Jan. 30, 1951 FP.

BRADFORD 2,539,889
METHOD OF MANUFACTURING SOAP
Filed June 16, 1947

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INVENTOR.

BY
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477.7 CDARP fwyaf y^
Patented Jan. 30, 1951
UNITED STATES PATENT OFFICE 2,539,889
METHOD OF MANUEFACTURING SOAP
Purdy Bradford, Paos Heights, E., assignor to
Swift & Company, Chicago, Ill., a corporation
of Elinois
Application June 16, 1947, Serial No. 754,949
2 Claimis. (C. 269-413)
The present invention relates to a method of
manufacturing soap. More particularly, the in
vention has to do with a continuous soap-making
process wherein the saponifiable material is Sub
jected to a purification treatment before Saponi
fication, whereby the resulting soap is of in
proved quality and may be employed in the
preparation of high-grade toilet Soaps.
Important steps in the art of Soapmaking in
volve the selection of the saponifiable raw ma
terial and the treatment thereof to produce a
soap having the desired characteristics. For
example, a high degree of purity, as evidenced
by the whiteness of the soap, is highly desirable
in high-grade toilet soaps. Crude Saponifiable
fatty material contains color bodies which, if not
removed from the fatty material, are often car
ried into the finished soap product, thus making
it impossible to obtain a high degree of white
ness and purity in the finished product. In pro
ducing a superior toilet Soap, it is often the prac
tice. to select superior raw material relatively
color free, and to subject the said material to a
bleaching operation before Saponification.
The quality of whiteness possessed by the
high-grade soap is not only due to the nature
of raw material treated, but is also partly due
to the Soapmaking process employed. When the
so-called full-boiled process of making soap is
employed, a series of operations are involved, as
a result of which the color characteristics of the
finished soap are improved. In the full-boiled
soap-making process, Saponification is carried
out in successive stages, which involve boiling of
‘the soap in water, graining or Salting out the
soap, removing the aqueous layer containing
various impurities and glycerine, and settling.
In other soapmaking processes, such as the
semi-boiled and cold processes, the operations of
boiling, graining and settling are omitted. Con
sequently, any improvement in color in the fin
ished product due to these omitted operations is
lacking. For these reasons, the Soap product
obtained from the aforesaid soapmaking proc
esses is usually inferior in color characteristics
to that obtained from the full-boiled process.
Because it is desirable that a high-grade toilet
soap possess a high degree of whiteness, the full
boiled process of making Soap is generally em
ployed in the manufacture of the Superior White
SOa).
More recently, in the art of Soapmaking, there
have been developed processes for the continuous
saponification of fats. The continuous saponi
fication process generally involves a careful mix
2,539,889
2
ing of the fat or fatty acids, often in the presence
of a diluent with the correct amount of caustic,
Saponifying the mixture, then spraying the re
Sulting soap into a spray or flash chamber,
wherein the volatile products of saponification
are flashed off, and the Soap is recovered as a
dry product.
The washing effects of the various operations
of the full-boiled process are lacking in con
tinuous Saponification processes. The degree of
Whiteness in the finished product, therefore, is
inferior to that of the full-boiled soap, and is
about equivalent to that possessed by the soap
obtained by the Semi-boiled Or cold process.
Íö An object of the invention is to produce soap
of improved color characteristics, employing a
continuous Saponification process.
Another object of the invention is to produce
Soap of improved color characteristics by means
of a continuous saponification process, which
SOap is Superior to or equivalent to full-boiled
SOap,
A further object of the invention is to provide
a continuous Saponification process, wherein
purification of the Saponifiable fat is continuously
effected.
Yet anOther object of the invention is to pro
vide a continuous saponification process, where
in the diluent for the fat employed in the con
Si tinuous Saponification of the fat is utilized in
the purification of the fat before the continuous
Saponification thereof.
A still further object of the invention is to
provide a process wherein the diluent is recovered
from the Soap, is employed in the purification of
the fat, and is simultaneously purified with the
fat.
Other objects and advantages of the invention
will be apparent from the following description.
iO - The invention contemplates broadly a con
tinuous Soapmaking process, wherein a solution
of the fat to be saponified is effected with the
diluent or Solvent, such as kerosene, employed
in the saponification operations, the resulting
solution bleached and then subjected to saponi
fication conditions of temperature and pressure,
Whereby the fat is converted into soap and glyc
erine. The products of Saponification are then
discharged into a vaporization zone maintained
50 under reduced pressure, wherein the volatile ma
terials, including diluent, are separated from the
soap by vaporization.
More particularly the invention contemplates
forming the fat to be Saponified into a solution
With the diluent employed in the continuous sa
 2,589,889
3 4.
ponification of the fat. The solution is treated
with a bleaching agent, for example, fuller's
earth, at elevated temperatures. After bleach
ing of the fat solution, the Solution is filtered
and the earth-free solution mixed with a caustic
saponifying reagent. The resulting mixture is
charged to a saponification Zone to effect the
Saponification reaction, following which the Soap
is separated from the Volatile products of Saponi
fication, including the diluent. The diluent is
recycled and is used to form a Solution. With new
fat. The solution is treated with a bleaching
agent, whereby both the fat and the recovered
Solvent may be decolorized.
In carrying out the invention," it is contem
plated to employ a continuous Saponification
process, wherein a diluent is employed for the
saponification reagents and the products of sa
ponification. It is also understood that the
diluent exhibits Solvent action for the fat to be
saponified. A suitable saponification process for
accomplishing the purposes of the present in
vention is shown, for example, in Patent No.
2,401,756 to Gunther, issued June 11, 1946.
The aforesaid patent discloses a continuous
Saponification proceSS, employing a relatively di
lute caustic alkali solution and an amount of dil
uent or solvent for the saponifiable material in
excess of 50 per cent, and preferably at least
about 75 per cent, based Cn the Saponifiable mat- :
ter. The relative large amounts of diluent make
it possible to effect the saponification reaction
at lower temperatures than would be possible
were the diluent not present and to maintain the
Soap product fluid at temperatures below the
melting point thereof.
In accordance with the Gunther patent, the
caustic alkali solution, saponifiable material, and
diluent, formed into an emulsion, are subjected
to conditions of Saponification in a Zone of re
stricted cross-section, under pressure, to prevent
vaporization of any of the reactants and products
of saponification. Upon completion of the Sa
ponification reaction, the mixture is heated and
then sprayed into a low-pressure Zone, wherein,
by partial pressure distillation, the volatile prod
ucts of saponification and the diluent are vapor
ized and continuously removed, leaving the Soap
product, which may also be continuously re
moved. -
The invention will be more fully understood
from the following description read in connec
tion with the accompanying drawing which shows
diagrammatically a form of apparatus which can
be employed for carrying out the process.
Referring more particularly to the drawing,
the numeral O indicates a tank for holding sa
ponifiable fat, for example, tallow. Another tank
f is provided for the storage of the diluent, or
solvent, for the fat, such as kerosene. The fat
and diluent are introduced through conduits 3
and f4, respectively, into a bleaching tank S.
Bleaching tank 6 may be provided with a hopper
for the introduction therein of bleaching ma
terial, such as fuller's earth, and means, such as
an agitator 8, to effect intimate admixture of
the solution and earth. The bleaching tank may
also be provided with means for supplying heat
to the contents thereof, since it is preferred to
carry out the bleaching operation at tempera
tures above 212° F. Following the bleaching op
eration, the bleached fat solution is withdrawn
from the bleaching tank through line 22 and, in
the form of a slurry, is pumped by means of
pump 23 into a filter press 25. The filtered fat
solution is collected through line 27 in feed
tank 29.
The solution of Saponifiable fat in the Solvent
and aqueous caustic soda of the desired strength
held in tank 3 are drawn in the proper ratio
through conduits 33 and 35, respectively, by pro
portioning pump 37, driven by motor 38. From
the proportioning pump 37, the Saponification
reactantSflow in a common Stream through con
duit 40 to homogenizer I ; t. The homogenizer may
be any suitable apparatus wherein the fat Solvent
solution and the caustic may be thoroughly mixed.
