Noy. 7, 1939, B. H. THURMAN 2,179,001 PROCESS FOR THE CONTINUOUS RECOVERY OF GLYCERINE FROM SOAP Filed June 14, 1937Patented Nov. 7, 1939 2,179,001 PROCESS FOR THE CONTINUOUS RECOV- ERY OF GLYCERIN FROM SOAP Benjamin H, Thurman, Bronxville, N. ¥., assien- ‘or to Refining, Inc., Reno, Nev., » corporation of Nevada, Application June 1, 1937, Serisl No. 148,240 11 Claims. (C1. 260—418) 2,179,001 UNITED STATES PATENT OFFICE ‘This invention relates to a process for the treat- ment of soap and more particularly to a process in which a mass of soap made in a kettle, or serie Is proceed to remove volatiles there- 5 from. In the commercial manufacture of soap mix- ture of soap and water is produced. If glycerides are employed as the saponifiable materiel, this mixture also contains glycerin. ‘The removal and 10 recovery of the glycerin from soap mixtures, as hheretofore practiced, is more difficult and time consuming than the original preparation of the soap mixture, In prior processes, a strong salt solution is added to the mixture in order to throw 15 the soap out of the solution while at the same time dissolving the glycerin. ‘Then, after the salted mixture has been boiled for a considerable time, it is allowed to settle for several hours, ‘The soap lye which separates contains much of 20 the elycerin but a portion remains associated with: the soap. ‘To further purify the soap and remove additional glycerin therefrom, it is necessary to repeatedly subjest the soap to washing or salting out operations. 125 Also the recovery of the glycerin from the soap lye from prior process requires a long and com- plex process. It usually involves chemical treat~ ment followed by evaporation of water, resulting in an appreciable loss of glycerin. ‘The orude a0 glycerin thereby obtained has to be further treat ed by distillation and other processes, resulting in additional loss of glycerin, before s commer- cially pure glycerin is obtained: “The soap mass after the glycerin has been with- 35 drawn therefrom is then treated to remove mols ‘ture if a solid or powdered soap is obtained. ‘The various’ processes of removing this moisture are also expensive and time consuming, ‘The present favention eliminates all of these difficulties and 40 rapidly produces extremely pure glycerin and soap in marketable form. ‘In accordance with the present invention, the slycerin and water are removed from a soap mix- ture by vaporizing the same and the soap can be 48 recovered in substantially anhydrous and glyc- erin-free form. ‘This process of separating elyc- erin from the soap 1s continuous and large quan- tities may be treated in a relatively short time. It is, therefore, an object of the invention to 40 provide an tmproved process of separating vola~ tiles from soap mixtures such as are produced in the manufacture of soap. "Another object of the invention is to provide fa continuous process of recovering siycerin of In addition the soap mixture can by the pres- ent process be subjected to temperatures and pressures far in excess of those possible in the conventional methods of processing soap mix- tures even if no glycerin is present or it is not 5 desired to recover the same. By such high tem- ‘peratures various colored and odorous impurities contained in many soap making materials, for example, higher alcchols such as sterols, may be vaporized and the vapors separated from the soap 10 in an evaporating zone thus producing a purer soap. Also many insoluble impurities which ordi- narily color the soap or later break down to sive the soap an undesirable odor, for example, insol- uble proteinaceous materials, are broken down by 16 ‘the high temperatures, capable of being employed in the present process, into non-odorous or color~ Jess compounds or rendered vaporizable or soluble so that they may be removed by evaporation or ‘washed out of the resultant soap. ‘Thus very low gp grade soap mixtures, such as cottonseed or other soapstock resulting from refining operations or soap mixtures made from low grade fats, can be treated by the present process to produce much. Lighter colored and better grades of soap than can 9 be made by conventional processes. ‘The high temperature treating step may be of such short ‘duration that the soap is not injured.even though ‘prolonged treatment of the soap at the high tem- erature would decompose the same. Tt is, therefore, another object of the iriver tion to subject a soap mixture to high temper ures in order to vaporize or break down colored, and odorous impurities. "A still further and quite important object of 35 my invention 1s to provide a process wherein saponification may be effected in a kettle, for