Note: Descriptions are shown in the official language in which they were submitted.
~ 32~7~
PROCESS FOR MAKING CONCENTRATED SURFACTANT GRANULES
Daniel L. Strauss
Charles L. Stearns
Thomas E. Lobaugh
FIELD OF INVENTION
The present invention relates to a process for preparing
concentrated ~condensed) surfactant granules.
BACKGROUND OF THE INVENTION
Granular surfactant compositions are principally prepared by
spray or drum drying. In the spray drying process the surfactant
components, plus perhaps salts and builders, are mixed with as
much as 35-50% waker to form a slurry. The slurry obtained is
heated and spray dried9 which is expensive~
Such spray drying requires 30-40 wt.% of the water to be
removed. The spray drying equipment used is expensive. The
granule obtained has good solubility but a low bulk density, so
the packing volume is large. Th~ particles also may be sticky,
particularly when hot, and thus wall buildup is an additional
problem. There are other known disadYantages in preparing gran-
ular materials by spray drying, such as environmental concerns and
heat sensitivity. An agglomeration process, on the other hand,
would be cleaner, as well as less expensive, both in terms of
equipment and operat~ng costs.
Ther~ are many prior art nonspray-drying processes which
produce surfactant granule~. Most, howaver, require mixing of the
surfactant with other materials such as inorganic salts or alumi-
nosilicate-type materials. Some other processes require use of an
acid form of the surfactan~ to work. In most cases, a diluted
surfac~ant particle is obtalned. The major problem with the use
of a high active surfaotant paste as a starting material in a one
step granulation process is its stickiness.
In U.S. Pat. No. 4,515,707, Brooks, issued May 7, 1985;
Japanese laid-open Appln. No. 183540/19B3, Kao Soap Co., Ltd.,
filed S@pt. 30, 1983; and Japanese Sho. 61-118500, Lion K.K.,
227 ~ ~
June 5, 1986, high shear and/or cold mixing processes are dis-
closed. Typically, excess carbonate is required (2-10 molar
excess) to assure reasonable conversion of the surfactant acids.
Excess carbonate adversely drives up the wash water pH to the very
alkaline range which can be undesirable, particularly for some
nil-phosphate formulas and formulas containing peracid bleaches.
Such high shear and cold mixing processes are known, but they have
drawbacks, e.g., some require an extra grinding step or some other
action, as well as the addition of other ingredients, primarily
solids. Others use a dry neutrali~ation technique for mixing the
acid form of the surfactant with sodium carbonate.
A practlcal problem with the use of a surfactant acid form is
that it requires immediate use after it is made, or cool tempera-
ture storage, for such highly reactiYe acids, such as the alkyl
sulfate acids9 are subject to degradation unless cooled. They
also tend to undergo hydrolysis during storage, forming free
sulfurie acid and alcohol. In practical terms, such prior art
processes require close coupling of surfactant acid production
with granulation which requires an additional capital investment.
~n U.S. Pat. No. 4,162,994, Ko~alchuk, issued July 31, 1~7~,
it is disclosed that calcium salts are re~uired to overcome
problems in process~ng by nonspray drying (i.e.~ mechanical) means
~ormulations based on sodium salts of anionic surfactants and
certain nonionic surfactants. A drawback to that process is that
insoluble calc~um salts can lower the solubility of the formu-
lation, which is of particular importance in stress situations,
such as in pouch-type executions.
U.S. Pat. No. 4,427,417, Porasik, issued Jan. 24, 1~84,
discloses preparing granular detergent composit;ons from hydrat-
~o abl e particul ate detergent salts, etc., under conditlons insuring
complete hydration and agglomerating them into storage stable,
dry, pourabl e agglomerates.
SUMMARY OF THE INV~NTION
The present invention relates to an economical process for
making a dense, concentrated surfactant granule from a high active
surfactant paste using fine dispersion cold granulation.
