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41
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July 2» 1946»
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B. H. THURMAN
2,403,413
PRocEss oF MAKING soAP
Filed llarch 23, 1942
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Patented July 2, 1946
2,403,113
UNITED STATES PATENT OFFICE
2,403,413
PROCESS 0F MAKING SOAPBenjamin H. Thurman, Charlotte, N. C., assignor,
by mesne assignments, to Benjamin Clayton,
Houston, Tex., doing business as Refining,
Unincorporated
applicati@ March 23, 1942, serial No.v 435,900
12 Claims. (ci. 252-39)
1
2
.
tively high temperatures so as to produce a
This invention relates to a process of making
soap and more particularly to a process by which
soap is produced from glycerides and glycerine is
liberated and recovered and in which a saponi
fying agent which does not react readily with
glycerides may be employed.
The invention has particular utility in
conjunction with the production of
molten substantially anhydrous glycerine free
soap- although a desired quantity of glycerine may
water
insoluble soaps such as aluminum soaps. mag
nesium soaps, lead soaps and other soaps of 10
polyvalent metals, although it may be employed
be -left in the soap if such glycerine is desired in
the ñnalproduct. Also a desired amount of
moisture may 'be reincorporated into the soap
before discharge of the same from the process.
A lubricating oil may be added to the materials
prior to the vapor separating step or to the soap
withdrawn lfrom the vaporizing step depending
upon the nature of the lubricating oil and the
temperatures employed in the vapor separating
to produce water soluble soaps such as alkali
, step. Th'e resultant soap may thus be discharged
metal soaps, for example, sodium and potassium
from the process as glycerine free anhydrous
soaps even though compounds of alkali metals
which do not react readily. with glycerides are 15 soap, as anhydrous soap containing glycerine, as
anhydrous soap admixed with lubricating oil, or
employed as saponiñcatlon‘agents. It also has
as anhydrous soap admixed with lubricating oil
utility in the production of various soap mixtures
and glycerine, or a desired amount of water may
which may contain both soluble and insoluble
be incorporated in the soap before itis discharged
soaps. The soap making process of the present
invention is capable of producing glycerine free 20 from the process, irrespective of whether the
soap contains any other material such as
anhydrous soaps or soaps containing any desired
glycerine or lubricating oil. In any case a sub
-amounts of glycerine and water and may also
stantially anhydrous soap which may or may not
include saponiñcation in the presence of a
contain glycerine. lubricating oil or both, is at
lubricating oil- or the addition of such oil to the
resultant soaps preferably while the soap is in 25 least an intermediate product in the process.
Anhydrous soaps of polyvalent metals usually
molten anhydrous form so as to produce
have substantially lower melting points than
lubricating greases.
anhydrous alkali metal soaps. Also glycerine
The term "saponiñcation” is employed herein
may be substantially completely separated in
to mean a reaction in which soap is one of the
products and is not intended to cover or embrace 30 vapor form from soaps of polyvalent metals at
temperatures substantially below the melting
reactions involving de-esteriñcation only of
point of anhydrous alkali metal soaps if the
esters such as the splitting of glycerides without
polyvalent metal soap or soap mixture is molten
the formation of soap. Similarly the term
at such temperatures when anhydrous. The
“saponifying agent” is employed to mean an
agent which reacts with fatty material to form 35 melting points of anhydrous alkali metal soaps
'are usually substantially above 550° F. and at
soap irrespective vof whether any de-esterlflcation
is involved.
Y
such temperatures glycerine is quite rapidly
decomposed in the presence of excesses of caustic
In carrying out the process of the present
alkali. At least 'slight excesses of saponifying
invention, the glycerides are ñrst split so as to
produce a mixture consisting essentially of fatty 40 agent are desirable in soap making processes to
insure completion of the reaction. In general,
acids, glycerine and water. Saponification of the
glycerine may be substantially completely
fatty acids is then rapidly produced under
relatively high temperature conditions without
recovered in vapor form from soaps of polyvalent
prior separation of glycerine and water from the
metals under vacuum conditions at temperatures
fatty acids. Under these conditionslv relatively
below 550° and usually below 500° F., which
inactive saponifying agents, which will not
temperatures do not cause appreciable destruc
readily attack glycerides, rapidly convert the
tion of glycerine even though excesses of sapOni
fatty acids into soap and any unsplit glycerides
fying agents are present. That is to say
in the'glycerine-fatty acid mixture are reacted
and their glycerine recovered even though the
saponiñcation agent is not sufliciently active for
effective saponiñcation of a material Consisting
essentially of glycerides.
The glycerine and water may be separated
from‘ the resultant soap by vapOrìZatiOn at rela
glycerine will substantially completely vaporlze
from soap at 400° F. under` a vacuum of at least
28% inches of mercury if the soap or soap mix
ture is molten when anhydrous at that tempera
ture. This is one of the primary reasons'why thc
5“ present process has particular utility in the `
_ ’
2,403,413
3
production of the lower melting point water
insoluble soaps. `
Alkali metal soaps may, however, be produced
and glycerine recovered by the present invention -
4
A still further object of the invention is to pro
vide a complete process in which an insoluble soap
is made from glycerides and in which a saponify
ing agent which does not‘readily react with glyc.
erides is employed.
Other objects and advantages of the invention
will appear in the following description of pre
ferred embodiments of the invention made in
pounds of alkali metal, for example sodium
connection with the attached drawing oi which
carbonate, di-sodium phosphate, tri-sodium
Fig. 1 is a schematic diagram of an apparatus
phosphate, etc. In such cases all of the saponi 10
for carrying out the process of the present in
fying agent may be a non-caustic alkali
vention; and
compound or the majority of the saponifying
Fig. 2 is a view similar to Fig. 1 illustrating a
agent may be an alkali metal hydroxide so long
modification of certain of the apparatus of Fig. 1.
as the caustic alkali is insuñlcient to provide an
In one embodiment of the present invention,
excess after the fatty material is completely 15
suitable apparatus for which is shown in Fig. l,
saponified. The caustic alkali all reacts with
glycerides are ñrst split into glycerine and fatty
the fatty material leaving the non-.caustic com
acids in a batch splitting step. Since the re
pOund to constitute the excess and such excess
mainder of the process may be carried out in a
non-caustic compounds are much less de
structive of glycerine at high temperatures than 20 continuous manner, a plurality of reaction cham
without substantial destruction of glycerine even
in the presence of excesses of alkali metal com
pounds if such excesses are non-caustic com
alkali.
»
bers, for example, three reaction chambers I0, II
,
and I2 may be provided for producing a mixture
By carrying out the glycerine vaporization step
of fatty acids, glycerine and water from glycerides
or saponification and glycerine vaporization steps
in the presence of a lubricating oil which does not ~ by the reaction between the glycerides and water,
volatilize in the glycerine vaporization step, a soap 25 usually in the presence o_f a catalyst. Reaction
chambers I0, I I and I2 may be of the autoclave
mixture comprising an anhydrous mixture of soap
type for operation under relatively high tempera
>and lubricating oil, which remains liquid in the
tures and pressures, for example 120 to 150 pounds
vapor separating chamber at temperatures below
per square inch and at a temperature approxi
the melting point of the anhydrous soap. may be
produced so as to lower the- temperature neces 30 mately at the boiling point of water at the pres
sure employed. In such processes, suitable cata
sary in the vapor separating chamber for effec
lyst are ordinarily employed such as small
tive separation of glycerine vapor. Also, by em
amounts of zinc oxide, calcium oxide, magnesium
playing mixtures of- compounds of alkali metals
oxide, caustic soda, sodium acid sulphate, sulfuric
and compoundsv of polyvalent metals as the
saponifying agent, anhydrous mixed soaps of 35 acid, etc. It is preferred, however, to carry on
the splitting operation 'in a batch operation at
alkali metals and polyvalent metals, which have
lower melting points than anhydrous alkali metal
substantially atmospheric pressure, an example
soaps, may be produced so as to lower the effec
of which is the “Twitchell" method which employs
sulfuric acid and benzene sulfonic acids or naph
tive glycerine vaporizing temperatures. Depend
ing upon the product desired, either or both of 40 thalene sulfonic acids as a catalyst at tempera
tures in the neighborhood of 212° F. Low tem
perature enzyme or lypolytic splitting steps are
soaps containing substantial amounts of alkali
particularly adapted to the present invention.
metal soaps and containing an excess of alkali
Although this type of splitting is known to the
while reducing glycerine destruction. Also if a
art and produces rapid splitting at low tempera
polyvalent metal soap containing a high boiling
tures and light colored products, it has not been
point lubricating oil is desired, the vaporization
step can be carried out in the presence of the
employed to any considerable extent because of
these operations may be employed to produce
the dimculty of resolving extremely troublesome
lubricating oil to reduce the melting point of the
emulsions produced in the splitting step. Such
resulting soap mixture so as to enable glycerine
recovery at a lower temperature. In many cases 50 emulsions have been diñlcult to handle even 1n
substantially complete separation of glycerine -in
substantially above 400° F. The employment of
evaporation or distillation steps for separating
glycerine, fatty acids and water. In the present
process where saponiiìcation of the fatty'acids is
a light hydrocarbon which vaporizes during the
produced prior to glycerine separation at- high
. vapor form can be obtained at temperatures not
vaporization step, in any case, assists in releasing 55 temperatures, this diiliculty is eliminated.
The reaction chambers I0, Il and I2 may be
glycerine vapor from the molten soap or soap
closed or substantially closed to the atmosphere
mixturel thus enabling glycerine vaporization to
and provided with an agitator I3 and a. heating
be carried on at temperatures not substantially
coil I4. The glyceridê to be split may be intro
above the melting point of the anhydrous soap
or soap mixture so long as this temperature is not 60 duced into the chambers through a pipe Il, and
water containing the catalyst or enzyme intro-_
substantially below 400° F.
'
duced into the reaction chambers through the
An object of the present invention is, therefore,
pipe I1. Although such reaction chambers need
to provide an improved process of producing soap
not be closed from the atmosphere for operations
from glycerides in which saponifying agents
which do not react readily with glycerides -are 65 at substantially atmospheric pressure, it is de
employed.
sirable to maintain the reaction mass out _of con
tact with the atmosphere and for this purpose
Another object of the invention is to provide an A
improved process of producing soap in which
closed reaction chambers may be provided with a
glycerides are ñrst split into glycerine and fatty
vent pipe I8 which may have a suitable pressure
acids, the fatty acids are saponiñed in the pres 70 relief valve so that a slight super-atmospheric
pressure may be maintained in the reaction
ence of the glycerine and glycerine removed in
chambers, if desired, and any steam or water
vapor generated therein vented to the atmos
vapor form from the resulting soap.
A further object of the invention is to provide
an improved process of producing soaps admixed
with lubricating oils to produce greases.
phere.
76
,
Depending upon the nature of the glyceride em
‘uu’ vill-.Huw u u
COMDÉUNDS»
5
2,403,41 3
ployed the nature of the splitting operation and
the amount of water relative to the amount of
glyceride, glycerides can be substantially com
pletely split by the Twitchell method at temper
atures between 210" and 220° F. in periods rang
ing between four and twelve hours and in a some
what shorter time and at lower temperatures by
the enzymc method. A large excess of water over
6
.
admixed with the saponifyins agent in the tank
28. In such case the tank 34 with associated pro
portioning pump 35 and heat exchanger 31 may
Abe eliminated. If alight hydrocarbon is employed
the most important consideration is that it be
present in the vapor separating step to aid in the
liberation of glycerine vapor and it may, there
fore, be added at any time prior to the intro
duction of the materials into the vapor separa
that necessary to react with the glycerides is pref
erably employed to force the splitting reaction 10 tion step. If a lubricating oil which has a boil
toward completion and the resulting mixture
ing point substantially above that required for
consists essentially of fatty acids, glycerine and
glycerine vaporization is desired in the final prod
water. Any small amounts of unsplit glycerides
uct, it .is likewise desirably added at some time
which may be present are split and the fatty acids
prior to the introduction of the materials into
saponified in succeeding steps of the process.
the vapor separation step.
'
By providing a plurality of reaction chambers,
The pumps 24, 29 and 35 may be driven by a
the reacted mixture may be withdrawn from one
variable speed electric motor 38 directly driving
of the chambers while splitting is progressing in
pump 24 with a variable speed device 39 connect
the other chambers. -For example, the mixture
ed between the motor and the pump 29 and a
of fatty acids, glycerine and water may be drawn 20 variable speed device 40 connected between the
from the tank I0 through the pipe I9 by open-.
pump 24 and the pump 35. This proportioning
ing the valve 2| while the valves 22 and 23 are
apparatus is shown merely by way of example
maintained in closed condition. This mixture
and any suitable proportioning apparatus known
may be Withdrawn by means of a proportioning
to the art may be employed, the preferred pro
pump 24 and delivered through heat exchanger
portioning apparatus being of the type shown in
2B to a mixer 21. A saponifying agent, for exam
the patent to Thurman No. 2,142,062 granted De
ple a slurry of aluminum hydroxide, if alumi
cember 27, 1938. The mixer 21 may be any suit
num soap is desired in the final product, may
able type of flow mixer, for example, one of the
be withdrawn from a tank 28 by meansof a pump
type shown in the patent to Thurman referred
29 and delivered through a heat exchanger 3l to 3 l) to above but may be a closed mechanical mixer.
the mixer 21. The tank 28 preferably contains
The heat exchangers 25, 3| and 31 may likewise
an agitator 32 driven from any suitable source
be of any suitable type capable of rapidly heating
of power for maintaining the solution or slurry
or cooling materials in -rapid stream ñow and
ofl saponifying agent in uniform condition, if nec
preferably include a coil 4| through which the
essary, and may also be provided with a heating 35 material to be heated or cooled is passed, sur
coil 33 to heat the saponifying agent. Thus the
temperature of the saponif'ying agent may be
rounded by a casing 42 through which any de
îilt'êiâ heating or cooling medium may be circu
maintained at temperatures up to those ap
proaching the boiling point of water. or even
By preheating the various materials delivered
higher so as to increase the solubility of the 40 to the mixer 21 in the heat exchangers 26, 3|
saponifying agent in water, if the tank 28 is closed
and 31 to a relatively high temperature. for ex
and capable of being operated under pressure.
ample temperatures in the neighborhood of 300"
a
Since the mixture including fatty acids and glyc
ly With the fatty acids in the mixture delivered
to the mixer from the glyceride splitting step.
In order to provide time for completion of the
reaction and to raise the temperature still fur
ther, the mixture from the mixer 21 may be passed
as concentrated as it is possible to maintain in a,
uniform pumpable admixture.
If it is desired to incorporate a lubricating oil
into the finished product, this may be done prior
to saponiñcation, for example by withdrawing a
stream of such lubricating oil from a tank 34 by
through one or more heat exchangers 43 and 44.
A pump 45, driven from any suitable 'source of
power,.may be employed to produce further mix
ing between the heat exchangers 43 and 44 and
to assist in forcing the mixture undergoing
means of a proportioning pump 35 and passing
the same through a heat. exchanger 31 to the
mixer 21. This operation is possible when the
by va rization, it is advantageous to incorporate
a. lig t hydrocarbon, such as a hydrocarbon in
the kerosene or fuel oil ringe, to assist in liberat
ing glycerine vapors in 'the vapor separation step.
Instead of supplying the lubricating oil or light
hydrocarbon or both from a separate tank 34
with a proportioning pump 35, either or both
may be admixed with the products of the split
-
as aluminum hydroxide are caused to react rapid
the saponifying agent solution or slurry may be
higher than any temperature reached in the va
porizing step of the process hereafter described.
Even if no lubricating oil is desired in the final
product or the lubricating oil desired in the final
product has a boiling point too low to be intro
duced prior to separation of water and glycerine
'
F. even such relatively inactive saponifying agents
erine usually contains a' large excess of water
lubricating oil has a boiling point substantially
.
55
saponification through the system.
In general .
the saponiñcation reaction will be substantially
completed in the heat exchanger 43 4and the last
heat exchanger 44 will be employed to introduce
further heat into the mixture entering the vapor
se'paration step. The pressure in heat exchanger
43 will ordinarily be suñìciently high to prevent
any substantial formation of vapor but the pres
sure in the heat exchanger 44 may be sufliciently
low to enable substantial amounts of water vapor
or light hydrocarbon vapors, if present, to be
generated. The temperature reached in the heat
exchanger 43 will ordinarily vary between 350°
and 400° F'. depending upon the nature of the
glyceride and saponifying agent employed while
ting operation in the reaction chambers I0, Il 70 the temperature reached in the heat exchanger
and l2 preferably just prior to starting the de
44 will ordinarily vary between 400° and 550° F.
livery of such material to the saponiñcation step
but in mos-.t cases will range between 420° t0 500"
of the process. For example, the lubricating oil or
F. also depending upon the nature of the saponi
light hydrocarbon or both may be introduced
fying agent and the glyceride employed.
through the pipe I6 or either or both may be 75
The substantially completely saponiñed mix
4
2,4os,41s
7
.
_
ture of soap. slycerine, water and vapors as well
as lubricating oil or light hydrocarbon, if present,
8
`
i
delivering the same to a iiow mixer I4 to which
the stream of molten anhydrous soap from the
vapor separating chamber 4l may also be de
livered. If necessary to maintain the resulting
is discharged into a vapor separating chamber
46 through nozzles 41 so as to flow down the in
clined lower walls 48 of the vapor separating 5 mixture of soap in fluid form after admixture
chamber. The walls 48 are preferably main
of the lubricating oil. the lubricating oil may be
tained~ at a temperature at least as high as that
passed through heat exchanger 66 to increase
of the entering materials, for example by means
its temperature before being delivered to the
of a heating jacket 49 through which any de
mixer 64. The heat exchanger 6B as well as
sired heating medium may be circulated. By 10 the heat exchangers 43 and 44, heretofore re
operating the vapor separating chamber 4B at
ferred to, may be of the same type as the heat
a temperature above the melting point of the
exchangers 2B, Il and 31. The mixer 54 Amay be
soap or soap mixture when anhydrous and main
of any suitable type such as described with ref
taining a relatively high vacuum therein, water
erence to mixer 21. The mixture of anhydrous
vapors, glycerine vapors and vapors of light hy 15 soap and lubricating oil may be delivered from
drocarbon, if employed, may be withdrawn from
the mixer B4 into any suitable cooling device, for
the vaporv separating chamber through a pipe
example a screw conveyor B9 provided with a
5I. It has been found that if the soap or soap
cooling Jacket 1|, and- the cooled material dis
mixture deposited in the vapor separating cham
charged from the process. Such screw conveyor
ber remains molten that glycerine can be sub 20 may be of the type shown in the patent to Thur
stantially completely separated therefrom along .
man No. 2,190,615 granted February 13, 1940.
with water and other vapors <at temperatures
Il.' the product contains a substantial amount
as low as approximately 400° F. with a vacuum
ranging from 281/2 to 29 inches in mercury. This
of lubricating oil so that a grease is produced
which flows readily after cooling, it is apparent
relatively’low temperature operation is possible 25 that other types of heat exchangers, for example
with many insoluble soaps such as aluminum,
calcium or magnesium soaps of the usual fatty
acids encountered in glycerides as these soaps
have melting points substantially lower than
one similar „to the heat exchanger I1, may be
employed to cool the grease before discharge to
the atmosphere.
'
With certain types of greases,.for example, cal
sodium or potassium soaps. ’I'he presence of a 30 cium greases, a slight amount off‘moisture is de
lubricating oil which does not volatilize in the _ sirable in the nnished product and one way of
vapor separating chamber will also in most cases
reduce the melting point of the soap mixture.
A thin film of molten material ?owing downl the
incorporating this moisture into the product is
to mix a small amount of water with the lubri
cating oil in the tank. l2, the mixture being main
walls of the vapor separating chamber 4l causes 35 tained uniform by means of an agitator 12. If no j
the glycerlne vapor to _be relatively easily liber
ated.
The vapors withdrawn from the vapor separat
ing chamber 46 through the pipe 5| may be de
livered to one or more oondensers 52 and Il con
nected to suitable receivers 54 and 50 respective
ly, As illustrated, a plurality of condensers can
be employed for fractionally condensing the vari
ous materials such as water, glycerine and light
lubricating oil is added to'the soap at this stage
of the process and a small amount of moisture is
desired in the finished product, it may be added
, from the tank 02 in the absence of lubricating
40 oil. If no lubricating oil is to be added to the -
liquid product from the; vapor separating cham
ber 48, it is apparent that the screw conveyor 09'
can be positioned directly below the vapor sepa
Y rating chamber 45 to receive the molten material
' hydrocarbon, the number of condensers and re
45 directly therefrom withoutthe employment of a
ceivers employed depending upon the number of
pump Il., It is also possible to introduce the
l fractions desired. A fractionating column may
lubricating oil. water or both directly into such
be employed instead of a plurality of condensers.
a screw conveyor.