ex- ‘ample, under relatively low temperatures and for f relatively long period of timt after which the Tesulting mixture, including soap, glycerin and gy water is continuously and quickly passed through. & heating zone where it is subjected to an ele- ‘ated temperature for @ short period of time be- fore continuously discharging it into a vacuum ‘chamber where the glycerin, water and other ma- 45 terials are vaporized therefrom and separately condensed while the soap is discharged from the vacuum without breaking the-same. ‘Still more specifically, the invention compre- hends the employment of a pumping mechanism 99 interposed between the relatively large kettle con- taining the saponified or partially saponified product and the coll, constituting the heating zone, for performing the dual function of fore~ ng the saponified mixture through the coll at ggw 0 4s 50 85 0 6 2 a substantial rate of flow to maintain the mix- ture while it is subjected to high temperatures and of more thoroughly mixing the saponified ‘material, thereby providing for contact between ‘ny unseponified material and saponifying agent to further the saponification before the mixture Teaches the high temperature zone. Other objects and advantages of the invention ‘will appear in the following description of the preferred embodiments of the invention which are described in connection with a schematic draw- ing of a suitable apparatus, of which: ‘Pigure 1is an assembly view of the entire appa- ratus, and: Figure 2s a fragmentary view in section show- {ng an arrangement of nozzles in the evaporating chamber, Referring to the drawing, (0 indicates, in gen- eral, apparatus suitable for carrying on a saponi- fication step; 11 indicates @ heating device for heating a soap mixture; 2 indicates in general an evaporating chamber which is provided with @ conveyor system indicated at 13 for removing soap from the evaporating chamber; and (4 indi- catesa condensing system for condensing glycerin, and water vapors. ‘The apparatus (0 for making soap mixture may include conventional soap Kettles 18 and 18, pro- vided with heating jackets 17 through which steam or other heating medium may be passed by the pipe 18. Pipes 19 and 20 are provided for introducing a measured quantity of a saponifiable material and a saponifying reagent, respectively. These materials are mixed in the kettle by an agitator 2/ driven by a motor 22 while the mate- rials are heated by the steam jacket (7. The saponifying reagent, which is usually a caustic alkall, reacts with the saponifiable material to form a soap mixture, Duplicate kettles will ordl- narily be Provided so that soap can be made in one kettle while the soap mixture fs being with- drawn from the other and processed. Instead of ‘making the soap mixture in the Kettles illustrated, it may be produced in other apparatus and de- lvered to the Kettles from which it is supplled to the remainder of the process. For withdrawing the soap from either kettle, pipes 23 and 24 leading from the bottoms of the Kettles are provided and are connected to a pipe 28 leading to a pump 26. Valves 27 and 28 are positioned in the pipes 24 and 24, respectively, in order to provide for withdrawing soap from elther Kettle. Also a pipe 29 connected to pipes 23 and 24 through valves 30 and 31 may be employed for diverting portions of the soap mixttre to other processes or for cleaning purposes. ‘The soap mixture in the kettles should be maintained in substantially uniform admixture during with- drawal of the same as, for example, by the agitators 21 or by passing steam through the mix- ture, and should be rendered sufflcfently fluld to enable it to be pumped through the process by heating or dilution, Pump 28 may be any type of pump suitable for forcing the soap mixture under a relatively ‘high pressure through @ heating coll #2 post. toned in a casing 33 forming part of the heating device 11. Heat may be applied to the coll by any suitable means, for example, by burner 34 in the lower portion of the casing 33. In order to control the amount of heat applied to the coll a sultable thermostatic device 38 may be employed for controlling the amount of fuel- delivered to the burner 34. Such a device may include @ ‘member 38 into which the heated materia's from 9,179,001 the coll 3° are delivered by the tube 37 so that these materials flow in contact with the walls of the member 36 and are discharged through a Pipe 38, In the device shown, the products of combustion from the burner 34 also contact the member 36 so that the temperature of this mem- ber is determined by both the temperature of the materials discharged from the coil 32 and that of the products of combustion. A valve 39 4s connected to one end of the member 36 so that expansion due to increase in temperature of this member partially closes the valve to reduce the flow of fuel to bumer 34. Likewise a decrease in temperature of the member 35 increases the flow of fuel to burner 34. ‘The normal position of the valve 39 can be controlled by a hand-wheel 40 mounted upon shaft 41 rotatively attached to one endof the member 38 and screw-threaded through, ‘@ member 42 attached to the casing 33. By ad- Justing the hand-wheel 48, any desired tempera ture of the materials discharging from the coll 32 can be automatically maintained. Any desired pressure may be imposed upon 8 mixture in the coll 32 by the pump 26 and this Pressure may be maintained by valve 43 in the Pipe 38 or by a restricted discharge orifice in the nozzles 44 positioned in the evaporating chamber {2 Alternatively, if desired, the diameter of the tube forming the coil 32 may be made sufficlentiy small to maintain the desired pressure, If glycerin is to be recovered, the soap mix- ture is heated in the coil 32 to a sufficient tem. perature to cause the glycerin. thereof to be Vaporized when discharged into the evaporating chamber (2 and is maintained out of contact with the atmosphere in its heated state. As herein. after explained, the pressure and temperature in the coil 32 may be regulated, if desired, so that water or glycerin vapors are generated in the coil 32. ‘The pressure at the discharge end of the coll will depend upon the temperature employed 80 as to secure the desired amount of vaporization in the coll. ‘The evaporating chamber may include an inner closed to the atmosphere and having a heating Jacket 48 positioned therearound. Steam or other heating medium may be admitted to the heating jacket 46 through a pipe 47 and the heat~ tng Jacket is preferably surrounded by an instlat= ing covering 4%. Tt has been found advantageous todirect the mixture discharge from the nozzles 44 against the heated walls of the evaporating chama- ber so that the mixture flows down these walls in & relatively thin film and the glycerin and water Vapors are more easily liberated. A preferred ar. rangement of the nozzles 44 to accomplish this purpose is shown in Pig. 2. Tt will be noted that the Mberated vapors are not required to pass through & spray of materlal delivered into the evaporating wardly through the central portion of the cham. ber. By this arrangement entrainment of quid or solid: materials in the vapors leaving the evaporating chamber is substantially eliminated, are withdrawn through the pipe 49 and en- trainment separator 48" to a condenser $8 DIO. Vided with a receiver 8/. The entrainment sepa rator 49° removes any traces of solld or lqulds the vapors and returns them through pipe to the evaporating chamber. The entrainment, ‘separator is preferably provided with a heating facket 1° to prevent condensation of glycerin ‘{theretn, In the condenser 61 most of the glycerin 10 6 2s 60 Er)0 5 9,170,001 vapors are.condensed and glycerin flows into the receiver 61 while the water vapors are withdrawn from the receiver 1 through a pipe 62 to a water condenser §3 in which they are condensed ‘and the resulting water flows into a receiver ‘A vacuum pump $8 withdraws uncondensed vapors from the receiver $4 and maintains a ‘vacuum throughout the condensing system 14 and evaporating chamber 45. Suitable cooling means (not shown) may be provided for the condensers. 50 and 83 and the temperature therein controlled so that fractional condensation of the water and glycerin takes place. A fractionation column may be employed instead of separate condensers, if desired, ‘The condensate from the various re- ceivers may be removed through the pipes 86 and 51, for example, by pumps (not shown). small portion of glycerin ordinarily is found admixed with the water in recelver‘Bt and this water may be employed as part of the water in the saponifica~ tion step so that the glycerin is subsequently re- covered in the process. A greater number of condensers may be provided if a greater num- bber of condensate fractions are desired. ‘The heating jacket 48 around the evaporat- ing chamber 45 supplies additional heat for vaporizing glycerin and in some instances it is desirable to furnish still more heat by injecting steam, preferably superheated, into the evaporat~ ing chamber by a pipe 60. ‘This steam also has a further function of assisting in berating the glycerin vapors froin the soap and carrying them to the condensing system 14. ‘In order to remove substantially all of the glye- erin from the soap,,the temperature in the evaporating chamber 45 must