Патент USA US2110899код для вставки
March 15, 1938. W. WOELFLIN 2,110,899 ` ELECTRICAL METHOD FOR MANUFACTURING SULPHONATED OILS Original Filed Dec. 26, 1933 HTTo/efwsy 2,110,899 Patented Mar. 15, 1.938 l UNITED STATES PATENT OFFICE ELECTRICAL LIETHOD ‘ FOR IHANUF'ACTUR'e ING SULPHONATED‘ OILS wmnm woemin, 'ung Beach, oeuf., assigner zu Petroleum Rectifying Company of California, Los Angeles, Calif., a corporation of California Application December 26, 1933,\Serlal No. 703,945 Renewed June 5, 1937 19 Claims. My invention relates to an improved electrical process and apparatus for the manufacture of ` , sulphonated oils such as textile oils, leather oils, chemical emulsifying and demulsifying agents the fatty raw material employed in making sul pho-fatty bodies is a mixture of fatty acids and Vglycerides prepared by splitting or partially split- . ting triglycerides by means >of acids or splitting and the like, such as are used in the textile, leath- l agents like Twitchell reagents. erv or other industries. l The presently described process is also appli - In general the problem of manufacturing sul phonated oils and sulphonated fatty materials is not new. Oils, fats, and the fatty acids occurring therein have previously vbeen reacted with lsul cable to the preparation of such materials as -Twitchell reagents, whichl .are the products of sulphonation of a fatty body and an aromatic body by means of sulphuric acid or a derivative phuric acid, oleum, chlorosulphonic acid, etc., thereof, this material to be sulphonated being in- - and the resulting products of such reactions have found utility in the textile, leather, and other industries, especially in a partially or completely ble of reaction with sulphuric acid or a derivative.l neutralized state, these products being sulpho cluded within the term “organic fatty body capa thereof”. _ ' , \ - The presentprocess is then, in general, appli 15 cable to sulphonation reactions in which the principalingredient is an organic fatty body cap fatty bodie‘sand containing in some cases acid sulphates, and in others ~true sulphonic acids. More recently the higher alcohols, e. g., cetyl al cohol, have been employed as ingredients in sim ilar processes to produce sulpho-bodies of some-‘ present, in addition to‘these primary ingredients, what similar properties. various other reactive or inert ingredients, such Y able 'of reaction with sulphuric acid or a deriva tive thereof, as herein defined. There may be The present process relates to an'improved 1 as petroleum distillates, aromatic bodies, like ben- ` process and apparatus for vthemanufacture of such sulpho-fatty »materials and particularl to Va sulphonation process using sulphuric aci as a. reaction agent. . I shall hereinafter employ the term “organic fatty body capable of reaction with _ sulphuric acid or a derivative thereof" for the material preliminarily- treated in the manufac ture of such products. By4 the‘word “derivative” in this term, I have reference to a derivative zol or naphthalene or phenol, carbon tetrachlo- ‘ ride', etc.‘ ‘ ~ . ' 'I'he process of this invention is applicable in the preparation 'of sulphonated fatty derivatives containing large percentages ,ofi sulpho-com pounds, as well as in the preparation of sulpho natedffatty bodies in which the percentage of sulpho-compounds is small, i. e., in which the 30 amount of organically combined sulphur trioxide which is an equivalent of the sulphuric acid. In _ present is very small. -The products of such sulphonation processes I this term are included fatty bodies such as gly-v cerides, animal andy vegetable oils, fats, waxes and shall refer to as sulpho-fatty bodies, or sulphof the fatty acids occurring therein, ’as well as thel fatty derivatives, it being distinctlyunderstood 35 that in these terms I include not only sulpho the oils, fats, and waxes in physical appearance .nated oils and sulphonated fatty acids, but also and in many of their properties. Of these higher- sulpho-alcohols and sulpho-.aromatic fatty bodies. alcohols, I include specifically those having more The sulpho-bodies referred to herein may be than eight carbon atoms `inwthe molecule, of either true sulphonic bodies, containing the sul phonic group, or they may be acid sulphate bodies which group cetyl alcohol, octädecyl alcohol, me higher aliphatic-alcohols, which latter resemble lissyl alcoholï and ceryl alcohol may be named containing the sulphate group. The present method of manufacturing such The fatty bodies referred to above includes the l sulpho-fatty materialsl consists usually of the fol 'unsaturated' oils, fats,- and fatty acids commonly lowing general steps: (l) Mixing a sulphonat _employed in preparing sulphonated fatty deriva-V > ing agent in the form of sulphuricV acid or a suit' as examples. _ tives. > 40 . . They also include otherY fatty. materials, e. g., hydroxystearic acid, which owe their re able derivative thereof with an organic fatty body4 capable of reaction with such sulphur acid, either alone or with the addition of suitable solvents,` diluents, or other ingredients, `allowing the fr_e activity, in the presence of sulphuric acid or its derivatives, to -the existence of areactive group, like the hydroxyl group, in the molecule. The , action to proceed for a desired length of time and' more common members of this group of organic at a desired temperature. (2) Washing the acidic .fatty bodies-capable of reactionwith' sulphuric -reaction massv with a suitable amount of an acid are oli’ve'oil, castor oil, fish oils, sperm oil, aqueous washing medium which may be water i whale oi1,`oxeic acid (red ou), etc. In sqmecases, Q1.’ other suitable aqueous solution. _ By wash . 2, 110,899 2 . ing, I mean mixing or contacting, more or_less color the product or be detrimental to the ap intimately; the acidic reaction mass and the suit pearance or quality thereof. able aqueous medium. In most cases, mixing is continued `until a4 homogeneous mixture is pro duced, which may separate more or less slowly. (3) Allowing the mixture to stand in a quiescentI state until it separates into two layers. The excess sulphonating agent and the Washing me dium, with possibly -some Water-soluble organic .matten like glycerin, comprise the lower aqueous 10 layer, leaving an oily supernatant layer in the upper part of the settling zone. (4) Withdraw ing the lower aqueous layer. (5) Partially or completely neutralizing the oily supernatant lay 15 er consisting of sulphonated, sulphated, or oth erwise altered’fatty matterial, this neutralizing action being effected by adding a suitable neu tralizing agent, usually one of the common al ` In the present process the above-mentioned defects' are'overcome and a superior product is obtained by utilizing electrical means for assist ing in performing either or both separating steps. Thus, the acidic >reaction mass, together with the " water or other aqueous medium mixed there with, may be subjected tothe action of an elec tric field which quickly coalesces the excess of water or aqueous medium and sulphonating agent into masses of suñlcient size to be easily and rapidly removed byA gravitational or centrifugal methods. The same -method can be used in separating the neutralized or partly neutralized material. ' » Among the important objects of the present invention is the provision of a method and ap _kali metal bases, caustic soda, `caustic potash, _ paratus- for forming such sulphonated' products 20 anhydrous or aqueous ammonia, etc., or one of the alkali ‘carbonates or bicarbonates, `or other bases like those of the alkaline earth metals. (6) Allowing the neutralized or partially neu tralized mass to stand in a quiescent state to permit settling therein of the small amount of aqueous solution remaining after the first set tling period and the neutralizing step, as well as to allow a settling of more or less of the water which may have been added With'the neutral so izing agent. ' . ~. produce an improved andv superior product- of in creased effectiveness. l It is a further object of the invention to pro vide a novel step in the process of producing sulphonated fatty derivatives, Whereina mixture of an acidic reaction mass and a washing me-`l dium is subjected to the action of an electric field. _' The length of time required for. these separa tory steps is quite large, which effects not only a distinct saving of time, 20 apparatus and materials in the manufacture of these products, but which has' been found to . » » 30 >A further object lies in the subjection of a The ñrst such step, ,finished or Áa semi-finished product consisting of a partially or completely neutralized sulphonated wherein the lower /aqueous layer is"formed`after washing the acidic reaction mass, frequently re 35 quires from eight to thirty-six hours, depending on the temperatures employed in washing, the nature of the ingredients, the reaction tempera turek employed, and other factors. The.- second separatory step also requiresa prolonged time of settling to remove the Water or aqueous solu tion. In some' cases separation of aqueous ma fatty derivative to the action of an electric ñeld. A'I further advantage of the present process is 35 that a saving is effected in the amount of neu tralizing agent needed to neutralize the material . to a desired point, as compared with the amount needed whe/n prolonged gravitational settling is resorted to, and it is a further object of the in_ 40 vention to/'pròvide a process and apparatus which- _ vaccomplishes súch a saving in the amount of îterial continues for as long as a month, and products behaving in .this fashion cannot be y. materials required. ’ It is not necessary to thepresent process. that safely marketed untilf substantially all traces of l . ; an “anhydrous product be obtained.-> The sul this material are removed. Centrifugal methplds >are commonly ineffectual in that they fail ma'. .plioiiiated fatty derivatives prepared in accord terially to accelerate and facilitate the separa-¿f ance with the present process may sometimes still contain considerable amounts of water, though in tion and stratification of the constituents; ` Not only do either or both of these settling steps many instances the process results in the pro result in a great waste of time and necessitate duction of a product containingonly traces of much additional equipment which would- other wisc be unnecessary, but my, experiments have shown that> it- is .very undesirable to maintain such water or aqueous solutions in contactwith the fsulphonated products. i water. ' It has sometimes been found desirable to util ize an electric field of special‘oscillatory charac, ter, andl it is another object of the present in I have yfound that__ vention to use one or more electric fields of this 55 prolonged contact between these materials pro duces undesirable side reactions which material ly