Патент USA US2403413код для вставки
41 äomPouNnS. y July 2» 1946» Í ` » ' B. H. THURMAN 2,403,413 PRocEss oF MAKING soAP Filed llarch 23, 1942 Whe. ë ,i î 62/ il / 83 Si? 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 A lubricating oil may be added to the materials prior to the vapor separating step or to the soap withdrawn lfrom the vaporizing step depending upon the nature of the lubricating oil and the temperatures employed in the vapor separating to produce water soluble soaps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.