A suitable homogenizer may comprise a container
and an agitator 43 driven by any suitable Source
of power through a pulley 44. In the homo
genizer an emulsion is formed comprising mi
croscopic globules of caustic soda solution dis
persed in the solution of Saponifiable material.
The emulsion usually contains a Soap formed by
20 the instantaneous neutralization of the free fatty
acids contained in the fat, which functions to
stabilize the dispersion of the aqueous caustic
phase in the inert medium. -
From the homogenizer the emulsion is pumpe
by means of pump. 46 through conduit 47 into
saponification coil 48, which is provided with any
suitable heating means to raise the temperature
of the emulsified mixture to that necessary for
substantially complete saponification. The tem
perature of reaction will vary inversely with the
length of time the mixture remains in the coil,
being about 400° F. for a 7-minute reaction pe
riod and lower for longer, periods of residence-in
the coil. The pressure in the saponification coil
is sufficiently high to prevent substantial evap
oration of the diluent. This pressure may be ap
proximately 100 pounds per Square inch. Upon
completion of the saponification reaction, the
fatty mixture passes from the saponification coil
40 through conduit 50 into a relatively short pre
heating coil 52. The temperature of the reaction
mixture may be raised in coil 52 high enough,
for example, to about 480° F., to supply sufficient
sensible heat to facilitate flash evaporation of the
45 inert diluent and glycerine from the soap product
when the pressure is reduced. The preSSure, in
the preheating coil is maintained Sufficiently high
to avoid vaporization which might interfere with
keeping the saponification reaction products...in
50 a fluid state. :
The reaction mixture passes through conduit
54 to a nozzle 56, from which it is continuously
sprayed into a vaporizing, or flash, Zone 58. The
chamber 58 is held at relatively low pressure,
preferably less than 40 mm. of mercury absolute,
whereby a substantially complete separation of
water, glycerine, and other volatiles from the
Soap, product usually occurs. The conditions in
the heating coils and flash chamber are prefer
60. ably controlled. So that the temperature of the
soap and vapors after flashing is reduced to about
320 F. to 350 F., or to a temperature just above
the boiling point of the highest boiling volatile
constituent at the existing conditions. In some
cases, particularly where it is desired to produce a
Soap product having a high glycerine content or
where glycerine recovery is not material, the pre
heating coil may be eliminated. In the latter
case, the reaction mixture passes directly from
70 the saponification coil and through the spray
nozzle into the flash chamber. In such cases,
more volatile diluent is preferably employed
and/or heat supplied through the jacket of the
vaporization chamber in order to flash the dji
75 uent. The preheating coil is preferred, however,
 ?,589,889
7 8
fat in the presence of the solvent are preferably mately mixed in the homogenizer to form ari
above 212 F., for example, between about 215.F. emulsion. The emulsion was continuously passed
and 220° F., in order to evaporate moisture, the through a saponification coil at a temperature of
presence of which seems to render the bleaching about 415 F., under a pressure of about 100
operation less effective. In the absence of Water pounds per square inch. The time of flow of
the bleaching step may be accomplished at lower the reaction mixture through the Saponificationi
temperatures, a temperature as low as 140 F. coil Was about Seven minutes, after which time
having been found satisfactory. the Saponification reaction was completed. Fol
I have found that bleaching of fat in the pres lowing saponification, the mixture was passed
ence of a solvent prior to charging the resulting 10 through a preheating coil and the temperature
bleached solution to a saponification process re thereof raised to about 480° F. in about 25 Sec=
quiring the presence of a diluent, as hereinabove onds, while maintaining the pressure of about 100
illustrated, produces a Soap of Superior color char'- pounds per Square inch. The mixture was thieri
acteristics. The Soap produced in this manner sprayed through a restricted nozzle into the flash
may be used in the preparation of high-grade chamber, which was maintained at about 400 F.