usually be suMl- lent to cause the soap to be in a molten or plastic condition, although the soap may deposit in the bottom of the evaporating chamber in a powdered form with certain types of fat, particu- larly if the conditions are such that all of the giycerin is not vaporized. - However, if glycerin is to be evaporated, the soap collecting in the bottom of the chamber 45 is at a temperature such that contact with the atmosphere will cause deterloration. The soap must be promptly re- moved from the evaporating chamber as the tem- perature therein is sufficient to cause deteriora- tion of the soap if it is maintained at this tem- perature for a prolonged length of time. It is, ‘therefore, necessary to promptly remove the ssp and cool the same hefore it is allowed to come in contact with the atmosphere. ‘A sultable apparatus for this purpose is the conveyor system 13. ‘This system may include a screw conveyor 61 having a casing 62 opening into the bottom of the evaporating chamber 48. ‘The inclined walls 63 of this chamber direct the soap into the conveyor casing 62. Jackets 64 and 665 surround tlie conveyor casing 62 for heating or cooling the same. Either a cooling medium or hheating medium may be pasted. through the jacket 68 depending upon the temperature of the soap in the conveyor. Tt is necessary that the soap be sitficiently solld before leaving the con- veyor system that it effectively plugs the dis- charge from the conveyor and in some cases this may require cooling by the jacket 65, although ordinarily a heating medium will be passed through this jacket in order to help maintain the temperature in the evaporating chamber 45, ‘A cooling ‘medium is passed through the jacket 64 in order to cool the soap. Also the conveyor shaft 68 may be made hollow and may be p1 vided with an inner pipe 61 so as to enable a 3 heating or cooling “medium to be introduced through the pipe 67 and discharged through the pipe €8 connected to the pipe 61 through a sult- ble packing gland 64”. ‘This last means pro- ‘Vides an extremely sensitive device for controlling the temperature of the soap being discharged by the conveyor #1. In order to asclst in causing the soap to be discharged by the conveyor 61, stationary members 69 extending through the ‘conveyor casing may be provided to prevent the Soap mass from turing with the conveyor. Slots 40 are provided in the screw portion of the con- ‘yeyor to receive the members 68. It has been found advantageous to enlarge the conveyor shaft adjacent the discharge end as at 68’, in order to provide a tapered and restricted discharge pas- ‘age to assist in casing the soap mass to seal the conveyor against entrance of air to maintain the vacuum in the evaporating chamber. ‘The sealing of the conveyor may also be assisted by reducing’ gq the pitch of the screw adjacent the discharge end thereof as shown in the drawing. ‘in order to further cool the soap it may be toreed through a grid, indicated at TI, formed of small tubes passing through the discharge portion ff the conveyor 61, ‘The grid 11 also assists ma- terially in maintaining a seal for the vacuum in the chamber 45. Tf has been found that adai- tional vapors can be withdrawn from the con- ‘veyor casing 62 by a vent 12, preferably leading to the vapor pipe 4 Preferably the conveyor 61 discharges into a second conveyor 13 positioned at right angler thereto and provided with @ cooling Jacket 14 although a single conveyor may, in some in- Stances, be sufflelent. ‘This conveyor may be of the same type as conveyor 61 and discharges through a valve 18 to the atmosphere. "This valve is employed in starting up the apparatus in order to maintain a vacuum in the chamber 48 before the conveyor system becomes filled with soap. ‘The conveyor shafts are rotated by means of the sprockets 78 and are provided with bearings 17 adjacent the sprockets, but no bearings need be employed at the discharge end of the conveyors. 48 ‘A pipe 11’, leading into the inlet end of the sec- ond conveyor 14 may be provided for the intro- Guction of other materials into this conveyor for admixture with the soap therein. ‘The conveyor serew moves the soap away from this portion of 50 the conveyor so that a low Dressire space is pro- vided for the introduction of materials. ‘Thus ‘water for rehydrating the soap to any desired ex- tent or perfume or soap bullders or fillers may be Introduced and mixed with the soap. ‘in carrying out the process of the present in- vention batch of ‘soap 1s made in one of the Kettles 16 or 16 or other suitable apparatus and delivered by the pump 26°to the heating device Il, ‘The temperature during, saponification the proportions of materials used. may be those Known to the prior art. ‘Thus, temperatures in the order of 150 to 212° F. may be employed or even higher temperatures up to, for example, 450° F, if closed receptacles are provided so that saponification is under pressure, may be em- ployed in the saponifeation step without danger of injuring the soap or soap making materials ‘The agitation should be continued during with- drawal of the soap mixture in order to maintain the mixture substantially uniform. ‘The pump 26 not only provides pressure for forcing the Materials through the heating deviée and into the evaporating chamber 48 but also aids in fur- ther mixing the materials passed theretiiough. 78 6 7010 0 4 ‘The coll 42 has been found to provide efficient heating without local overheating, but any other type of heating device in which the materials can be heated to a high temperature and under pres sure without local overheating may be . Also the thermostatic device 35 performs a fur~ ther mixing function immediately before the ma- terials ate delivered into the evaporating cham= ber 48, although any other type of mixing device may be substituted therefor and in many ins stances such mixing has been found to be un- Recessary. The temperature to which the ma- terials are raised in the heating device will de- Pend upon the type of glyceride or fat being treated, and in general these temperatures will bbe between 450° and 620" P. As has been indi- cated before, it is generally necessary to have the soap deposited in the evaporating chamber in a molten or plastic condition In order to satis~ factorlly recover the glycerin, and for this purpose the temperature of the mixture introduced into the evaporating chamber should be sufficiently. high to produce such molten or plastic soap. Even, it glycerin is not present or is not recovered, It may be desirable to employ temperatures in the upper portion of the above range in order to Vas orize or break ‘down impurities in the soap. Tt is important that the material subjected to the ‘higher temperatures be substantially completely saponified as such temperatures, in many cases, tend to discolor glycerides and fatty acids, In many cases, soap mixtures from commer- cial soap making processes may contain unsapon- ifed fatty acids or glycerides occluded in soap masses or particles and these may even be pres ent in the finished soap from prior processes, ‘The present invention is particularly adapted for handling such soap mixtures since the rapid flow through at least the first part of the heating zone along with the passage of the material through the soap pump and connecting pipes breaks down any agglomerations of soap and un. saponified material and enables the unsaponified material to be substantially completely sapon'fled. Even in cases where fatty acids are employed as the saponifiable material so that no glycerin is Present in the soap mixture or it is desired to leave glycerin in the treated soap, a higher tem- Perature is employed in the heating zone than in the saponification step. ‘This tem- Perature/must be sufficient to rapidiy vaporize the water either in the heating zone or in the evaporating chamber and the present process Provides for rapidly heating the soap mixture to this temperature so that the soap mixture is not subjected to the higher temperature for prolonged periods of time. ‘Thus the saponification step may be carried on by heating to relatively low temperatures over considerable periods of time so as to obtain substantial saponification without danger of injuring the soap or saponiflable ma~ terial by hich temperatures. The temperature may then be rapidly raised in the heating zone and the volatiles promptly removed 50 that the soap mixtures are subjected to the higher tem= erature for a brief period as compared to the time of treatment in the saponification step. A period of 2 to 5 minutes is usually sufficient for the entire heating step. ‘The temperatures neo essary to vaporize the water do, however, accel- erate the saponification reaction and even the Short period of treatment at the higher temper atures, accompanied by rapid flow of the soap mixture, substantially completes the saponifica tion of the unsaponified materials, Because of 2,179,001 the rapid saponification in the heating zone, par- fal saponification only may be accomplished in the prior saponification step and excellent re- alts obtained by completing the saponification in the heating step. If unsaponifted fatty acids or glycerides are present at the highest temper- ‘ature in the heating zone, this temperature should not be above the “lash point” of the tunsaponifled materials, When the temperature ts raised above this flash point, as is usually necessary to vaporize glveerin, care should be taken that saponifica- Hon is substantially complete before this tems Perature is reached, since such temperatures are ikely to discolor unsaponitied fatty acids or slye= 1 erides as above indicated. Even in this ease, ‘however, the first or lower temperature portion of the heating zone may be employed to complete the saponification of unsaponified material since the temperature progressively increases during the 9 ‘Passage of the mixture through the heating tone and the saponification reaction proceeds very Tapldly as the temperature increases especially it the material being heated has been more thor oughly mixed by passage through the soap pump ‘and connecting pipes. ‘The invention therefore provides an extremely inexpensive and quick process, Moreover, by reason of the rapidity of flow of the partially or wholly saponified mixture through the coll 32,'a 31 high temperature may be imposed thereon suifi~ lent to flash off not only the glycerin and water but otter impurities as well, without detrimen- tally affecting the soap because of its momentary exposure to the elevated heat treatment ard the 31 ‘fact that saponification has proceeded under rela tively low temperatures and for a relatively tong Period of time in the kettle or other receptacle 17, An important advantage of the present inven tion is that various types of volatile saponificas tion accelerators, for example, beta naphthol, can be employed in the saponification step even though they are undesirable in the finished soap, Such vecatile accelerators can be substantially ‘completely removed from the soap in the evap. grating step after they have performed thelr function of decreasing the time necessary for the saponification step. On the other hand certain non-volatile saponification accelerators have val- uable anti-oxidant properties in the finished soap and can be retained therein by the present proc. ess even though they are water soluble and would be to a large extent removed by the washing or glycerin removal steps of conventional processes. In either case, in addition to shortening the time necessary for the saponification step, the accel” erator assists in substantially completely saponi- tying the saponiflable material before high tem= Peratures which would injure the same are Feached. ‘The pressure imposed by the pump 26 must be Sufficient to allow the desired temperature to be attained. In actual operations for the recovery of glycerin, the temperatures and pressures are ordinarily controlled so that water vapors and preferably some glycerin vapors are formed in the heating device 11 at the pressure therein. Usually it is found desirable to thus vaporioe substantially all of the water. Such operation perndts more heat to be imparted to the mix. ture and requires less vaporization with conse uent ‘absorption of heat in the evaporating chamber 45. Sufficient heat must be supplied to the evaporating chamber elther from the heating device 11 or by other means to maintain a va 769,179,001 porlzing temperature for the glycerin therein, By forming at least part of the vapors in the heating device 32, less additional heat is required to be delivered to the evaporating chamber 4 although in many cases, it is possible to carry fon the present process without forming vapors in the heating device 22, : ‘The temperature of the soap deposit! in the evaporating chamber will depend upon the amount of glycerin to be recovered therefrom fand the nature of the saponifiable material being treated. Certain soaps, for example, those from the lighter fatty acids, will be molten at 455° F., while others require temperatures as high as 565° P. In order to vaporize the glycerin in the evaporating chamber it Is preferable that as near f perfect vacuum as possible be maintained in the evaporating chamber and that heat be sup- plied to the evaporating chamber either by means of a heating Jacket 46 or by superheating steam through the pipe 60. Both of these expedients may also be employed. “Thus the present invention provides an im- proved process which eliminates the expensive And time consuming process of removing volatiles from soap made by conventional processes. The saponifying reaction should be substantially com- plete before the materials are heated to a glycerin ‘Yaporizing temperature in order to prevent pos- ible discoloration of the fatty acids or glycerides. Giycerin can be recovered in a relatively pure and concentrated form and substantially all of the glycerin can be obtained. Also, the soap may be produced in a commercially usable form