decrease the effectiveness of the finished prod uct. Among these side reactions may be cited 60 hydrolytic and polymerizing reactions which vare quite detrimental to the ñnished product. Furthermore,- incomplete and imperfect sepa ration of .the aqueous material before neutral ization results `in the retention of excessive amounts of the sulphonatin'g agent by the oily ‘ acidic mass _after washing and settling. causes the- amount of vneutralizing agent required .to be excessive, which in turn results in higher costs and, if _the neutralizing base be employed This . character in the removal-of excess water or other aqueous constituents from a sulphonated fatty derivative. . . Other objects and advantages of the invention 60 will be made apparent hereinafter. The said organic fatty body capable of reaction with sulphuric acid or a derivative thereof is ñrst mixed with the sulphuric acid or other suitable sulphonating agent in a reaction or mixing cham ber of any common or desired form, with or with 65. out the addition of diluents, solvents, reactive or inert aromatics, etc. In the annexed drawing, I have diagrammatically shown a tank III into which these organic fatty materials, etc., and the sulphonating agent are respectively introduced in aqueous solution, also results in undesirable as through pipes I I and I2. dilution lof the product. Other disadvantages are, lfor example, the inclusion of large amounts be stirred by any suitable agitator means, not shown, _or by a Wooden paddle. The result is" of mineral sulphates which may separate on standing, or which may cloud or otherwise dis the formation of an acidic reaction mass. These materials may When the‘reaction has proceeded for the de 2,1 10,899 3 transference to a‘vsecond vessel. Thus, in the ration of theaqueous layer. In some cases, the rod and electrode may be so mounted or moved that a constant distance is maintained between the electrode and the constantly rising surface latter-process, the aqueous washing medium in the form of water or other suitable aqueous me dium commonly employed to remove the excess be constantly raised as separation proceeds under the influence of the process.` sired length of time, the acidic reaction mass may be transferred to arwashing chamber or it may be washed in the same tank I0 without of thesaid aqueous layer, i. e., the electrodel ‘may In other instances the electrode structure may be retained in a ñxed position in the tank 2| so that as the level indicated by the dotted line 2l ris'es the field between this level and the screen electrode 25 will increase in intensity. Any suitable means may be utilized for`build ing a. potential between the rod 24 and the tank reaction mass by any suitable agitator positioned _ 2|. Best results are-obtained if an altern-ating 15 or pulsating current is utilized. In manyin in the tank I0 or by manual means. stances it is possible to secure entirely satisfactory If desired, the mixture may be allowed pre liminarily to settle in the tank Ill to permit the treatment by'connecting the high tension wind in_g of a transformer between the tank 2| and bulk of the aqueous medium, consisting of wash „in'g medium, excess sulphonating agent, and any the rod 24, this transformer being one which 20 other ingredients of the acidic reaction mass ' builds a high voltage therebetween. Potentials such- as glycerol, which may be preferentially less than 10,000 volts in magnitude are ordinarily sulphonating agent from such mass, such as so dium chloride, or sodium sulphate solution, is in troduced into the tank Il) by any suitable means. Diagrammatically, I have illustrated a pipe I3 for introducing this aqueous washing medium into the lower end of the tank I0. This washing medium is intimately admixed with the acidic soluble in water, to separate naturally by gravity, reserving theapplication of the electrical treat ment for the removal of the last traces of re movable aqueous material. If this is done the ' material which gravitationally separates can be removed through a pipe I4, allowing the remain der of the material to move through a pipe i5 to the electric treater 2|).ä Generally, however, the process of this invention is_most advan tageously employed by quickly subjecting the very satisfactory,` though usually the potentials employed should be above 1,000 volts. Very sat isfactory'results will thus accrue if a 5500-volt transformer is utilized thereby making -an aver age gradient of 1,000 volts per inch. These limits are, however, not exclusive, for in some instances it is possible to use potentials higher or lower ‘ than those above mentioned. ' The limits set forth are illustrative, and I do not limit myself thereto. With such a system the alternating po whole mixture ol' acidic reaction mass and wash ing medium to the action of an electric field to separate the "removable aqueous material as rap tential can be continuously applied or can be idly and completely as possible, for reasons pre viously recited herein. In this instance the en tire mass of material is moved through the pipe one-half cycle if desired, or may be of such length f as to include more than one-half cycle or several complete cycles if desired. i In some instances it has been found desirable |5‘and into the treater 20. _ As diagrammatically illustrated, this treater 20 40 mayinclude a tank 2| comprising an outer 4 vgrounded electrode on which insulators 22 are periodically interrupted