White toilet Soaps which heretofore have gener and at a reduced pressure of about 20 mm. Of
ally required the full-boiled process for the manu mercury absolute. Solid soap in the form of a
facture thereof. I have found that if the fat is White powder settled to the bottom of the flash
first separately bleached prior to being formed into chamber and was continuously removed there
a mixture with the diluent and then saponified, ; from. The vapors Were continuously discharged
the resulting soap does not possess the degree into a fractionating tower, also maintained at a
of whiteness characteristic of soap produced by preSSure of about 20 mm., wherein the vapors
the full-boiled process or the process herein dis were separated by rectification. The tempera
closed. ture of the vapors coming off the top of the tower
In soapmaking processes heretofore practiced 2 5 Was about 100 F., at which temperature the
it has not been customary to bleach a solution of major portion of the solvent condensed as a reflux
the fat, for such a process used in connection condensate and was taken off of an upper plate
therewith would have no particular utility. For of the column and recycled to the system. The
example, if the aforesaid process were applied Lo volatile materials, including the small proportion
the full-boiled process of soap manufacture, the 30 of uncondensed diluent, passed into a condenser,
Solvent Would require removal after the bleach wherein water and the diluent were condensed and
ing operation, an expensive operation and one Separated by stratification in a settling tank.
which would tend to discolor the fait, thus ren Employing portions of the same tallow used
dering the whole Operation useless. For these in accordance with the foregoing process, saponi
reasons, bleaching of the fat has heretofore been 35 fication of one portion of the tallow was effected
accomplished in the absence of a solvent. by following the full-boiled process, and the
In accordance with the present invention, how other portion according to a continuous process,
ever, the bleaching of the fat in the presence of Substantially - as hereinabove described, except
the diluent employed in the continuous Saponifi that bleaching of the tallow was effected in the
:cation process has many advantages. For exam 40 absence of solvent. Three 40-gram samples of
ple, the heat imparted to the fat in effecting the Soap, representing each of the three methods,
Solution thereof may be advantageously utilized were separately dissolved in 100 ml. of specially
in the Saponification reaction. In addition, by denatured ethyl alcohol, and the three solutions
Virtue of the combination of the bleaching step measured for color on the Lovibond scale. Soap
With the Steps in the continuous saponification .i 5 from the continuous process, wherein bleaching
proceSS, it is not required to remove the solvent was performed without the solvent, gave a read
after bleaching. The Solvent is removed after ing of 2.3 R., while the full-boiled soap gave a
Saponification from the Soap, an operation which value of 1.2 R., and Soap prepared in accordance
is inherent in the continuous Saponification proc With the present invention, 1.0. R. The results
eSS. For this reason no disccloration of the fait : show that the present invention is productive
occurs through distillation of the solvent there of a Soap of a higher degree of whiteness than
from, and the process is rendered economical. By Soap prepared by prior art methods.
using fat immediately after decolorizing and with AS another illustrative example of the inven
out removing solvent there is no opportunity for tion, a second lot of tallow was substituted for
fat to deteriorate and a better colored soap is i5 5 the fat used in the preceding example. Bleach
obtained. Moreover, I have found that the sol ing and saponification conditions were the same
vent distilled from the products of the saponifi as in the first example. Color tests were then
cation reaction is often discolored, but that in performed by comparing, for color, the alcohol
reusing the Solvent in the bleaching of additional Solution of the resulting Soap with the solutions
fat, the Solvent is decolorized along with the fat : of Soap made from portions of the same tallow
and may thus be used indefinitely. by the full-boiled process and the continuous
As an example of the invention, 100 parts of Soap process wherein the tallow had not been
prime tallow, not darker than 17 F. A. C., hav bleached in the presence of the diluent. The
ing a free fatty acid content of 2.5 per cent, and colors of the three solutions were as follows:
-125 parts of a petroleum fraction boiling between (5 3.6 R. for. Soap obtained by the continuous proc
about 450 F. and 500 F. were formed into a Solu eSS Wherein bleaching of the fat was effected in
tion. The solution was then agitated in the pres the absence of solvent; 2.6 R. for full-boiled
ence of about 1 per cent fuller's earth for about Soap, and 2.5 R. for Soap obtained in accordance
one-half hour and at a temperature of about 215 With the invention.
