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Патент USA US2407648

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Patented Sept. 17, 1946
2,407,647
UNITED STATES PATENT OFFICE
2,407,647
SYNTHETIC ORGANIC NONSOAP DETER
GENT IN BAR. FORM AND PROCESS OF
MAKING SAME
John W. Bodman, Winchester, Mass., assignor to
Lever Brothers Company, Cambridge, Mass., a
corporation of Maine
No Drawing. Application August 14, 1940,
Serial No. 352,519
8 Claims.
1
(chm-121)
2
.
>
This application is a continuation-in-part of
application Ser. No. 85,985, ?led June 18, 1936,
gent a harsh action when applied to the skin,
which, obviously is undesirable in. high grade
which matured as Patent No. 2,215,539 on Sep
toilet preparations.
tember 24, 1940. Application Ser. No. 85,985 is
It is now possible in accordance with my in
vention to prepare non-soap detergents in bar
a continuation of application Ser. No. 665,063,
?led April 8, 1933.
The present invention relates to an improve
ment in the manufacture of detergents and re
lates more particularly to the preparation of the
form which can be used economically as Waste or
disintegration of the bar on use is minimized. If
desired, the usual diluents or ?llers may be omit
ted entirely without a sacri?ce of bulk and wear
so-called “non-soap detergents" in commercially 10 ing qualities.
desirable forms.
The diluents commonly used have no marked
The term “non-soap detergents” is used herein
cohesive properties and when used in any mate
to designate materials having a cleaning action
rial proportlons render the detergent non
which are derivatives of higher fatty compounds
cohesive and di?cult of successful preparation in
or compositions other than the usual soaps, i. e., 15 bar form.
Attempts have been made to
soluble metal salts of fatty acids. For con
neutralize at least in part this lack of cohesive
venience, I prefer to utilize the, type of non-soap
ness by the use of binding agents. The addition
detergents which are readily available in their
of such addition agents for the purpose of bind
relatively pure form and which under normal
ing together the adulterated detergent particles
conditions of temperature and pressure are non 20 into bar form. however, is generally undesirable.
liquid. Of these may be mentioned the Gardinols
Among the other disadvantages, for example, of
which are salts of the sulfated higher fatty
such a bar or cake, is that it will not dissolve
alcohols, the Emco preparations which may be
into a clear solution. Moreover, the bar or cake
described as sulfocarboxylic acid esters of alcohol
is not coherent and coalescent, being made up
amine derivatives, and the A-type of the Igepon 25 of individual distinct particles, and does not
class of products which are fatty acid esters of
possess the ?rmness, ?ne texture, and appear
hydroxyethane sulfonic acid. All such composi
ance desired in toilet preparations. My invention
tions are well known in the art and may be de
may be utilized to produce a coherent and coales~
?ned generically as synthetic non-soap organic
cent bar or cake of non-soap detergent without
compounds having surface active properties.
30 the use of any binding agents whatsoever.
In accordance with my invention, non-soap
The products of my invention may be made
detergent compounds may be prepared in. a co
entirely from non-soap detergents and with or
herent and coalescent bar or cake form which
without small‘ amounts of diluent. If it is desired,
has the ?ne texture, ?rmness, shape stability and
varying. amounts of soap may be incorporated
wearing qualities desirable in high grade toilet 35 therewith. In fact, it is found to be advanta
soaps. Moreover, the product may be character
geous in many cases to combine the desirable
ized by a desirable mildness while possessing the
properties of non-soap and soap detergents.
bulk and degree of solubility preferred in deter
While liquid or semi-?uid non-soap detergents
gent bars or cakes.
generally may not be prepared in bar or cake
Non-soap detergents as a class of compounds
form, I have found that in accordance with my
are relatively expensive and highly soluble -in
invention they may be so modi?ed that they
comparison with the usual soluble soaps which
may be e?ectively used in the bar form when suit
they are intended to replace for cleansing and
ably blended with other detergents having a
other purposes. In marketing these compounds
normally solid form, such as a hard soap or other
heretofore, it has been considered necessary to 45 non-soap detergent.
prepare a product which has the bulk of an
In accordance with my invention the non-soap
equally effective soap product and at the same
detergents may in one preferred form be aerated,
time will not be materially higher in cost. To
i. e., may have small amounts of a compatible
accomplish this result, it has been customary to
gas distributed throughout the detergent mass.
add diluents generally of an inactive character, 50 If desired, the detergent may be su?iciently
for example, of the type of sodium sulfate or
aerated to reduce its speci?c gravity below that
sodium chloride. Also those which have at least
of water, thereby producing a ?oating product.
some of the properties of a soap builder may be
The formation of the improved products of my
added. The presence of material proportions of
invention may be carried out by working the
inorganic electrolytes may impart to the deter‘- 55 materials in admixture with small amounts of
3
2,407,047
4
water, preferably in a closed container, at tem
peratures sui?cient to render the mass plastic or
semi-?uid to ?uid. Under these conditions, it is
possible to manufacture a coherent bar of non
soap detergent which may be aerated or non
aerated, ?oating or non-?oating depending upon
the conditions of processing; and one having in
the preferred embodiment a characteristically re
ture should permit uniform blending and a con
tinuity of the mass in the ?nal product.
The method utilized for obtaining the desired
temperature conditions is not critical. For con
venience, the non-soap detergent stock, for ex
ample, in particle form, may be preheated in part
or in whole to the desired temperature prior to
charging it into the mixing apparatus, or heat
duced solubility and tendency to disintegrate;
may be applied to the detergent while it is in the
and also one having the properties of fine texture, 10 mixer, either during or before agitation, in any
continuity and appearance as well as other de
sirable characteristics important to the produc
tion of a commercially acceptable product in cake
convenient manner.
The processing of the non-soap detergents may
be carried out at a moisture content varying over
orbar form.
a wide range and depending primarily upon the
In producing the the new non-soap detergent 15 type of non-soap detergent selected for process
bar or cake, a non-soap detergent stock, prefer
ing. In most cases, a moisture content of from
ably in relatively pure form and solidi?ed in the
10-20% will be satisfactory. A moisture content
form of pellets, particles or fragments, is reduced
of less than 10% may be utilized with most non
to a heated plastic or semi-?uid condition while
soap detergents, if desired, but in general lower
it is intensely agitated or worked in a chamber 20 percentages of moisture render the material di?i
closed to the atmosphere. The particular kind of
cult to plasticize, at least in the types 01' appa
mechanical agitation to which the non-soap de
ratus which are available at present. When a
tergent mass is subjected for preferred results
moisture content of approximately 20% is ex
should be su?icient to move all portions of the
ceeded, the product in most cases tends to have
soap mass relatively to each other and expose 25 a rather soft and sticky form. The upper mois
them equally to any source of heat which may
ture limit, however, will vary considerably, de~
be utilized. The operation may be discontinued
pending upon the type of non-soap detergent
when there results a unitary mass of non-soap
selected. For example, it has been found that
detergent suitable for passing into form-impart
the Emco products referred to hereinbefore may
ing means where it may be cooled and solidi?ed 30 be formed into a ?rm bar with a moisture con
while retaining its continuous structure. If an
tent as high‘ as 35% if used alone. If blended
aerated mass is to be produced, a compatible gas,
with other detergents that would be made un
such as air, may be introduced into the mass
desirably liquid or sticky by high proportions of
while in a plastic, semi-?uid to ?uid state and
water or high temperatures, a lower average wa
thoroughly distributed through the mass during 35 ter content would be more suitable.
the Working operation.
For convenience, I prefer to utilize as a start
The process may be carried out in a batch type
ing material those non-soap detergents prepared
of operation or may be practiced in a continuous
commercially with a moisture content within
manner, if desired. It is possible to use a ma
the limits set forth above; if necessary, however,
chine of the Banbury mixer type as disclosed in 40 the moisture content may be regulated prior or
the patent to Banbury, No. 1,200,070, issued Octo
during processing in any suitable manner known
ber 3, 1916. A more desirable type of apparatus
to the art.
for continuous operations would be the appara
With a view to obtaining preferred charac
tus described in the patent to Pease, No. 2,048,236,
teristics in the product, it is desirable to subject
issued July 21, 1936. The apparatus which is se 45 the non~soap detergent mass to pressure while
lected should be adapted to thoroughly mix, shear
working. This insures an effective working ac
or knead the non-soap detergent stock under de
tion and minimizes the escape of moisture and
sired conditions of temperature, moisture con
air from the mass. It is desirable to have the
tent, and pressure.
air distributed in a ?ne uniform condition and
The temperature range under which I prefer
it is believed that the use of pressure increases
to carry out my invention will depend primarily
the desirable air distribution. The pressure may
upon the type of non-soap detergent selected.
cause the air to be dissolved in the plastic or
The temperature should be sufficient to render
semi-?uid mass. The air is then released in a
the detergent plastic or semi-?uid to ?uid and
highly dispersed form throughout the mass upon
capable of being readily worked into a coherent 55 release of pressure upon the mass. Any con
coalescent body of a continuous structure in the
venient pressure ‘beginning at slightly over at
types of apparatus described above. For most
mospheric to 100 pounds per square inch or more
commercially available non-soap detergents, a
may be used. Pressures of 25 pounds per square
temperature range of from 100 to 200° F. will be
inch have been found suitable. The pressure is
satisfactory. Temperatures above 200° F. may 60 preferably increased when higher temperatures
are employed.
be used but possibly without achieving the full
bene?ts of my invention in its preferred form,
In carrying out my invention, it is desirable
for with some non-soap detergents it has been
to use non-soap detergents which are available
found that when excessively high temperatures
are used, the resulting detergent product will be
subjected to generally undesirable shrinkage in
bar form during cooling, although in other re
spects the results may be satisfactory. Tempera
commercially in a relatively pure state or which
65
may be readily puri?ed. In addition to having
a milder action on the skin, it has been found
that the absence of inorganic salts increases the
?rmness and ?ne texture of the resulting prod
tures below 100° F. may be utilized with some
uct. However, small percentages of inorganic
non-soap detergents, provided the desired degree 70 material, for example, up to 15%, may be present
of plasticity is obtained. In using liquid or semi
in the detergent product without undesirable
liquid non-soap detergents with solid detergents
effects.
the temperatures used should be sufficient to
If desired, varying percentages of ordinary
make plastic or otherwise modify the solid de
soaps may be incorporated with the non-soap
tergent to the most desirable form. The tempera
detergents. These materials may be mixed in all
a
2,407,647
5
Example III
Proportions and for many purposes as high as
‘70% to 80% of soap may be used. When ma
terial percentages of soap are incorporated it
generally is desirable to modify and blend the
non-soap detergent with the soap by working as
Per cent
Non-soap detergent (sulfocarboxylic acid
ester of alcoholamine derivative) ______ __
Potassium chloride _____________________ __
described, utilizing preferably temperatures of
8.5
1
.5
Potassium sulfate _______________________ __
more than 145° F. and with a moisture content
Soap (20 coconut oil, 80 tallow) anhydrous__ 72
particularly desirable properties. The detergent
esters of mono-ethanolamine. When processed
18
Water _________________________________ __
of the soap of less than 25%. I have found that
by blending as described a non-soap and soap
The non-soap detergent utilized in the above
detergent a product may be produced having 10 example was composed of sulfocarboxylic acid
effectiveness is materially increased in hard wa
at a temperature of 180° F., this mixture pro
ter districts and in sea water and any tendency
duced a floating bar of good'texture.
for the more soluble non-soap detergent incor
Example 1V
porated to leach‘ out or separate is minimized in 15
Per cent
view of my processing. In its preferred form
Non-soap detergent (Santomerse) ______ __
Inactive ingredient ____________________ __
this product is aerated during processing, suffi
4.25
.75
ciently to float.
Soap (20 coconut oil, 80 tallow) anhydrous_ 77
For convenience, the non-soap detergent stock
to be used in carrying out my invention may be 20 Water ___________________________ _._.._.___ 18
The non-soap detergent used in this example
in the form of the usual commercial spray-dried
was an alkyl aryl sulfonate. When ‘processed at
product. When the operation is carried out in
a temperature of 200° F., this mixture produced
a continuous fashion the charging of the spray
dried non-soap detergent into the apparatus is
a ?oating bar.
In accordance with the disclosure herein it will
usually accompanied by the inclusion of sum 25
cient air to insure an aerated or even a ?oating
product. If a compacted charge is used, it may be
necessary to supply an additional quantity of air
to the apparatus. When operating under a batch
system, sufficient air may be made available for 30
be seen that a bar or cake may be prepared in
accordance with my invention which will wear
suf?ciently slowly to make its use economical
when compared to detergent products made from
ordinary soaps or from non-soaps with high pro
incorporation by only partly ?lling the machine.
portions of ?llers. The bar has the texture and
Agitation of the non-soap mass preferably with
appearance desirable in a high grade toilet soap
heating and under pressure may be continued
and is satisfactory in every respect for ordinary
for a sufficient period of time to disseminate the
usage. In addition it may be aerated sufficiently
air in a ?nely-divided condition throughout the
to float thus having, in addition to the advantages
entire mass and to plasticize the mass as a con
of a fine toilet soap, the well known desirable
tinuous and coherent body. When the mass is
properties of a ?oating soap.
completely mixed, it may be released or dis
It is to be observed that the amount of inert
charged by extrusion under pressure or otherwise
material present in an example of a preferred
into a mold or form-imparting means. If desired 40 product is a relatively small amount, for example,
the pressure may not be released until in the
less than 15%. Despite the presence of only a
form-imparting means. The detergent cools and
small amount of inert ?ller or its complete ab‘
solidi?es in a desired coherent and coalescent
sence the non-soap detergent product in bar form
form and may be reduced to any desired shape by
is not wastefully given off during ordinary usage.
cutting or trimming and impressed with a design 4.vi Because of this increased coherency of the mass
by a stamp or die.
The following examples serve to illustrate the
manufacture of a satisfactory coherent ?oating
bar from non-soap detergents.
as a result of the utilization of my process it is
possible to make a coalescent bar consisting en
tirely or in part of non-soap detergent material
without the disadvantage of using binders.
Apparently the processing as described tends V
Example I
Per cent
to decrease the solubility or disintegration of the
mass sufficiently to release upon use, and without
Sodium salt of lauryl sulfate _____________ __ 81
waste, only about that amount of deter-gent de
Inactive diluent __________________________ __
Water __________________________________ __ 10
sired or necessary for a detergent effect. A pre
ferred bar or cake results having a continuous
This mixture was Worked vigorously at a tem
perature of 200° F. and then extruded into a mold
and cooled. The resulting bar had a speci?c
body free from laminations or cleavage planes.
The aeration of the mass is also an important
factor in the production of a preferred form of
non-soap detergent bar for by aeration the bulk
9
gravity of 0.88.
Example II
of the relatively expensive ingredient is mate
rially increased and its solubility decreased. The
type of aeration is probably an important factor
in obtaining these results in a maximum amount.
Per cent
Non-soap detergent (sulfocarboxylic acid
ester of alcoholamine derivative) ______ __ 59.5
Potassium chloride _____________________ __
Potassium sulfate _______________________ __
The best embodiment, I have found, results from
65 aerating the mass while working in a plastic or
7
3.5
Water _________________________________ __ 30
semi-liquid heated condition under pressure.
The product so formed is characterized by an ex
tremely ?ne air distribution imparting a white
color and smooth feel. A material proportion of
the air cells in some masses so processed have
The non-soap detergent was composed of
sulfocarboxylic acid esters of mono-ethanol
amine. This mixture was Worked at a tempera
ture of 160° F. The resulting bar had a speci?c
gravity of 0.83.
been found to be highly irregular in shape and
constitute no more than tiny ?ssures between
crystals.
It will be apparent that my invention is sus
75 ceptible to many variations and all such varia
2,407,647
7
tions are intended to be included in the scope of
the following claims.
I claim:
1. A process for making a coherent and coa
lescent bar of a normally non-liquid synthetic or
ganic non-soap detergent compound having sur
face active properties, said bar having an aerat
ed continuous mass of ?ne texture and ?rmness
comprising subjecting a mass of a normally non
liquid synthetic organic non-soap detergent com
pound having surface active properties having a
moisture content of less than about 35% to a
U temperature of the order of 100 to 200° F., work
ing the mass in the presence of a compatible gas
under pressure, and thereafter. forming the mass
into bars or cakes.
8
5. The process of producing a ?oating bar
from a mass of a major proportion of alkali metal
soap and a minor proportion of a synthetic or
ganic non-soap detergent compound having sur
face active properties, said bar having ?ne tex
ture, ?rmness and a continuous aerated mass,
said process comprising subjecting said mass in
a closed chamber under pressure to intensive agi
tation while at a temperature whereby the mass
is in a plastic or semi-?uid condition and in the
presence of air and forming the continuous
aerated mass into a ?rm bar having a ?ne tex
ture and a continuous aerated mass.
6. An aerated cake or bar suitable for deter
gent purposes comprising a normally non-liquid
synthetic organic non-soap detergent compound
having surface active properties having a con
tinuous aerated mass of ?ne texture and ?rm
organic non-soap detergent compound having
nes-s, said aerated mass resulting from the cool
surface active properties, said bar having an 20 ing of a semi-?uid to ?uid and continuous nor
mally non-liquid synthetic organic non-soap de
aerated continuous mass of ?ne texture and
?rmness comprising subjecting a mass of a nor
tergent mass through which a compatible gas
2. A process for making a coherent and coa
lescent bar of a normally non-liquid synthetic
mally non-liquid synthetic organic non-soap
detergent compound having surface active prop
has been disseminated while Working under pres
ing, and thereafter forming the mass into bars
tergent compound having surface active proper
ties and an alkali metal soap, said bar having an
sure and at a temperature su?‘icient to render
erties having a moisture content of leSs than 25 said non-soap mass at least semi-?uid and con
tinuous.
about 35% to a temperature at which the mass
is semi-?uid to ?uid and continuous, aerating
7. A process for making a coherent and coa
the continuous mass under pressure while work
lescent bar of a synthetic organic non-soap de
or cakes.
3. A process for making a coherent and coa~
lescent bar of a normally non-liquid synthetic or
ganic non-soap detergent compound having sur
aerated continuous mass of ?ne texture and ?rm
ness which comprises subjecting a mass compris
ing not morethan 80% of soap with a moisture
face active properties, said bar having good wear
content of less than 25% and more than about
ing qualities and containing less‘ than 15% of 35 4% of said non-soap detergent to a temperature
diluent material, which comprises subjecting a
of more than 145° F., aerating while working the
mass of a normally non-liquid synthetic organic
mass under pressure in the presence of a com
non-soap detergent‘compound of at least 85%
patible gas and forming the said aerated mass in
purity having surface active properties, to a tem
bars or cakes.
'
perature at which the mass is semi-?uid to ?uid 40
and continuous, aerating the continuous mass
under pressure while working and thereafter
forming the mass into bars or cakes.
4. A process for making a coherent and coa
lescent bar of a synthetic organic non-soap de 45
tergent compound having surface active prop
8. A ?oating aerated cake or bar suitable for
detergent purposes comprising a synthetic or
ganic non-soap detergent compound having sur
face active properties in an amount of more than
about 4% and an alkali metal soap in an amount
of not more than about 80%, said cake or bar
having a continuous and uniformly aerated mass,
erties and an alkali metal soap, said bar having
said aerated mass resulting‘from the cooling of
an aerated continuous mass of ?ne texture and
a semi-?uid to ?uid and continuous synthetic
?rmness ‘which comprises subjecting a mass com
organic non-soap detergent compound having
prising more than about 4% of said non-soap 50 surface active properties in an‘ amount of more
detergent compound and not more than 80%
than about 4% and an alkali metal soap in an
of said alkali metal soap to a temperature at
amount of not more than about 80%, through
which the said mass is semi-?uid to ?uid and
which a compatible gas has been disseminated
continuous, aerating with working said semi
while working under pressure and at a temper
?uid to ?uid and continuous mass in the pres 55 ature su?icient to render said non-soap mass at
ence of a compatible gas under pressure and so
lidifying and forming the said aerated mass into
bars or cakes.
least semi-?uid and continuous.
JOHN W. BODMAN. >
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