be, from about 0.1 to 2 parts deter
ents so as to obtain optimum results. For example, the
gent to about 1 part of polyphosphate salt.
admixture of sodium carboxymethylcellulose powder with
substantial amounts of polyphosphate salts to form a con
centrated aqueous system may result in a marked tend
ency for instability of the product. This incompatibility
The ‘solids content is from about 15 to 75 parts, and
preferably about 30 to 60 parts, whereas the aqueous
35 liquid suspending medium or solvent is about 25 to 85
7 parts, and preferably about 40 to 70 parts by weight of
may be evidenced by the formation of two or more im
100 parts of the formulation. It is preferred that water
miscible phases such as by the precipitation or separa
is the liquid medium, particularly where the solids con
tion of the carboxymethylcellulose from solution or ‘by a
tent is from about 15 to ‘60 parts of the ?nal product.
tendency for the settling of the phosphate salts as a hard 40 Where a higher solids content is desired such as up to
cake in the bottom of the container.
75 parts, it may be advantageous to reduce or modify
In accordance with the present invention, it has been
found that a heavy-duty liquid detergent composition may
be prepared in the form of a pourable, substantially ho
mogeneous and stable suspension by a method of prepa
ration embodying a particular sequence of operations de
pendent upon the character of the ingredients and form
of the composition as herein described. More particu
larly, the present invention relates to the preparation of
a stable, homogeneous, pourable, liquid suspension com
prising forming a solution of said water-soluble carboxy
alkylcellulose salt in water, admixing therewith water
soluble inorganic polyphosphate salt with agitation to
form a homogeneous solution comprising said carboxy
alkylcellulose salt, polyphosphate salt and water, and
mixing the same with a water-soluble organic detergent
with agitation to form a homogeneous suspension.
Such product exhibits many desirable characteristics in
cluding, particularly, maximum stability of the suspen
sion without the formation of immiscible liquid phases
or of a precipitate over long periods of time. The liquid
detergent composition retains its attractive appearance as
' a pourable, substantially homogeneous opaque suspension
. upon aging. The composition may be prepared in such
stable form without the necessity‘ for hydrotropic com
, pounds or special suspending agents by use of the instant
manufacturing procedure and selected ingredients.
This suspension is of relatively high solids content and
the viscosity of 'a given formula by adding to the water
a minor amount of a compatible organic solvent. Exam
iples of suitable water-miscible solvent materials are a
lower aliphatic monohydric alcohol (e.g. ethanol or iso
propanol) and urea which may be employed in an amount
less than about 15 parts and preferably not in excess of
_ about 5 ,parts by weight of the product.
As indicated, it is an essential ‘element of the present
invention to form a homogeneous solution by the‘admix
ture of the polyphosphate salt with an aqueous solution
of the carboxyalkylcellulose salt. The obtention of this
type of composition is dependent in part upon the initial
r formation and use of an aqueous solution of the carboxy
alkylcellulose salt.
'
The water-soluble carboxyalkylcellulose salt is pref
erablythe alkali metal carboxy lower alkyl cellulose salts
such as the sodium and potassium salts of carboxymethyl
cellulose. Such materials are available usually in the
'form'of a powder, having a few percent (e.g. 5%)gof
moisture, in‘ various grades of purity and viscosity in s'olu
,tion. ‘The commercial grades of sodium carboxymethyl
cellulosehaving a purity from about 60% and up'to
65,1100% on a dry basis and which‘ are of low, medium or
high viscosity may be employed if desired. It is preferred
to employ such salts having a viscosity of about 20 to
1,000 centipoises in a 2%"concentration in water. The
degree of substitution of the carboxymethyl group per
may be utilized conveniently by the consumer by the ad
anhydroglucose unit in the cellulose molecule is variable
" dition of small portions of the liquid to a laundering bath 70 but is usually about 0.5 to 2, preferably up to 125 sub
or the like. In‘ general, the composition exhibits a wash
ing power during laundering that is comparable to the
titution.
,
“i
The sodium carboxymethylcellulose' or! the like“ is
3,075,922
utilized in the present‘ invention in the form of an aqueous
solution. The carboxyalkylcellulose particles should be
dispersed thoroughly. in the water ‘in order to form a
uniform colloidal dispersion.
4
pended ‘as discrete'particles. It is'clear that the-forma
tion of stable gel-like solutions is dependent in large meas
ure upon the type of ingredients and the order or parti
cular sequence for admixture.