F. to bleach the fat. Following the bleaching 70 . While the present invention has been - de
operation, the mixture was filtered and the result Scribed as being particularly adapted to the
ant earth-free Solution Was formed into a com Soapmaking process described in the Gunther
mon stream with a 50 per cent caustic solution patent aforementioned, it is understood. that the
in the ratio of 28 parts of the caustic to 100 parts
invention is not to be construed as being limited
of fat. -The fat solution and caustic were inti 75 thereto, but may be applied to other soapmaking
 2,589,889
9 10
processes embodying various modifications, and
which employ a diluent for the saponification
reactants and reaction products. For example,
the invention may be used in connection with
continuous saponification processes which en
ploy substantially smaller amounts of diluent
than are disclosed in the Gunther patent or
with processes which are characterized by the
use of an anhydrous Saponifying reagent and a
diluent.
Obviously, many modifications and variations
of the invention, as hereinbefore set forth, may
be made without departing from the spirit and
scope thereof, and therefore only such limita
tions should be imposed as are indicated in the
appended claims.
I claim:
1. In a continuous process of manufacturing
soap, the improvement which comprises: form
ing an intimate mixture of a Saponifiable ma
terial containing objectionable color bodies, a
solid adsorbent bleaching agent, and an inert
hydrocarbon boiling between about 230 and 500
F., said hydrocarbon having a property of form
ing a solution with both the Saponifiable ma 35
terial and the soap Subsequently formed there
from; separating the bleaching agent and objec
tionable color bodies from the solution of saponi
fiable material; subjecting the bleached saponi
fiable material while dissolved in the Said hydro
carbon to a saponification temperature and
pressure in the presence of an alkaline Saponi
fication reagent to convert the Saponifiable ma
terial into glycerin and Soap, Said Soap Sub
stantially free of objectionable color bodies being :
dissolved in said hydrocarbon; and discharging
the products of saponification and the hydro
carbon into a fractionation Zone to individually
recover the said products of saponification and
the hydrocarbon. 40
2. In a continuous process of manufacturing
soap, the improvement which comprises: form
ing in a mixing zone an intimate mixture of a
saponifiable material containing objectionable
color bodies, a solid adsorbent bleaching agent
and an inert hydrocarbon boiling between about
230° and 500° F., said hydrocarbon having the
property of forming a solution with both the
Saponifiable material and the Soap Subsequently
formed therefrom, and being present in an
amount at least between 100 and 150 per cent
by Weight of the saponifiable material; separat
ing the bleaching agent and objectionable color
bodies from the Solution of Saponifiable ma
terial; subjecting the bleached saponifiable ma
terial while dissolved in the said hydrocarbon
to a saponification temperature and preSSure in
the presence of an alkaline Saponification re
agent to convert the saponifiable material into
glycerin and soap, said soap Substantially free
of objectionable color bodies being dissolved in
the said hydrocarbon; discharging the products
of saponification including dissolved Soap, gly
cerin, and hydrocarbon into a fractionation zone
maintained at subatmospheric pressure to indi
vidually separate the soap, glycerin, and hydro
carbon; and recycling the Said hydrocarbon
without further processing to the mixing Zone
where it is bleached simultaneously with the
Saponifiable material.
PUROY BRADFORD,
REFERENCES C TED
The following references are of record in the
file of this patent:
UNITED STATES PATENTS
Number Name Date
2,100,146 Schmidt-Nielsenetal.-Nov. 23, 1937
2,255,875 BuxtOn et al. ——-----l— Sept. 16, 1941
2,318,748 BuXton et al. --————— May 11, 1943
2,383,630 Trent -------------- Aug. 28, 1945
2,401,756 Gunther –––------–– June 11, 1946
FOREIGN PATENTS
Number Country Date
251,290 Great Britain ------ July 25, 1947