If the saponifying agent employed is a carbonate
Instead of employing the batch splitting steps
so that relatively large amounts of carbon dioxide so described with reference to the reaction cham
are present lin the vapors withdrawn from the
,bers I 0, H and l2 of Fig. 1 a continuous splitting
vapor separating chamber, a carbon dioxide ab
operation producing substantially the same type
sorption tower 51 may be connected to the last
of mixtureas that produced in the splitting steps
receiver 56 so as to absorb the carbon dioxide
described with reference to F18. 1 maybe em
and relieve the load upon the vacuum pump 5l 55 ployed.L For example, as shown in Fig. 2 glycerides
employed to maintain a vacuum in the various
may be withdrawn from a tank 1I by means of
condensers, receivers and vapor separating cham
a proportioning pump 14 and passed through a
ber. A suitable carbon dioxide absorbing agent
heat exchanger 1I to a mixer 11. Water or
is an aqueous solution of sodium hydroxide which
water containing a suitable catalyst may be with
combines with the carbon dioxide to form sodi 60 drawn from a tank 'I8 by means of a proportion-V l
um carbonate, but other known agents such as
'ing pump 10 and passed through a heat exchanger
certain amines or ethanolamines may be ern
Il to the mixer 11. The water and glycerides
ployed.
,
may be heated to relatively high temperatures
In general it is preferred to maintain .a pool
under -pressure in the heat exchangers Il and
of molten anhydrous soap in the lower portion 65 1l, respectively, for example temperatures be
of the vapor separating chamber 46 and a stream
tween 300’ and 400° I". The mixer 11 may be of
of this molten anhydrous soap may be with
any suitable type such as described with refer
drawn from the vapor `separating chamber by
ence- to the mixer 21 of Fig. 1 and the resulting
means of a pump 6I. If the resulting soap is
mixture may be passed through a plurality of
to be employed in the manufacture oi' greases 70 heat exchangers, for example heat exchangers l2
and the lubricating oil employed therein is' not
and 83 wherein the mixture is subjected to rela
added prior to saponincation it may be' added
tively high' temperatures, for example tempera
to the stream of molten anhydrous soap. for
tures up to 600° F. at high pressures, for exam
example by withdrawing a stream of lubricating
ple pressures as high as 1000 to 1500 pounds per
oil from the tank 62 by means of a pump 83 and 'i5 square inch. Under these .conditions the glycer
CWDOUNDS,
41
Í'
ldes react rapidly with the water to liberate fatty
acids and glycerine.
A large excess of water is ordinarily employed
over that necessary to react with theV glycerides
so as to carry the reaction to substantial com
pletion, an amount of water equal in amount to
the amount of glycerides having been found sat
‘
10
ration can usually be carried on at a substan
tially lower temperature than is the case whe`
alkali metal compounds are employed as the
saponifying agent. The insoluble soaps in gen
el eral have a substantially lower melting point
than the soaps of alkali metals so that a molten
soap is produced at temperatures not substan
isfactory. Since the temperature of the mixture
tially above 400° F. As discussed above, glyc
discharged from the heat exchanger 83 will ordi
erine can be separated in vapor form at such
narily be higher than that desired in the saponi 10 temperatures if the _soap produced is molten.
fying reaction, another heat exchanger 84 may
Thus the present process enables insoluble soaps
be employed to cool the resulting mixture down
either in substantially pure form or admixed with
to temperatures, for example in the neighborhood
a lubricating oil to form a grease to be produced
of 400° to 450° F. This mixture may be supplied
rapidly from glycerides while at the same time
to the mixer 21 of Fig, l, for example by substi 15 glycerine is recovered. By fractionally condens
tuting the proportionìng pumps 14 and 'I9 of Fig.
ing this glycerine it may be recovered in concen
2 for the proportiom'ng pump 24 of Fig. 1. It is
entirely possible to make batch mixtures of the
trated substantially pure form.
It is of course
apparent that if any glycerine is desired in the
soap product that the temperature in the vapor
glycerine and water and splitting catalyst if used,
which are then delivered in succession through a 20 separating chamber may be somewhat lower or
series of heat exchangers such as the heat ex
the pressure somewhat increased so as to prevent
changers 82 and 83 so as to eliminate the propor
vaporization of all or a part of the glycerine.
tioning pumps 14 and 'I9 and mixer 11.
Nevertheless substantially all of the water can
The products of the saponiñcation process are
be removed from the soap even ifv substantial
substantially the same irrespective of whether the 25 amounts of glycerine are left therein so that an
glycerides are split in a batch operation as de
anhydrous soap or soap mixture is produced. If
scribed with reference to Fig. 1 or a continuous
water is desired as a component of the ñnished
operation as described with reference to Fig. 2.
product it can be added to the heated anhydrous
In any event the glycerides are ñrst split to ob
soap mixture before discharge from the process.
tain a. mixture of glycerine and fatty acids in
While I have described the preferred embodi
water which may contain some unsplit glycerides,
ments of my invention, it is understood that it
and a saponifying agent is then added -to sapon
may be varied within the scope of the following
ify the fatty acids and any unsplit glycerides.
Glycerine is then recovered or partially recovered
in vapor 'form from the resulting mixture of soap, 35
glycerine and water by separating glycerine and
claims:
-
l. The process of making soap and recovering
glycerine from glycerides, which comprises, split
water vapors from the soap so as to produce a
ting said glycerides lo produce a mixture of glyc
molten substantially anhydrous soap. If a light
erine, fatty acids anu water, adding a saponify
hydrocarbon is present during the vaporization
step, vapors of a light hydrocarbon will likewise 40 ing agent to said mixture to convert said fatty
acids into soap, and separating glycerine from
be removed in the vapor separation step and as
said soap.
sist in liberating glycerine vapors so as to some
2. The process of making soap and recovering
what lower the necessary vaporizing temperature.
glycerine
from glycerides, which comprises, split
As stated above. the present process finds its
ting
said
glycerides
to produce a mixture of glyc
chief utility in the production of insoluble soaps 45
erine, fatty acids and water, adding a saponify
such as aluminumy magnesium, calcium, lead,
ing agent to said mixture to convert said fatty
etc., soaps. The hydroxides or other alkaline
acids into soap, and separating water and glyc
compounds of materials forming insoluble soaps
erine from said soap by vaporizing said water
in general react slowly, if at all, with glycerides,
although calcium hydroxide reacts fairly rapidly. 60 and glycerine.
3. The process of making soap and recovering
Nevertheless, the present process can be advan
glycerine
from glycerides, which comprises, split
tageously employed with calcium hydroxide as
ting said glycerides to produce a mixture of glyc
~ the saponifying agent as substantially complete
erine, fatty acids and water, adding a non-caustic
saponification can ~be more readily obtained.
The process can also be_ employed for the pro 55 saponifying agent to said mixture to convert said
fatty acids into soap, and separating glycerine
duction of soluble soaps such as sodium or po
in vapor form from said soap.
tassium soaps. If the hydroxides of these mate
4. The process of making soap and recovering
rials are employed as the saponifying agent the
glycerine from glycerides, which comprises, split
ting said glycerides to produce a mixture of glyc
However, if carbonates or other alkaline com 60 erine, fatty acids and water, mixing a flowing
pounds of the alkali metals which do not react
hydroxide readily saponiiies with the glycerides.
stream of said mixture with a stream of saponify
ing agent so as to convert said fatty acids into
soap, delivering the resulting stream into a vapor
readily with glycerides are employed as a saponi
fying agent, the present Aprocess is advantageous
in that substantially complete saponiñcation is
easily obtained. The use of such non-_caustic
compounds of the alkali metals is advantageous
as substantially no glycerine destruction occurs
even if an excess of the saponifying agent is em
ployed and the relatively high temperatures, for
example temperatures about 550° F., necessary
for producing an anhydrous molten alkali metal
soap are used in the process.
When hydroxide or other alkaline compounds
of elements producing insoluble soaps are em
ployed as the saponifying agent the vapor sepa
es
separating zone at a temperature sutliciently high
to vaporize said glycerine. separating glycerine
in vapor form from said soap insaid vapor sep
arçting zone. and separately withdrawing glyc
erine and soap from said vapor separating zone.
„1o. The process of making soap and recovering
glycerine from glycerides, which comprises, split
ting said-glycerides to produce a mixture of glyc
erine, fatty acids and water, adding a saponifying _
agent to said mixture to convert said fatty acids
into soap, delivering the resulting mixture into a
vapor separating zone at a temperature sufficient
2,403,413
' ll
ly high to vaporize said glycerine while said re
sulting mixture is admixed with a lubricating oil
which does not vaporize in said vapor separating
stream oi' said mixture with a stream of saponi
fying agent comprising a polyvalent metal hy
zone, maintaining said zone under vacuum con
droxide so as to convert said fatty acids into
soap, delivering the resulting stream into a vapor
ditions and at a temperature sui’ñciently high to
cause glycerine to separate from said soap in
to vaporize said glycerine, separating glycerine
vapor form, and'separately withdrawing glyc
in vapor form from said soap in said vapor sep
separating zone at a temperature sufl‘lciently high
arating zone, and separately withdrawing glyc
erine vapor and soap admixed with said lubricat
erine and soap from said vapor separating zone.
ing oil from said zone.
10. The process of making soap and recovering
6. The process of making soap and recovering 10
glycerine from glycerides, which comprises, split
glycerine from glycerides, which comprises, split
ting said glycerides to produce a mixture of glyc
ting said glycerides to produce a mixture of glyc
erine, fatty acids and water, mixing a. ñowing
erine, fatty acids and water, adding a saponify
ing agent consisting essentially of a polyvalent
stream of said mixture with a stream of saponi
metal hydroxide to said mixture to convert said 15 fying agent comprising a polyvalent metal hy
fatty acids into soap, delivering the resulting
droxide so as to convert said fatty acids into soap,
,delivering the resulting stream into a vapor sep
mixture into a vapor separating zone at a tem
arating zone at a temperature suiiîiciently high
perature suiiiciently high to vaporize said glyc
to vaporize said glycerine, separating glycerine
erine while said resulting mixture is admixed
with a lubricating oil which does not vaporize- 20 in vapor form from said soap in said vapor sep
arating zone, separately withdrawing glycerinein said vapor separating zone. maintaining said
and soap from said vapor separating zone, and
zone under vacuum conditions and at a temper
adding a lubricating oil to said soap during with
ature'sufiiciently high tc cause glycerine to sep
arate from said soap in vapor form, and separate
drawal thereof.
ly withdrawing glycerine vapor and soap admixed 25
1l. The process of making soap and recover
ing glycerine from glycerides, which comprises,
with said lubricating oil from said zone.
7. The process of making soap and recovering
splitting said glycerides to produce a mixture of
glycerine from glycerldes, which comprises, split
glycerine, fatty acids and water, by reacting water
ting said glycerides to produce a mixture of -glyc
with said glycerides at a relatively low temper
erine, fatty acids and water, adding a saponify 30 ature in the presence of an enzyme, mixing a
ing agent consisting essentially o'f an alkaline
ilowing stream of said mixture with a stream of
earth metal hydroxide to said mixture to convert
saponifying agent so as to convert said fatty acids
said fatty acids into soap, delivering the resulting
into soap, delivering the resulting stream _into a
mixtureinto a vapor separating zone at a tem
vapor separating zone at a temperature suñlcient
perature sui’dciently high to vaporize said glyc
ly high to vaporize said glycerine, separating
erine while said resulting mixture is admixed
glycerine in vapor form from said soap in said
with a lubricating oil which does not vaporize '»
in said vapor separating zone, maintaining said
vapor separating zone, and separately withdraw
ing glycerine and soap from said vapor separat
zone under vacuum conditions and at a temper
ins zone.
ature sufiiciently high to cause glycerine to sep 40 12. The process of making soap and recovering
arate from said soap in vapor form, and sepa
glycerine from glycerides, which comprises, split
rately withdrawing glycerine vapor and soap ad
ting said glycerides 'to produce a mixture of glyc
mixed with said lubricating oil from said zone.
erine, fatty acids and water, by reacting said
8. 'I'he process of making soap and recovering
glycerides with water in the presence of a split
glycerine from glycerides, which comprises, split 45 ting agent at a temperature not substantially
ting said gLvcerides to produce a mixture of glyc
above the boiling point of water, mixing a flow
erine, fatty acids and water, adding a saponi- `
ing stream of said mixture with a stream of
fying agent consisting essentially of a compound
saponifying agent so as toconvert said fatty acids
of an alkaline earth metal to said mixture to
into soap, delivering the resulting stream into a
convert said fatty acids into soap, and separat 50 vapor separating zone at a temperature suf
ing water and glycerine from said soap by vapor- y
ñciently high to vaporize said glycerine, sep
izing said water _and glycerine.
arating glycerine in vapor form from said soap
9. The process of making soap and recovering
in said vapor separating zone, and separately
glycerine from glycerides, which comprises. split
withdrawing glycerine and soap from said vapor
ting said glycerides to produce a mixture ot glyc 55 separating zone.
erine, fatty acids and water. mixing a nowing
BENJAMIN H. THURMAN.
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