The preparation of this
F
The water-soluble polyphosphate sa'lts may be con
sidered as'derived from orthophosphoric acid or the like
carboxyalkylcellulose salt solution in the absence of the
polyphosphate permits adequate'swelling and hydration
by theremoval of water though they may be formed
of the cellulosic material. More’particula'rly, the cellu
losic salt in particulate form should be added slowly to
byany suitable means of manufacture.
These water
soluble molecularly dehydrated or condensed phosphate
salts are known in the art and comprise the alkali metal,
ammonium, alkylamine --and alkylolamine salts of tri
the water with e?icient stirring to form a homogeneous
and substantially colorless solution without lumps or the
like. This solution is poura-ble at room temperature and
polyphosphoric, pyrophosphoric and tetraphosphoric acids,
has usually a viscosity of about 50 to 6,000‘centipoises,
and the like. "It is preierred to use a potassium polyphos
preferably at least about 100 centipoises at room tempera
phate salt in view of its generally greater solubility in
ture at the time of preparation. The amount of water
is variable and the indicated proportion of about 0.2'to 15 water‘as compared to the corresponding sodium salt.
More ‘particularly, potassium pyrophosphate or a com
5 parts of the cellulosic salt is admixed with any desired
bination in any suitable proportions of potassium pyro
proportion of the water, usually at least 5 parts water,
phosphate and sodium tripolyphosphate hexahydrate
which is su?icient to obtain the desired solution with
(Naspsoro ' 5H'2o)
the indicated processing'conditions. In general, the use
of'increasing amounts of the cellulose salt will require 20 results in optimum effects generally. Other ‘suitable mate
greater amounts of water and it is most ef?cient'to
rials which‘may be incorporated-are potassium tripoly
operate with solution of less than about 15% ‘concentra
phosphate, sodium tripolyphosphate and tetrasodiurn
tion by weight, preferably from about 0.1 to 10%v con
pyrophosphate-in suitable admixture. An example thereof
centration.
’
a
isamixture of sodium and potassium poly/phosphates
25
_After the ‘preparation of the car-boxymethylcellulose
in a ratio from about 5:1 to about 2:1 by weight. These
solution, the polyphosphate salt is admixed with the'car
various polyphosphate‘materials may be utilized in pure
boxyalkylcellulose to form a pourable, smooth, homo
or in commercial. form ‘which may contain minor amounts
geneous, gel-like solution or'dispersion. In the resulting
of other phosphate materials provided the same dolnot
solution, the polyphosphat‘e salt is dissolved 'or ?nely
adversely affect the desired product.
dispersed in the colloidal‘dispersion'of the carboxyalkyl 30 substantially
The mixedsolution of cellulose and polyphosphate may
cellulose salt depending upon the solubility‘and propor
‘be utilized in'the'manufacture ‘of detergent compositions
tion'of the polyphosphate. It is highly‘stable ‘with no ‘ob
or‘Tm-ayfbe employeddirectly for-washing and‘ cleansing
servable separation over long periods of time. The poly
purposes. ‘More particularly, it may be admixed with
phosphate salt may ‘be incorporated in any‘suitable form
suitable organic detergents and additional water, if de
such as in the form of a dry powder or in [the form of any
sired, to form a stable, heavy-duty liquid detersive sus
convenient solution or dispersion in water depending ‘upon
pension. The organic-detergent is preferably a sulfo
the'speci?c polyphosphate salt. The temperature of the
‘nated detergent whichris-selected from the group con
admixture isv not critical and the ingredients maybe
sisting of the water-soluble‘ anionic organic sulfate‘ and
mixed at room temperature ‘or ‘at lower or higher‘ tem
'sulfonate ‘detergents; though water-soluble non-ionic-or
such
as
up
to
about
160°
F.
In
the‘manu
_ peratures
'ganic detergents may be incorporated also. These mate
facture of the ‘mixed solution, requisite care should be
rials are-known and have su?icient- water solubility or dis
taken to insure the formation of a uniform‘ system since
persibility to. form foaming and detersive aqueous solu
the polyphosphate salt has a tendency to" ‘salt-‘out the ‘car
tions in the concentrations which are‘suitable for‘ use, e.g.
boxyrnethyloellulose salt from solution. The polyphos
inwashing dishes, laundry and the like. They may be
phate salt should be added slowly with etlicient sti'rring'o'r
mixing action to'prevent separation‘or'the‘formation,
45 'used- individually or in any - desired combination.
of an undesirable precipitate. Such mixing operation‘ will
vary in degree dependent upon the‘ size'rof thebatch, type
of stirrer, etc., but is a’ readily ob'servable‘and determin
~A suitable synthetic detergent is a water-soluble higher
alkyl ar‘yl‘vsulfonate detergent, particularly those having
‘about '8 to 15 carbon-atoms in the alkyl group.