sub- stantially free from glycerin. ‘The resultant soap from commercial soap making fats is extremely Soluble and can be readily reduced to a pow- ered. condition. Tt absorbs moisture readily and can, therefore, be rehydrated to any desired moisture content and further processed by any of the known means in the art for producing solid or powdered soap. ‘This application isa continuation in part of my copending application, Serial No. 32437, fled Suly 20, 1985. ‘while I have. described the preferred em- podiment of my invention, its understood that Tam not to be limited to the details thereof and ‘that the invention may be varied within the scope of the following claims. ‘What T claim is: ~ 1, A method of making soap by the reaction betiveen a saponifiable material and a saponity- {ng material, which method ineludes the steps of: saponifying ‘@ mixture of sald materials under heat while maintaining the temperature below that value at which discoloration due to traces ‘of unreacted saponiflable material will result, thus producing @ soap mixture containing soap, flyeerin and traces of unreacted saponifiable Iaterial; then processing said soap mixture to saponify” said traces of unreacted. saponifiable ‘material to produce a completely saponified soap product still containing glycerin; then heating Said soap product to a higher temperature and Subjecting same to a vacuum, the heating being Sufficient to cause vaporation of glycerin under sald vacuum conditions; separating. glycerin Vapor from the soap while maintaining the soap in molten, plastic or semi-plastic condition while subjected to said vacuum conditions and prompt- ly, substantially as soon as the soap has been deposited in said vacuum, removing the same ‘without impairing the vacuum. 2A method of making soap by the reaction between a saponiflable material and a saponity~ ing material, which method includes the steps of: saponifying ‘a mixture of sald materials under heat while maintaining the temperature below that value at which discolorization due to traces 5 of unreacted saponiflable material will result, ‘thus producing a soap mixture containing sosp, glyéerin and traces of unreacted saponifiable material; then continuously moving a stream of sald soap mixture into and through mixing zone and subjecting seme to a: mixing action while therein to produce a completely saponified soap.product still containing glycerin; then sub- jecting sald completely saponified product to higher temperature and moving same into o chamber maintained under vacuum, the tem- perature of said soap product being raised to such an extent that glycerin vapors will separate at the low pressure maintained in said chamber; continuously removing the separated vapor from. sald chamber at such rate as to maintain the vacuum therein and removing said soap from sald chamber substantially as quickly as the same is deposited therein and before injury thereto. 3. A process for making soap and separating ‘elycerin which comprises the steps of: mixing saponifiable glycerides with a saponifying re- agent in a saponification zone to effect substan- tial saponification such that heating of the re- sulting mixture comprising soap, water and slycerin will produce substantially complete saponification before the temperature of the mix- ture reaches that at which glycerin will separate {in vapor form when discharged into a vapor sepa- rating zone, maintaining a relatively low temper- 35, ature during sald saponification in said sapont- fication zone insu‘ficient to render the soap molten when anhydrous whereby discoloration due to traces of unsaponified saponifiable material is prevented, withdrawing a stream of said mixture from the saponification zone and rapidly advanc- {ing the same under pressure through a separate heating conduit, drastically heating the mixture uring its rapld'and turbulent flow through sald conduit to a’ temperature greatly in excess of ‘that shaintained in the saponification zone and sufficient to separate said glycerin and other im- purities when introduced to @ vapor separating zone, continuously discharging the mixture into ‘8 vapor separating zone while maintaining a tem- perature suffclent to render the resulting an- hydrous soap in a molten condition, continuously ‘withdrawing the glycerin vapors at 8 rate suff clent to maintain @ vacuum therein and con- tinuously removing the anhydrous molten soap from said chamber without impairing sald vacuum 4. A process for making soap ‘and separating. glycerin which comprises the steps of: mixing saponifiable glycerides with a saponitying re- agent in saponifying Kettle to effect substan- tially saponification such that heating of the resulting mixture comprising soap, water and glycerin will produce substantisliy complete saponification before the temperature’of the mix- ture reaches that at which glycerin will separate in vapor forma when discharged into a vapor sepa- rating zone, maintaining relatively low tem- erature during the saponification in said kettle, insufficient to Tender the soap molten when an- hydrous, withdrawing a small stream of sald mixture from the saponification kettle and rapld- ly advancing the same, under pressure, through a separate heating condult, abruptly elevating the Yemperature imposed upon the previously sapon)- 15 1s 30 oo 06 9,179,001 ‘fed mixture while passing through said separate ‘heating conduit during its rapid and turbulent flow therethrough, sufficient to vaporize said glycerin and other impurities, discharging the 5 soap and vapors into a vapor separating chamber while maintaining the temperature sufficient to render the resultant anhydrous soap in a molten condition, continuously withdrawing the glycerin ‘Yapors at a rate sufficient to maintain @ YACULm 10 in said vapor separating chamber and continu- ously and promptly removing the anhydrous molten soap, before injury thereto, from said chamber without impairing said vacuum. 5. The process as defined in claim 4 in which as the abruptly elevated vaporizing temperature is Umited to such a few minutes as to prevent in- Jury to the soap. 6. The nrocess as defined in claim 4 in which the relatively low temperature and pressure con- 0 ditions maintained in the Kettle during saponi- fication are insufficient to vaporize the glycerin whereby to prevent discoloration of the soap and wherein the temperature abruptly imposed upon. the heating conduit is not substantially less than 450° heating of the resulting kettle soap containing glycerin will produce substantially complete saponification before the temperature of the Kettle soap reaches that at which glycerin will separate in vapor form when discharged into a ‘vapor separating zone, thereafter pumping & stream of said kettle soap through a heating zone to rapidly heat the same to a temperature suit ciently high to cause substantially all of said glycerin to be separated in vapor form when , ‘Said stream is introduced into a vapor sepatat- ing zone and above the melting point of the soap when sald glycerin has been separated, intro- ducing the heated stream into a vapor separating chamber maintained under vacuum, continuously , withdrawing glycerin vapors, and promptly and continuously withdrawing purified soap from sald chamber before the same 1s damaged by high temperatures and while sealing said chamber from the atmosphere. 10. The process of making soap and rapidly separating glycerin therefrom which comprises! mixing a saponification reagent with a glyceride of @ fatty acid in proper proportion, substan- tially completely saponifying said glyceride at @ 2 temperature below the vaporization point of glycerin and below the point at which discolora- Hon due to traces of unsaponified saponifiable material will result, thereafter rapidly heating a stream of the substantially completely reacted 5; mixture out of contact with the air to a tem- erature which will cause glycerin to be separated tn vapor form when sald mixture is introduced into @ vapor separating zone maintained under vacuum, introducing the heated stream into sald 5; vapor separation zone whereby said glycerin is soap is deposited in'said chamber, withdrawing Vapors at a rate which will maintain said vacu- 4 um, and rapidly withdrawing said soap before ‘the same has been damaged by said glycerin separating temperature, 11. A two-stage process for making soap which comprises the steps of: mixing a saponification 4: Teagent with a glyceride of a fatty acid in proper Proportions, substantially completely saponilying sald glyceride at a temperature below the vapori- zation Doint of glycerin and below the point at Which discoloration due to traces of unsaponified 9 material will result, thereafter elevating the tem- erature of the mixture to a degree which will eause glycerin to be separated in vapor form when said mixture is introduced into a vapor separating zone, introducing the heated stream into said vapor separation zone whereby said glycerin is substantially immediately separated in Vapor form and anhydrous substantially slycerin free soap is deposited in said chamber, withdrawing sald vapors from said zone and go rapidly withdrawing sald anhydrous soap sub- stantially as quickly as the same is deposited in sald zone and before the same has been damaged bby said glycerin separating temperature. BENJAMIN H. THURMAN. 5