A
~ 3 2 ,~ r~
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- OBJECTS OF THE_INVENTION
An important object of the present invention is to make a
denser and more concentrated surfactant granular product by an
agglomeration process without an expensive drying step. Another
object is to provide a more concentrated surfactant granule which
can be stored and then admixed with other ingredients to provide a
final end product. Another object of the process of this inven-
tion is to provide a formulated granule containing higher total
surfactant levels than typically obtained via other means. Yet
another object of the present invention is to prepare a very high
active surfactant granule essential free of hydrated inorganic
salts. Other objects of the present invention will be apparent in
view of the following.
DETAILED DESCRIPTION OF THE INVENTIQN
The process of the present invention comprises fine dis-
persion mixing and cooling o~ a high active surfactant paste to
provide a very concentrated surfactant granllle. Most high active
surfactant pastes are too tacky at normal m;xing temperatures to
successfully granulate using fine dispersion mixing. So the high
active surfactant paste is cooled as needed to a granulation tem-
perature while mixing. Iarge discrete particles (granules) are
surprisingly formed right in the mixer. Thus "cold" granulation
of a hlgh surfactant past is achleved.
The granulation temperature, according to the present inven-
tion9 ranges from about -65-C to 25C using a critical fine
dispersion mixing tip speed of from about 5 m/sec. to about 50
m/sec. Dry ice is a preferred cooling means.
A benefit of the present invention is that the preferred
30 granules made according to the present invention are large,
essentially pure surfactant granules. They preferably have a bulk
density of from about 0.4 to about 1.1 9/CC9 more preferably from
about 0.5 to about 0.8 g/cc. The weight aYerage particle size of
the preferred particles of th~s invention are from about 200 to
about 2,000 mkrons. The more preferred granules have a particle
size range of from 300 to 1,200 microns. Yields of 25% to &5% in
these ranges can be achie~ed. A second brief mixins increases
~3~27~
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y;e!ds of granular particles in these preferred ranges. Oversized
and undersized particles can also be recycled.
The more preferred granulation temperatures of the high
active surfactant paste ranges from about -40C to about 10C, and
most preferably from about -30C to about 0C. More details of
the present invention are highlighted below.
The resultant surfactant granules made by the process of the
present invention can comprise a combination of all, or substan-
tially all, of the ingredients Qf the total composition or th~y
can be used as an intermediate. Thus, such granules greatly
reduce or even eliminate tha need to admix additional materials
for a final detergent formulation. Also, the possibility of
segregation of ingredients during shipping, handling or storage is
greatly reduced, especially if only minor quantities of other
materials of differing particle si~es or densities are to be
included.
Separately, the concentrated granule of this invention can be
admixed with detergent granules produced by more conventional
means to increase the total surfactant level in a final formu-
lation.
Methods of CoolinqLthe Hlq~!-Active Surfactant Paste
Any suitab1e method of coollng the high active surfactant
paste to a granulation temperature can be used. Cooling jackets
or coils can be integrated around or into the mixer. Chipped dry
ice or liquid CO~ can be added or ~njected into the uniform paste.
The idea is to lower the high active surfactant paste temparature
to a granulation temperature so that it can be finely dispersed or
"granulated" into discrete particles.
_ste Viscositv and Processinq
Two important parameters of the high active surfactant pastes
which can affect the parameters of ~he mixing and granulation step
of the present invention are the paste temperature and the paste
viscosity. The viscosity is a function of surfactant concen-
tration and its temperature. The high active surfactants of the
present invention have viscosities which range from about 10,000
cps to 10,000,000 cps; preferably, from about 70,000 to about
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~2~7~
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7,000,000 cps; and more preferably from about 100,000 to about
1,000,000 cps. These viscosities are measured at a temperature of
about 50'C for the present invention.
The high active surfactant paste can be introduced into the
mixer at an initial temperature in the range of about 5-70C,
preferably about 2U-30C. Higher temperatures reduce their
viscosities but a temperature greater than about 70C can lead to
poor initial mixing due to increased product stickiness.