to form a series of im pulses. Such impulses may be of a duration of to utilize the circuit shown in the accompany 40 ing drawing, especially when treating masses of ~ an especially conducting nature. In the form/ These insulators, of any desired shown, I have illustrated a transformer 3|]v in cluding a high voltage winding 3|, one terminal 'mounts a rod 24, which latter_` element may„in of which is grounded and connected tothe tank. 2|. The other terminal is connected to the rod some instances, in itself comprise an inner elec trode. In the exemplary form shown, a screen 24 through a spark gap 33. It is usually prefer electrode 25 is retained at the lower end of the able,V though not always necessary, to place a rod 24. As treatment progresses, there is formed condenser 34 across the high tension winding 3|, supported. number, carry a cross bar 23 which adjustably in the bottom of the tank I2| an aqueous layer the level of which slowly rises until` the mixture ì has been substantially completely separated. I as shown. The transformer 30 includes a low 50 tension winding 35 which is connected to va suit able commercial-frequency,supply line through -a ' ' have -indicated the' ultimate uppermost surface choke‘coil 352 . When a treater thus connected i‘s placed in‘ 4of this lo'wer aqueous layer by the dotted line 2l, and have found it preferable to> position’the operation, the current flow throughl .the treat screen electrode -25 a slight distance above this ing space will be limited by the choke'coil 36.. At surface 21. If, then, a potential difference is- the same time, by properadjustment of the spari;y maintained between the tank 2| and the rod 24, gap 33, this gap will periodically break down asv treatment will take' place not only in the space the potential thereacross builds up. _Thus, as the ' around the rod, i. e., between this rod and the potential across the electrodes is building up?the tank 2|, but will also take place between the condenser 34 will be charged, and when a, suf screen electrode 25 and the tank 2|. In addition, ficiently high_,potential is attained, the spark gap 33 will break down. vAtkthis, instant, a low treatment will take place between the screen elec trode 25 and the surface of the aqueous lower resistance -path is formed across thejterminals layer which -is of a conducting nature. _The of theI spark -gap and cu'rrent can flow there electrode 25 and the rod 24 should not at any Athrough to the electrodes. During this break time be submerged below the upper level ofV this down period, the condenser 34 discharges to. the lower -aqueous layer, since short-circuiting would electrodes. "This discharge is an oscillatory one and is usually of high frequency, this frequency be caused.l . v ^ ‘ being determined by the-electrical characteristics Til It is to be distinctly understood that the posi tion of the rod and electrode in relation to the surface ‘of the lower aqueous layer vis not to be regarded as necessarily fixed. Different reaction masses may require different adjustments of the rod and electrode to -attain most efficient sepa of the condenser 34 and theY remainder of the circuit. However, any current flowing to ~the electrodes decreases the potential across' the winding 3|, especially when a choke coil 36 is being used. Thus, the potential is reduced to such y2,110,899 4 an extent that the arc will not persist'across the ~ ized products to the electrical separation process spark gap- 33, thus stopping a major portion of the current flow to the electrodes. The cycle is repeated when the potential across the trans former winding 3| again builds up. Other types of high frequency systems producing an oscil latory potential may also be _used to advantage. Further, by using a rectiñer with spark gap and condenser, direct-current impulses can be ob tained. These may also be used to advantage in of the invention is that a »product of superior `homogeneity can frequently be so prepared. For certain instances. _ _ - After such electrical treatment the lower aque ous layer may be withdrawn from the tank 2| through a pipe 4D including a valve 4l. There after the=oily acidic mass remaining in the treater may be neutralized therein, or it may be removed from the treater to another container in- which _ this neutralization takes place. _In the form il lustrated the electrode structure is so formed as to be easily removable from the insulators 22, thus permitting the neutralization step to take place inthe tank 2 |-. The neutralizing agent may I be added by any suitable means, as by a pipe 42. ' This- neutralizing agent is in the form of a suitable ‘basa The common neutralizing agents are sodium, potassium, and ammonium hydrox example, sulpho-fatty materials that have been; neutralized only slightly past the point where all the strong acidic hydrogen has been neutralized are sometimes marketed in this form and ñnd particular utility in certain. commercial processes over products which are neutralized to a greater If the separation is allowed to take place 10 degree. by gravitational means, such relatively under neutralized _products exhibit the very undesirable property of settling water or other aqueous s_olu tion over an extended period of time. If, there fore, such products are marketed immediately 15 upon completion of manufacture, the separation of such _aqueous material in the container pro du‘ces an unfavorable reaction on the purchaser. