Nov. 19, 1946, L. SENDER 2,411,469 MANUPACIURE OF soxP Filed Nov. 25, 1943 a a = * Ql g a x 5 zg ow aa =e ge & gS eo x a § vg Ss = 1] 1 x S Oe « \E § Qs nid oS x “LS x 2 s—i_ < z xb = g KS § ° H g KR << N x N | sy J : (NVENTOR WITWESS: a SS Legoale Sende Mellel, ay Maurie, A, Cred ATTORNEY.Patented Nov. 19, 1946 UNITED STATES 2,411,469 PATENT OFFICE 2,411,469 MANUFACTURE OF SOAP Leopold Sender, Baltimore, Md, assignor to The ‘Sharples Corporation, Philadelphia, Pa., a cor- poration of Delaware Application November 25, 1943, Serial No, 511,706 1 Claim, 1 ‘The present invention relates to the art of soap making, and was conceived as a method of making soap continuously with the afd of cen- trifugal separators. Processes for the manufacture of soap by pass~ ing a saponifying reagent continuously into con~ fluence with @ source of fat, saponifying the fat by passize of the mixture at saponifying tem- perature continuously through mixing apparatus, and separating spent reagent from soap by cen- ‘trifugation are described and claimed in the pa- tents of Ashton 'T. Scott, 2,900,749 and 2,300,750, of November 3, 1942. ‘The present invention is primarily a development and improvement with respect to the procedure of these two patents. In the processes of the above-mentioned Scott Patents, the fat 1s continuously saponified by treatment with a saponifying reagent such as lye, ‘the saponification being accomplished by intense- ly mixing the fat and lye while passing them at a saponifying temperature through mixing ap- Paratus. ‘The resulting soap-containing mass is maintained under intensive agitation until it is passed into a centrifugal separator for remov- ing the spent aqueous reagent from the soap. ‘The soap is grained, and thus conditioned for removal of the spent aqueous reagent, prior to centrifugation, by the addition of a salt solution, or an excess of saponifying reagent which serves ‘as a salting-out agent. In the process of Pat~ ent 2,300,760, the salting-out operation 1s accom plished by addition of the salting-out agent be- fore the start of the saponification reaction. ‘The present invention may include any or all of the features of elther of the prior patents to Scott discussed above. It includes steps of effect~ ing continuous saponification by passage of the {at and saponifying reagent together through a saponifying mixer, graining the mixture by addi- tion of a salting-out agent either simultaneously with the saponifying reagent or subsequently to the addition thereof, and centrifugation of the mixture of spent saponifying reagent and grained soap resulting from the saponification while the grained soap is in a condition of substantially ‘uniform dispersion in the spent saponifying 1 agent. * ‘The novel feature of the present invention con- sists in the fact that the mixing step by which intimate contact of the saponifying reagent with the fat is attained to cause the saponification and to bring the soap formed by the saponifying re- action into a state of uniform dispersion is di- vided into two steps, and a step of aging and sep- aration of a part of the aqueous phase is inter- (cl. 260—418) posed between these two mixing steps. In the Practice of the present invention, the fat and Teagent are first mixed during maintenance of a saponifying temperature to cause saponification, and the soap formed as e result of the reaction is grained. ‘The resulting mixture is then sub- jected to aging by maintenance of a period of relative quiescence or lesser degree of agitation, and a part of the aqueous phase settles from the grained soap during this aging step and is removed. ‘The mixture of grained soap and spent saponifying reagent remaining after removal. of ‘8 portion of said saponifying reagent is then pref- erably subjected to a further period of agitation in order to provide sufficient dispersion of the soap in the aqueous phase to afford substantially uniform distribution of the soap in that phase as the mixture is passed to the centrifugal separa- tor for separation of the remaining spent reagent from the grained soap. The succession of steps of the invention, as de- scribed above, may be performed both in the first stage of soap making as described in connection with the first stages of the respective prior pat- ents to Seott discussed above, and in any or all Of the series of subsequent saponitying stages, of which each involves addition of saponifying re- agent, graining and separation as described in the prior Scott patents. ach stage in which a saponifying reagent is added is thus referred to as a “saponifying stage” herein, even though the addition of saponifying reagent in the last such stage may be wholly or partly for the purposes of recovering glycerine and preparation for fin- ishing, and no actual saponification occurs in such stage, ‘By the practice of the invention as discussed above, the following advantages are attained, ‘The quiescent treatment or churning obtained m the aging step causes a change in the mix- ture which facilitates subsequent centrifugation, ‘The removal of a part of the aqueous phase dur- ing this aging step also improves centrifugation, and makes it possible to improve the through- put of the centrifugal in separated soap or to improve the degree of removal of aqueous phase from the soap product. Tt has been found that, in cases in which the saponified and grained mix- ture presents substantial difficulty of separation. in the practice of the Soott patents, the inclu- sion of the intervening aging step in accordance with the present invention assists in avoldance of these difficulties, ‘The aging treatment also provides a longer ‘55 time of contact between the fat and lye, or the 10 1% 30 35 409,411,460 3 formed soap and lye, and this longer period of contact with the saponifying reagent tends to destroy constituents of the mixture which would otherwise cause rancidity of the soap after the soap-making operation has been completed, In addition to the above advantages, the aging treatment, by giving a longer time of contact of the unsaponified fat with the lye, assists in depletion of the lye and attainment of a higher degree of saponification. ‘The detailed nature of the invention and its attendant advantages will be better understood by consideration of the following detalled deserip~ tion in the light of the attached flow sheet, in which the single figure illustrates a preferred embodiment of the invention. Referring to the flow sheet by reference char- acters, fat from container 10 is passed into con- fluence with saponifying reagent from container 14. This saponifying reagent may be an aqueous solution of lye and salt, designed to effect sapon- ification of the fat and graining of the soap formed by the saponifying reaction, as described in Scott Patent 2,300,750. As illustrated in the flow sheet, the solution of lye and brine employed in the first stage of saponification may be a so- lution derived in whole or in part from the step of separation of @ subsequent stage; 1 e. the process may involve counter-current operation as described in the prior Scott patents. ‘The fat from container 10 and saponifying reagent from container 11 may be pumped into confluence with each other by pumps 12 and 13 to and through the mixer [4'in the desired ratio, ‘The reaction mixture, or its constituents, is (are) heated to.a temperature (e, g., 200° F.) sufllelently high to effect saponification of most, of the fat during passage through the mixer (4, ‘The mixture is maintained in a state of intensive agitation dur- ing passage through the mixer 14 in order to in- sure rapid saponification of the fat. When a sraining agent such as salt is included with the saponifying reagent, the soap is grained prompt- ly upon formation thereof, It is possible, how- ever, to introduce the saponifying reagent and graining agent separately, as described in Scott Patent 2,300,149, and when operation of this type is accomplished, the graining agent is preferably added before the reaction mixture leaves the mixer ¢4, or at Ieast before it enters the ager (5. ‘The reaction mixture is passed continuously trom mixer 14 through an aging tank 18. The mixer {is preferably provided with agitating Blades to insure violent agitation, but the ager 15 need not be provided with such elements. Tt 4s desirable that the mixture be gently agitated during passage through the ager 15, but this re~ sult can be accomplished either by the natural movement of the mixture through that tank, or by provision of agitating blades which provide much less violence than that maintained tn the mixer 14, ‘The ager 15 is preferably provided with a t pered bottom designed to permit removal of spent ‘aqueous reagent separated from the grained soap during the aging step through the draw-off valve {7. ‘Thus, the ensuing © -p of centrifugation is facilitated by removal at this point of a part of the aqueous phase which would otherwise be re- moved by subsequent centrifugation, ‘As the result of maintenance of relative quies- cence during passage of the mixture through the ager 15, aqueous-phase which still remains dispersed in'grained soap flowing from that ager will be much less nearly uniformly distributed 10 1 45 ” ™ 4 than would be the case if the mixture from mixer 4 were to be introduced directly from that mixer into centrifugal 18, ‘This may cause difficulty in subsequent centrifugation unless corrected. In order to attain a degree of uniformity of mixing of aqueous phase and grained soap flowing from ager 1§ sufficient to insure efficient centrifuga tion, the grained soap-containing mixture flow- ing from ager 18 is passed through a mixer 16 which provides a higher degree of agitation than ager {5 and effects uniform dispersion of the soap in the remaining aqueous phase before the ma- terial enters the centrifugal, From the mixer 16, the mixture of spent re- agent and grained soap is passed to centrifugal 18 for separation of the spent reagent from the soap as in the two Scott patents referred to above. After discharge from the centrifugal 18, the largely saponified mass containing the ‘soap formed in the first stage is subjected to a second ‘stage of saponification in order to complete con- Version of the source of fat into soap. As in the prior Scott patents, this may be accomplished by introduction of the saponifying reagent into the cover of centrifugal 18, ‘Tnus, a solution of lye and brine, which may elther be a fresh solution or a solution derived from a subsequent stage of treatment, is introduced from container I? into the cover of centrifugal 18 by pump 20, and the resulting mixture is passed thence by pump 21 to mixer 22, through this mixer 22 to ager 23 and from ager 28 through mixer 24 to Centrifugal 25, these eloments of the flow sheet accomplishing’ the same functions as are per- formed by the pumps and elements 14, 15, 16 and (8 of the first stage of the process, as 'de- scribed above, ‘The soap discharged from the second stage centrifugal 25 may be subjected to further ‘treatment, as described in the two Scott patents referred to above, and if such further treatment includes further’ steps of saponification, they will preferably include an aging step, as de- scribed above with respect to the first two stages of treatment. The performance of the step of aging has a particular advantage in the last stage of soap making, since the maintenance of the fully saponified soap-containing mixture in con- tact with an excess of the free alkali for a sub- stantial period of time assists in avoiding rencid- ity, as discussed above, and it is therefore de- sirable to provide an aging period after the fat hhas been fully saponified, ‘The partly spent aqueous solution discharged from the centrifugal 25 may be passed by pump 21 to container 41 for reuse in the first stage of the process, in order to make the process truly counter-current, as described in the Scott pat- ents referred to above, Aqueous reagent with- drawn from ager 23 through valve 26 may be combined with the partially spent aqueous 1 agent from centrifugal 28 for recycling to the earlier stage of the process therewith, ‘Spent aqueous reagent removed through valve 17 from ager 18 may similarly be combined with aqueous phase discharged from centrifugal 8, in order that the combined aqueous phase thus obtained may be subjected to treatment for slycerine recovery. ‘Various modifications in the above-described procedure are available to the person skilled in the art, an¢ are hence within the scope of the in- vention. For example, instead of including the2,411,460 5 graining reagent hs a part of the saponifying so- lution, this graining reagent may be added sub- sequently to the saponifying reagent, as described in Scott Patent 2,300,749, ‘The remixing step, after removal of part of the saponifying reagent 8 from the mixer and before centrifugation, may also sometimes be omitted. Many other possl- bilities for modification fall within the scope of the invention, and I do not therefore wish to be limited except by the scope of the following claim. 10 Iclaim: Tn the manufacture of soap, the process com- prising continuously converting fat into soap by mixing said fat vigorously with a sapontfying re- agent at & saponifying temperature during pas- sage through a mixing zone, graining the soap resulting from sald mixing step, thereafter pass- 18 6 ing the resulting mixture of grained soap and ‘aqueous phase through an aging zone in which. the mixture ts churned by agitation of a degree Jess than that maintained in the preceding mix- tpg zone, removing a part of the aqueous phase by gravity settling through said aging zone, pass- ing aqueous phase and grained sap from said ‘aging zone into a second mixing’zone in which they are agitated more vigorously than in the aging zone until substantially uniform disper- sion of the soap is obtained, and finally passing the mixture resulting from agitation in said last- mentioned mixing zone to a centrifugal separator and thereby separating the grained soap from ‘aqueous phase. LEOPOLD SENDER,