The process of the present invention surprisingly forms
large, but usable~ granules, preferably in the 200 to 1200 micron
range. Such large granules are preferred, particularly if the
surfactant granule is to be admixed with other materials which
have a tendency to be dusty. Particles of similar size are
preferred to minimize segregation. No extra grinding step is
required or desirable. In general, larger particles are less
dusty, which is important in many consumer applications, especi-
ally those which comprise porous, unitized dose pouch-like
products. Such porous products are designed: ~1) to avoid con-
sumer contact with the product ilnd (2) to reinforce the con-
venience and nonmessiness perceptions of a unit ked pouch form.
- If desired, granules of insufficilent size can be screened after
drying and recycled to the fine di<;persion mixer.
The Fine Pisper$lQ~ ~ting and Gran~Jation
Unless otherwise specified, the terms "fine dispersion
mixing" and/or` "granulation," as used herein are synonymous and
mean mixing and granulating of a htgh active surfactant paste in a
fine dispersion mixer using a blade tip speed of from about 5
m/sec. to about 50 m/se. The total residence time of the mixing
and granulatlon process is preferably in the order of from 0.1 to
10 m1nutes, more pre~erably 0.5-8 and most preferably 1-6 minutes.
The more preferred mixing and granulation tip speeds are about
10-40 m/sec. and about 15-35 m/sec.
The Little~ord Mixer, Model #FM-130-D-12, with internal
chopping blades and the Cuisinart~ Faod Processor, Model #DCX-
Plus, with 7.75 inch (19.7 c-) blades are two examples of suitable
mixers. Any other mixer with fine dispersion mixing and granu-
lation capability and which preferably has a residence time in the
132~7~
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order of 0.1 to 10 minutes can be used. The i'turbine type"
impeller mixer, having several blades on an axis of rotation, is
preferred. The invention can be practiced as a batch or a con-
tinuous process.
The mixer must finely disperse the paste and, if desired, the
other ingredients. When the contents of the mixer are cooled, the
mixing ~ust be conducted at said fine dispersion tip speed in
order to granulate the surfactant into discrete particles. Care
must be taken not to use too low or too high of a tip speed at the
granulation step. While not being bound to a theory, ~Itoo high a
shear" is believed to prevent granulation because of a wide
variety of str~sses, e.g., a broader particle size distribution
caused by the high~r tlp speeds with a higher level of fines
generated. Also, too high of a tip speed increases the tempera-
ture of the material and additional cooling is required.
Care must be taken not to overload any fine dispersion mixer
with two much or too little surfactant paste material. If there
is more than one material the results ara poor mixing and unsat-
isfactory granulation. Thus, care must be taken to load the mixer
with a proper level of paste material so that satisfactory mixing
and granulation are achieved. Sim~lar to too low of a tip speed,
overloading the mixer results in poor dispersion, reduced uni-
formity and large lumps. On the other hand, too high of a tip
speed increases the production of undesirable fines.
The work input required for fine d;spersion mixing in the
practice of the present invention varies with: (1) the type of
fine dispersion mixer used, (2) the mixer loading level, (3) the
viscosity of the paste material, and ~4) the amount and the type
of dry solids used~ if any. E.g., the Total Work required for
mixing and granulation of several preferred paste materials using
a laboratory Cuisinart food processor, Model ~DCX-Plus varied from
about 7 BTU's to about 16 BTU's per pound of paste material. The
rorresponding I~crem~ntal Work varied from about 0.4 BTU's to
about 2.6 BTU's per pound of paste material. Tha No Load Work for
the Cuisinart food processor ~s about 0.2 BTU's per second. The
Cuisinart food processor has a single 19.7 cm flat horizontal
~227~
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propeller and is operated at 1800 rpm, which is a tip speed of
about 1~.55 m/sec.
The Total Work required to mix and granulate the surfactant
paste of the present invention can vary from about 3 BTU's to
about 30 BTU's per pound of material depending on viscosity, load,
etc. A preferred range is from about S BTU's to about 20 BTU's
per pound. These BTU ranges in kilogram of material are, respec-
tively, from about 6.6 to 66, and from about 11 to 44 BTU/Kg.
Some benefits of fine dispersion mixing and granulation
include: (1) a lower level of granulated fines; (2) a more uniform
granular particle size distribution; an~ (3) a hlgher density
granule than a granular product made with standard agglomeration-
type mixers, such as pan type mixers.
Hiqh Active Surfactant Paste
The activity of the aqueous surfactant paste is at least 50%
and can go up to about 98%; preferred activities are: 60-80% and
65-75%. The balance of the paste is primarily water but can
include a processing aid such as mineral oil. The resultant con-
centrated surfactant granules can be added to dry detergencybuilders or conventionally agglomerated with blnders with these
builders or other materials to yield desired finlshed formula
compositions.
In the process of the present invention, it is preferable to
use higher active surfactant pastes to minlmize the total water
level in the system during mixing and granulating~ The benefits
of lower water levels are to allow for (1) higher levels of other
liquids in the formula without causing stickiness; (2) less
cooling, du~ to higher granulation temperatures; and (3) less
granular drying to meet final moisture limits.
Tt is important that the mo~stur2 or solvent (hereinafter
referred to as "molsture") content of the high activ~ surfactant
should not exceed 50%. The total moisture can range from about 2%
to about 50%, but is preferably from about 10% to about 40%, and
more preferably from about 15Yo to about 30%. The lower granu-
lation temperatures are used for the higher mois~ure-containing
~L322~
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pastes. Conversely, the higher granulation temperatures can be
used for lower moisture pastes.
Paste compositions which have lower moisture contents of
below 5X~ e.g., about 1% to 4,~, can contain an effective amount of
an organic liquid solvent or processing aid. Examples of such
aids are selected from suitable organic liquid, including ~ineral
oil, glycerin, short chain alcohols, and the like, and mixtures
thereof. The processing aid preferably can be used at a level of
"0.5% to 20~," more preferably about 1-lOYo; most preferably about
2-579 by weight of the paste.
The desired moisture content of the surfactant granules of
this inYention can be adjusted by adding other deslred dry ingre-
dients prior to cooling and granulation. Thus, additional
"drying" is unnecessary in low moisture formulations. ~hen
desirable, drying the discrete granules can be accomplished in a
standard fluid bed dryer. Tha idea here is to provide a free
flowing granule with a desired moisture content of 0.5-10%,
preferably 1-5%.
lhe aqueous surfactant paste contains an organic surfactant
selected from the group consisiting of anionic, zwitterionic,
ampholytic, nonionic and cationic surfactants, and mixtures
thereof. Anionic surfactants are preferred. Surfactants useful
herein are listed ln U.S. Pat. No. 3,664,961, Norris, issued
May 23, 1972, and in U.S. Pat. No. ~919,678, Laughlin et al.,
issued Dec. 30, 1975.
Useful cationic surfactants also include those described in U.S.
: Pat. ~o. 4,222,905, Cockrell, issued Sept. 16, 19~0, and in U.S.
Pat . No . 4, 2~9, 659, Murphy, i ssued Dec ~ 16, 1980 ~
The following are representative
~0 examples of surfactants useful in the present compositions.
~ater-soluble salts of the higher fatty acids, i.e., "soaps,"
are useful anionic surfactants in ~he compositions herein. This
includ~s alkali metal soaps such as the sodium, potassium, ammo-
nium, and alkylolammonium salts of higher fatty acids containing
from about 8 to about 24 carbon atoms, and preferably from about
12 to about 18 carbon atoms~ Soaps can be made by direct saponi-
ficatio~ of fats and oils or by the neutralization of frse fatty
acids. Particularly useful are the sodium and potassium salts of
the mixtures of fatty acids derived from coconut oil and tallow,
..
.. ..
~t~
, . .
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g
i.e., sodium or potassium tallo~ and coconut soap.