It is pre
ferred/to use-the higher alkyl benzene sulfonate detergent
50 for optimum, effects, though other similar detergents hav
' able state.
This homogeneous ‘solution of ‘the'carboxyalkylcellulo‘se
ing‘a mononuclear 'aryl-nucleus, such as- toluene, xylene,
salt and ‘polyphosphate ' salt ‘ may ‘contain ‘a “variable
or’ phenol, may belused also. ‘The higherlalkyl-substitu
amount of ‘water proportioned ‘so as to ‘achieve the de
‘ent‘on the aromatic nucleus maybe branched or straight
sired state. 1In general, the water conteiitfwill' be iii-om
chained-in structure; examples of such group beingnonyl,
‘about 5 to ‘85' parts by weight and preferably v'10 to 70 55 . decyl, keryl, and tetradecyl and pentadecyl groups derived,
parts, since either a desired proportion'yor "the total
from polymers of lower mono-ole?ns, and the like.
amount of water which is present in the ‘?nal product
Examples-of- suitable. aliphatic detergents are the nor
may be incorporated at this stage of 'the' process. It ‘is
preferred to add a portion of‘ the water later ‘when’ the
organic detergent is added toiorin‘the‘susp'ension. 'As
indicated,‘ the’ carboxyalkyl‘c‘ellul'ose will‘ 'be‘ present ‘in' an
0.2 ‘to 5 parts
and’ the polyphosphate'
from
‘amount from
.
.,
.
‘aboutJS to 45 parts ‘by weight. This mixed solution" is
usuallyturbid and of variable viscosity. ‘It has a'visco'sity
usuallylfrom about 50 to 6,000’ centipoi'ses, preferably
from about 100' to 4,000 centipoises, dependingupori ‘the
--__amount of water present and the. proportions of the other
ingredients.
“HAS indicative of the signi?cance’ ofidefscribed' sequence
mal and secondary higher alkyl ‘sulfate detergents, partic
ularly those IhavingYAabout'S to 15 carbons in the fatty al
60 coho‘l residue,‘ such 'as lauryl ‘(or ‘coconut fatty‘ alcohol)
‘sulfate. Otherisuitabledetergents'are the sulfuric-acid‘
1'esters of polyhydric alcohols incompletely esteri?ed with
“higher fatty‘ acids,’*e.g.r coconut oil monoglycerideT mono»
sulfateythe higher fatty‘ acid-e‘sters of low molecular
65 weight‘ alkylol‘ sulfonic- acids, e.g. oleic acid ‘ester of
- isethionic acid; the higher fatty acid (e.g. coconut) ethan
v'olamide sulfate; the higher fatty‘ acid ‘amide of amino
" alkyl sulfonic‘acids, e.g. lauric acid-amide of :taurine; and
like.
of steps for obtention of this solution, it has been found 70 theThese‘fsulfate
and sulfonate detergents are used in the
vithat,‘ if the carboxyalkylcellulose salt in the form of ' a
‘formjoftheirwaterjsoluble
salts; such as the alkali metal
dry powder is added with‘ agitation to- a suspension or
and
"nitrog'enlcontaining,
e.g.
lower alkylolamine,‘ salts.
solution of the polyphosphate’ salt in water,‘ there does
.uetresult the‘ desired state but rather (the product vtends
to form two phases with the carboxyalkylcellulose 'sus
‘Examples ‘are'the sodium, potassium; ammonium,‘ i‘soprop
anolamine, " mono- and‘ tri-“ethanolaniine‘ "salts ' of said
5
3,075,922
higher alkyl benzene sulfonate, higher alkyl sulfate and
the like. In commercial practice, it is preferred to use
the alkali metal salts.
Examples of suitable nonionic detergents are the water
soluble non-ionic polyalkylene oxide detergents. In gen
eral, these detergents are the products produced by the
6
water, since the presence of Water is not critical but facili
tates the mixing of the ingredients. The detergent solution
is preferably warmed, e.g. about 150° B, so that any ad
ditional ingredients to be added which are'of limited
water-solubility, such as lauric isopropanolamide, are pres
ent in molten form. It is preferred that the organic de
introduction of a controlled number of alkylene oxide
tergent solution be a concentrated solution, such as of the
groups into an organic hydrophobic compound or group,
order of a 20 to 75% organic detergent by weight.
usually of an aliphatic or aromatic structure. The hydro
The initial carboxyalkylcellulose-phosphate salt solution
phobic organic group contains usually at least about 8 10 is then admixed slowly with the detergent with e?icient
carbons, and preferably up to 30 carbons, condensed with
stirring at room temperature (or at elevated temperature
at least about 5 and usually up to about 50 alkylene oxide
if desired) to form a homogeneous and uniform liquid
groups.
It is preferred to use the polyoxyethylene con
opaque suspension. The viscosity of the suspension may
densates derived from ethylene oxide, although other
be varied as indicated by control of the proportions of
lower alkylene oxides such as propylene oxide, butylene 15 the ingredients. The initial mixed solution may be added
oxide and the like have generally similar properties and
to the detergent solution or the reverse order may be em
may be substituted therefor.
Among the non-ionic detergents, it is preferred to use
the polyakylene oxide condensates of alkyl phenol, such
as the polyoxyethylene ethers of alkyl phenols having an
alkyl group of at least about 6, and usually about 8 to 12
carbons, and an ethylene oxide ratio (number of moles
per phenol) of about 7, 9, 12 and 20, though the number
of ethylene oxide groups will be usually from about 8
ployed as desired.
Various other ingredients may be added as desired in
cluding compatible perfumes, coloring materials, corrosion
or tarnish inhibitors, germicides, bleaching agents, optical
bleaches or ?uorescent dyes and the like. Other phos
phate materials or builder salts may be included in the
‘product provided that they do not substantially adversely
affect the desired results. The physical characteristics of
to 18. The alkyl substituent on the aromatic nucleus 2.5 the product may be modi?ed in degree by the incorpora
may be diisobutylene, diamyl, polymerized propylene, di
tion of various compatible materials as desired to modify
merized CrC7 ole?n, and the like.
7
or adjust the viscosity or other characteristics of a given
Further suitable detergents are the polyoxyalkylene
formula. Suitable examples are small amounts of waxes
esters of organic acids, such as the higher fatty acids, rosin
(e.g. castor wax) and colloidal materials such as bentonite
acids, tall oil acids, or acids from the oxidation of petro 30 and similar clays.
leum, etc. These polyglycol esters will contain usually
The following examples are additionally illustrative of
from about 12 to about 30 moles of ethylene oxide or its
the nature of the invention and it will be understood that
equivalent and about 8 to 22 carbons in the acyl group.
the invention is not limited thereto. All parts are by
Suitable products are re?ned tall oil acids condensed
weight unless otherwise speci?ed.
'
with 16 or 20 ethylene oxide groups, or similar polyglycol 35
Examples I-III
esters, of lauric, stearic, oleic acids, etc.
Additional non-ionic agents are the polyalkylene oxide
condensates with higher fatty acid amides, such as the
I
II
III
higher fatty acid primary amides, mono- and diethanol
amides. Suitable agents are coconut fatty acid amide 40
condensed with about 10 to 50 moles of ethylene oxide.
The fatty acyl group will have about 8 to 22 carbons,
and usually about 10 to 18 carbon atoms, in such prod
Part A:
.
Sodium carboxymethylcellulose _________ _.
Water __________________________________ __
Part B:
P tEllejtrapotassium pyrophosphate _________ __
or
:
.
1.00
30. 00
1.00
30. 00
20.00
20.00
1.00
30. 00
10.00
ucts. The corresponding polyalkylene oxide condensates
of higher fatty acid sulfonamides maybe used also if de
Sodium dOdecyl benzene sulfonate ______ __
Lauric-myristic isopropanolamide (1:1)-..
Color ___________________________________ _-
1.00
1.00
1.00
sired.
Water __________________________________ _.
31.10
30. 10
41. 10
100. 00
100. O0
100. 00
Other suitable polyether non-ionic detergents are the
polyalkylene oxide ethers of higher aliphatic alcohols.
Suitable fatty alcohols having a hydrophobic character,
preferably 8 to 22 carbons, are lauryl, myristyl, cetyl,
stearyl and oleyl alcohols which may be condensed with
an appropriate amount of ethylene oxide, such as at least
about 6 and preferably about 10 to 30‘ moles. A typical
product is oleyl alcohol condensed with about 12, 15 or
11. 90
17. 90
5.00 ______ __
11.90
5. 00
These suspensions are prepared in the following man
ner: As Part A, the carboxymethylcellulose powder (66%
pure) is mixed with the water slowly with stirring to form
a ?uid gel-like solution having a viscosity of 136 centi
poises. The pyrophosphate of Part B in powder form is
added to the carboxymethylcellulose solution at room
20 moles of ethylene oxide. The corresponding higher 55 temperature. This phosphate salt is added slowly in in~
alkyl mercaptansor thioalcohols condensed with ethylene
crements over a period of about 10 minutes, with stirring
oxide are suitable in the present invention also.
The
of the carboxymethylcellulose solution to form a homo
water-soluble polyoxyethylene condensates with hydro
geneous solution gel having a viscosity of about 2,500
phobic polyoxypropylene glycols may be employed also.
centipoises.
Further suitable non-ionic detersive-type materials 60 The ingredients in Part C are then mixed together to
which may be added are the higher fatty acid alkanol
form a uniform homogeneous mixture.
amides, such as the monoethanolamides, diethanolamides
and isopropanolamides wherein the acyl radical has about
benzene snlfonate detergent in powder form (84% pure)
The dodecyl
is dissolved in the Water (with color added) ‘and heated to
150° F. The isopropanolamide in Examples I and III is
acid, lauric, capric and myristic diethanolamides, and the 65 melted and then slowly added to the detergent solutions
10 to 14 carbon atoms.
Examples are coconut fatty
corresponding monoethanolamides and isopropanolam
with stirring to form a uniform mixture which is a mobile
ides. These alkanolamide materials tend generally to
gel having a viscosity of about 13,000 centipoises. The
improve the foaming power and detergency of the deter
Part C of Example II which does not have the amide is a
gent compositions and may be solubilized in the liquid.
solution.
The organic detergent is admixed with the carboxyalkyl 70 The initial gel-like mixture of carboxymethylcellulose
cellulose-polyphosphate solution in any suitable manner
and polyphosphate are then ‘added to the detergent mix
to form the ?nal liquid product. The organic detergent
tures of Part C with stirring at room temperature to form
may be added as a dry powder but it is preferred to employ
an aqueous solution of the detergent (including a suspen
a uniform and homogenerous liquid suspension.
The
viscosity of the ?nal product is about 1,150 centipoises
sion, gel, dispersion or slurry of the organic detergent in 75 for Example I, 768 centipoises for Example II and 2,016
3,075,922
hate having 8 to 15 carbons in the alkyl group, the pro
centipoises for ‘Example III. 'Ihese suspensions have‘been
portions thereof being 0.2 to 3 parts of said cellulose salt,
found to be extremely stable ‘with no signi?cant separa
10 to 30 parts of said pyrophosphate, 5 to 30 parts of
tion after many weeks of storage. They are markedly
said alkyl benzene sulfonate and the balance being pri
superior in stability to similar suspensions which do not
contain, carboxymethylcellulose or in which the carboxy 5. marily water based upon 100 parts by weight of the formu
lation and sui?cient to form a substantially stable and
methylcellulose was added in powder form to a polyphos
homogeneous, pourable liquid.
phate solution.
2. A liquid detergent composition prepared by the
Examples lV-Vl
IV
V
VI
process of claim 1.
1g
3. A process for preparing a detergent composition in
the form of a substantially stable and homogeneous, pour
able liquid which comprises preparing an aqueous solu
Part A:
Sodium carboxymethylcellulose _________ __
Water __________________________________ __
1. 35
14. 95
-
0. 90
13. 56
1. 36
13. 11
tion of an alkali metal carboxy lower alkyl cellulose salt
in a concentration from about 0.1 to 15% by weight,
Sodium tripolyphosphate hexahydratm _ _ _ ______ _ _
22. 6O
13. 56
Water __________________________________ __
13. 56
20. 80
15 subsequently adding a water-soluble inorganic polyphos
phate salt selected from the group consisting of sodium
and potassium pyrophosphate and tripolyphosphate in par
______________ ..
ticulate form and aqueous solutions thereof slowly and
with agitation to said cellulose solution to form a ‘pour
Part B:
Tetrapotassium pyrophosphate _________ -_
19.93
14. 95
______ _.
4. 52
Part 0:
Sodium dodecyl benzene snltonate (dry
powder 85% pure) ____________________ _-
11.46
Sodium dodecyl benzene sulr‘onate (48.5%
18. 63
18. 63
20 able, homogeneous liquid, and thereafter admixing said
Lauric-myristie isopropanolamide (l: 1) _ __
4. 98
4. 52
4. 52
Color ___________________________________ __
Water __________________________________ -_
l. 00
31. 38
0. 90
25. 33
0. 90
22.60
cellulose-polyphosphate solution with a water-soluble
aqueous slurry) _______________________________ _ .
higher alkyl benzene sulfonate detergent having about 8
to 15 carbons in the alkyl group, the proportions thereof
being 0.2 to 5 parts of said cellulose salt, 5 to 45 parts of
Viscosity, c.p ............................... ._ 1, 408
4, 000
1,184 25 said polyphosphate, 5 to 30 parts of ‘said sulfonated de
tergent, and the balance being primarily water based upon
These suspensions are prepared by the same procedure
100 parts by weight of the formulation and sufficient to
as in Examples I to III. Part B is prepared by adding
form a substantially stable and homogeneous, pourable
the phosphate salt slowly to the water with stirring. In
liquid.
Formula IV the phosphate salt is dissolved to form a 30
4. A process in accordance with claim 3 wherein said
solution and in Formulas V and VI the phosphate salts
polyphosphate is potassium pyrophosphate and said sul
are dispersed to form a suspension. The Part B products
fonated detergent is an alkali metal‘ higher alkyl benzene
are added slowly to the Part A solution with, strong mix
sulfonate.
ing action at room temperature as described to form the
5. A process in accordance with claim 3' wherein said
100. 00
100. 00
100. 00
desired homogeneous gel-like solution.
35 polyphosphate is sodium tripolyphosphate hexahydrate
The ingredients of Part C are mixed similarly to form
a uniform homogeneous mixture. The initial gel-like solu
tions comprising the carboxymethylcellulose and phos
and said sulfonated detergent is an alkali metal higher
alkyl benezene vsnlfonate.
6. A ‘liquid detergent composition prepared ‘by the
phate are then added to the liquid gel-like mixtures of
process of claim 3.
Part C with stirring at room temperature which results 40
References ‘Cited in the ?le of this‘patent
in the formation of a uniform and homogeneous liquid
suspension. These suspensions have been found to be
UNITED STATES PATENTS
extremely stable also.
Although the present invention has been described and
2,486,921
Byerly ____, ____________ __ Nov; 1, 1949
illustrated with a reference to speci?c examples, it is un 45 2,560,839
vAyo _________________ __ July 17, 1951
derstood that modi?cations and variations of composition
and procedure are contemplated within the scope of the
appended claims.
Having thus described the invention, what is claimed is:
1. A processfor preparing a detergent composition 50
in the form of a substantially stable. and homogeneous,
FOREIGN PATENTS
650,222
678,445
688,754
716,517
Great
Great
Great
Great
Britain _________ __ Feb. 21,
Britain __________ __ Sept. 3,
Britain _________ __ Mar. 11,
Britain __________ __ Oct. 6,
1951
1952
1953
1954
pourable liquid which comprises preparing an aqueous so
OTHER REFERENCES
lution of sodium carboxymethylcellulose in a concentra
tion from about 0.1 to 10% by weight, subsequently add
ing a polyphosphate selected from the group consisting
Trexler: “Phosphates,” Soap and Sanitary Chemicals,
July 1950, pp.,39—41 and 82.
Hercules CMC, Cellulose Gum, Properties and Uses of
of potassium pyrophosphate in particulate form and
aqueous solutions thereof slowly and with agitation to
Copyright 1951 by Hercules Powder Co., 20 pages.
.lVIonsanto TechnicalBulletin No. P5139, “Sodium Tri
polyphosphate,” Monsanto Chem. C0,, St. Louis, July 8,
liquid, and thereafter admixing said oellulose-pyrophos
phate solution with an alkali metal alkyl benzene 'sulfo 50 21949,, 5 pp.
said cellulose solution to ‘form a pourable, homogeneous
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