Useful anionic surfactants also include the water-soluble
salts, preferably the alkali metal, ammonium and alkylolammonium
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. (Included in the term "alkyl" is the alkyl portion of acyl
groups.) Examples of this group of synthetic surfactants are the
sodium and potassium alkyl sulfates, especially those obtained by
sulfating the higher alcohols (Cg-C1g carbon atoms) such as those
produced by reducing the glycerides of tallow or coconut oil; and
the sodium and potassium alkyl benzene sulfonates in which the
alk~l group contains from about 9 to about 15 carbon atoms, in
straight or branched chain configuration, e.g., those of the type
described in U.S. Pat. Nos. 2,220,09g and 2,477,383. ~specially
valuable are linear straight ~hain alkyl benzene sulfonates in
which the average number of carbon atoms in the alkyl yroup is
from about 11 to 13, abbreviated ax Cll-C13 LAS.
Other anionic surfactants herein are the sodium alkyl glyc-
eryl ether sulfonates, espectally those ethers of higher alcohols
derived from tallow and coconut oil; sodium coconut oil fatty acid
monoglyceride sulfonates and sulfates; sodium or potassium salts
of alkyl phenol ethylene oxlde cther sulfates containing from
about 1 to about 10 units of ethylene oxide per molecule and
wherein the alkyl groups contain from about 8 to about 12 carbon
atoms; and sodium or potassium salts of alkyl ethylene oxide ether
sulfates cont~ining from about 1 to about 10 units of ethylene
oxide per molecule and wherein the alkyl group contains from about
10 to about 20 carbon atoms.
Other useful anionic surfactants herein include the water-
soluble salts of esters of alpha-sulfonated fatty acids containing
from about 6 to 20 carbon atoms in the fatty acid group and from
abnut 1 to 10 carbon atoms in the ester group; water-soluble salts
of 2-acyloxy-alkane-1-sulfonic acids containing frQm about 2 to 9
carbon atoms in the acyl group and from about 9 to about 23 carbon
atoms in the ~lkane moiety; alkyl ether sulfates containing From
about 10 to 20 carbon atoms in the alkyl group and from about 1 to
:~322~
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30 moles of ethylene oxide; water-soluble salts of olefin sulfo-
nates containing from about 12 to 24 carbon ato~s; and beta-
alkyloxy alkane sulfonates containing from about 1 to 3 carbon
atoms in the alkyl group and from about 8 to about 20 carbon atoms
in the alkane moiety.
The preferred anionic surfactant pastes are mixtures of
linear or branched alkylbenzene sulfonates having an alkyl of
10-16 carbon atoms and alkyl sulfates having an alkyl of 10-18
carbon atoms. These pastes are usually produced by reacting a
liquid organic material with sulfur trioxide to produce a sulfonic
or sulfuric acid and then neutralizing the acid to produce a salt
of that acid. The salt is the surfactant paste discussed through-
out this document. The sodium salt is preferred due to end
performance benefits and cost of NaOH vs. other neutralizing
agents, but is not required as other agents such as KOH may be
used. The neutrali~ation can be performed as part of the fine
dispersion mixing step, but preneutralization of the acid in con-
junction with the acid production is preferred.
Water-soluble nonionic surfat:tants are also useful as sur-
factant in the compositions of thle invention. Many final deter-
gent compositions include nonionics or nonionic/anionic surfactant
blends. Inclusion of nonlonics in many applications is difficult,
particularly if a spray-dry process is used, because of potential
degradat~on and environmental concerns. A nonion1c granule can
thus be admixed with a spray-dry granule to produce a preferred
~inal formulation. Such nonionic materials include compounds
produced by the condensation of alkylene oxide groups (hydrophilic
in nature) with an organic hydrophobic compound, which may b~
aliphatic or alkyl aromatic în nature. The length of the poly-
oxyalkylene group which is condensed with any particular hydro-
phobic group can be readily adJusted to yield a water-soluble
compound having the desired degree of balance between hydrophilic
and hydrophobic elements.
Suitable nonionic surfactants include th~ polyethylene oxide
condensates of alkyl phenols, e.g., the condensation products of
alkyl phenols having an alkyl group containing from about 6 to 16
carbon atoms, in either a straight chain or branched chain con-
~322~
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figuratiQn, with from about 4 to 25 moles of ethylene oxide per
mole of alkyl phenol.
Preferred nonionics are the water-soluble condensation
products of aliphatic alcohols containing from 8 to 22 carbon
atoms, in either straight chain or branched configuration, with
from 4 to 25 moles of ethylene oxide per mole of alcohol. Par-
ticularly preferred are the condensation products of alcohols
having an alkyl group containing from about 9 to 15 carbon atoms
with from about 4 to 25 moles of ethylene oxide per mole of
alcohol; and condensation products of propylene glycol with
ethylene oxide.
Semi-polar nonionic surfactants include water-soluble amine
oxides containing one alkyl moiety of from about 10 to 18 carbon
atoms and 2 moieties selected from the group consisting of alkyl
groups and hydroxyalkyl groups con$aining from 1 to about 3 carbon
atoms; water-soluble phosphine oxides containing one alkyl moiety
of about 10 to 18 carbon atoms and 2 moieties selected from the
group consisting of alkyl groups and hydroxyalkyl groups con-
taining from about 1 to 3 carbon atoms; and water-soluble sul-
foxides containing one alkyl moiety of from about 10 to 18 carbonatoms and a moiety selected from thle group consisting of alkyl and
hydroxyalkyl moietles of from about 1 to 3 carbon atoms.
Ampholytic surfactants includle derivatives of aliphatic or
aliphatic derivat~ves of heterocyclic secondary and tertiary
amines in which the aliphatlc moiety can be either straight sr
branched ohain and wherein one of the aliphatic substituents
oontains from about 8 to 18 carbon atoms and at least one ali-
phatic substituent contains an anionic water-solubilizing group.
Zwitterlonic surfactants include derivatives of aliphatic
quaternary ammonium phosphonium, and sulfonium compounds in which
one of the aliphatic substituents contains from about 8 to 18
carbon atoms.
The h~gh active surfactant paste formulation must be solid at
about room temperature unless the granules are kept cool until
mixed with other detergent solids.
The terms "LASI' and "QS" as used herein mean, respectively,
"sodium lauryl benzene sulfonate" and "alkyl sulfate." The terms
13227~
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like "C4s" mean C14 and Cls alkyl, unless otherwise specified.
Some of these AS and LAS surfactants do not require cooling if
used at about 20-25~C.
All examples used a Cuisinart food processor, Model #DCX-Plus
with 19.7 cm metal blades operating at 1800 rpm. The tip speed is
18.55 m/sec.
DeterqencY Builders
The surfactant granules of thP present invention can be made
with some detergency builder and/or inorganic, water-soluble
salts. So, the surfactant paste can contain such materials at a
ratio of salt/builder to surfactant active of from about 0:1 to
about 1:1 on a dry weight basis. Any compatible detergency
builder or combinatiQn of builders or water-soluble salts can be
used in the process to produce desired end products or inter-
mediates. However, in most cases the inclusion of such solid
material is unnecessary and not desired. The present invPntion is
aimed at mak~ng a purer, denser surfactant granule.
The granular detergents of the present invention can contain
neutral or alkaline salts which have a pH in solution of seven or
greater, and can be either organic or inorganic in nature. ~he
builder salt assists in providing the desired density and bulk to
the detergent granules herein. While some of the salts are inert,
many of them also function as detergency builder materials in the
laundering solution.
Examples of neutral water-soluble salts include the alkali
metal, ammonium or substituted a~monium chorides, fluorides and
sulfates. The alkali metal, and especially sodium, salts of the
above ar~ preferred. Sodium sulfate is typically used in deter-
gent granules and is a particularly preferred salt.
Other useful water-soluble salts include the compounds
commonly known as detergent builder materials. Builders are
generally selected from the various water-soluble, alkali metal,
ammonium or substituted ammonium phosphates, polyphosphates,
phosphonates, pnlyphosphonates, carbonates, silicates, borates,
and polyhydroxysulfonates. Preferred are the alkali metal,
especially sodium, salts of the above.
~ 2 ~ ~3
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Specific examples of inorganic phosphate builders are sodium
and potassium tripolyphosphate, pyrophosphate, polymeric meta-
phosphate having a degree of polymerization of from about 6 to 21,
and orthophosphate. Examples of polyphosphonate builders are the
sodium and potassium salts of ethylene diphosphonic acid, the
sodium and potassium salts of ethane 1-hydroxy-1,1-diphosphonic
acid and the sodium and potassium salts of ethane, 1,1,2-tri-
phosphonic acid. Other phosphorus builder compounds are disclosed
in U.S. Pat. Nos. 3,159,581; 3,213~030; 3,422,021; 3,422,137
3,400,17S and 3,400,148.
Examples of nanphosphorus, inorganic builders are sodium and
potassium carbonate, bicarbonate, sesquicarbonate, tetraborate
decahydrate, and silicate having a molar ratio of SiO2 to alkali
metal ox~de o~ from about 0.5 to about 4.0, preferably from about
1.0 to about 2.4. The compositions made by the process of the
present invention does not require excess carbonate for process-
ing, and preferably does not contain ovPr 2Xo finely divided
calcium carbonate as disclosed in U.S. Pat. No. 4,196,093, Clarke
et al., issued Apr. 1, 1980. and
is preferably free of the latter.
It is preferred not to hydrate any hydratable builder salts
in the fine dispersion mixer in the process of the present inven-
tion.
her ODtionals
Other ingredients commonly used in detergent compositions can
be included in the compositions of the present invention to
produce desired end product laundry products, but are not neces-
sary, and are lncluded here to sh~w the breadth of this invention.
These include flow aids, color speckles, bleaching agents and
bleach activators, suds boosters or suds suppressurs? antitarnish
and anticorrosion agents, soil suspending agents, soil release
agents, dyes, fillers, optical brighteners, germicldes, pH ad-
justing agents, nonbuilder alkalinity sources, hydrotropes,
enzymes, enzyme-stabilizing agents, chelating agents and perfumes.
~322~ ~
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EXAMPLES
-
The invention will be better understood in v;ew of the
following nonlimiting examples. The percentages are on a weight
basis, in the mixes prior to any subsequent follow-up drying,
unless otherwise specified. The tables are followed with addi-
tional processing disclosure in the numbered examples.
The terms "LAS" and "AS" as used herein mean, respectively,
"sodium lauryl benzene sulfonate" and "alkyl sulfate." The terms
like "C4~" mean C14 and Cls alkyl, unless otherwise specified.
Some of these AS and LAS surfactants do not require cooling if
used at about 20-25C.
A Cuisinart food processor, Model #DCX-Plus with 19.7 cm
metal blades operating at 1800 rpm is used for all examples. The
tip speed is 18.55 m/sec.
The viscositles of LAS and AS are measured using Brookfield
HAT Serial No. 74002 as follows:
For S0% and 70%, at 0.5 rpm with spindle T-A at 50C;
For 74% AS, at 0.5 rpm with spindle T-F at 50C;
For 50% AS, at 2.5 rpm with splndle T-A at 50C.
The granulation temperature for each high active surfactant
paste is determined on a case by case basis.
EXAMPLF~_l
An aqueous anlonic C13LAS sur1factant paste havlng a detergent
activity of 70% with tha balance ~eing water, plus a small amount
of unreacted and sodium sulfate salt as a reaction by-product, is
mixed with dry ice in a Cuisinart food processor. The viscosity
o~ the paste is about 800,000 cps 5see note below on viscosity
measurement technique). The paste temperature was first about
25~C. The paste temperature drops from 25C to -50CC and sur-
factant granules are formed.
The following tables summar ke several examples of the
invention.
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TQBLE OF EXAMPLES (Part 1)
Example Surfactant % Surf. % Unre- % % Dry
No. (Yo~ActivitY~ Active acted Water Builder
1 C13LAS (70) 70 3 27
2 C13LAS (6~) 60 3 37
3 C13LAS (70) 63 3 34 lO(a)
4 C13LAS (93) 60 3 2 35(b)
C13LAS/C4sAS 1:1 (70) 70 4 26
6 C4sAS (743 74 5 21
7 C4sAS (50) 50 3 47
8 C4sAS(e) (74) 68.3 4 20
9 Barlox 12(~) (8~3 87 3 10
Barlox 12~C) (87) 55 2 6 37(b)
11 Amphoterge K(d) (70) 70 3 27
TABLE OF EXAMPLES (Part 2)
Granulation
Example Temperature
No. S~rfactant C
I C13LAS 50
2 C13LAS -?0
3 C13LAS -35
4 C13LAS 4
C13LAS/C4sAS 1:1 -5
6 C4sAS 23
7 C~,5AS -5
8 C4sAS(e) -2
9 Barlox 12(~3 -60
Barlox 12(C) -40
11 Amphoterge K(d3 -52
~a) Sodium sulfate
(b) Sodium carbonate monohydrate used in Examples 4 and 10
at 35% and 37%.
:L~22rl~5
(c) Lauryl (12, 14, 16 blend) dimethyl amine oxide.
Barlox 12 is the trade mark of Lonza~ Inc.
(d) Coconut based imidazoline amphoteric, monocarboxylic.
Amphoterge K is the trademark of Lonza, Inc.
S(e) Ex. 8 is made with 7.7% mineral oil as a processing aid.
.
EXAMPLE 2
Example 2 is similar to Example 1, except that a 60% active
(vs. 70%) C13LAS is used. The paste viscosity is about 350,000
cps. The temperature at granulation is about -20C.
EXAMP~E_~
Example 3 is simllar to Example 1, except that 10æ sodium
sulfate is added to the 7~ active C13LAS. The builder salt to
surfactant active ratio is 0.16. The temperature at granulation
is about -35-C.
~M_LE 4
Example 4 is similar to Exam~le 3, exce~t 93X active C!3LAS
is used and 35% sodillm carbonatle monohydrate 1s added to the
surfactant paste~ The paste vlscosity is >1,000,000 cps. The
builder salt to surfactant active ratio is 0.54, The temperature
at granulation is about 4'C.
~M~lE 5
Example 5 is simllar to xample 1, except a 1:1 blend of
~ C13LAS and C~sAS is used. Both pastes have an activity level of
7Q%. Th~ viscosity of the C4sLAS is >7,000,~00 cps. The tem-
perature at granulation is about -5^C.
~L~
Best MQde: Example 6 is similar to Example 1, except 74~O
active C4sAS (vs. 70YO active C13LAS) is usedO The viscosity of
the paste is >790009Q00 cps. The temperature at granula~ion is
ab~ut 23'C.
The yield of the~e granules in the 200-2,000 micron particle
slze range is about 42%. The granules are set under ambient
1~227~
- 17 -
conditions and placed back in the mixer and mixed for about 15
seconds. The final yield is about 85%; moisture is about 14%.
EXAMPLE ?
Example 7 is similar to Example 6, except 50% active (vs.
74%) C4sAS is used. The viscosity of the paste is 25,000 cps.
The temperature at granulation is about -5C.
EXAMPLE 8
Example 8 is similar to Example 6, except 7.7% mineral oil is
added as a processing aid. The temperature at granulation is
about -2C.
EXAMPLE 9
Example 9 is similar to Example 19 except 87% active Barlox
12 (C12 16 dimethyl amine oxide) is used instead of 70% C13LAS.
The viscosity of the paste is about 1,000,000 cps. The tem-
perature at granulation is about -60C.
EXAMPL~. 10
Example 10 is similar to Example 9, except 37% sodium car-
bonate monohydrate is added to the 87% active Barlox 12. The
bu-ilder salt to surfactant active ratio -is 0.65. The temperature
at granulation -is about -40C.
EXAMPLE 11
Examp1e 11 is similar to Example 1, except 70% Amphoterge K
is used instead of 70% C13LAS. The viscosity of the paste is
about 500,000 cps. The temperature at granulation is about -52C.
In the above examples dense, concentrated, highly active
surfactant granules are successfully made using the process of the
present invention.
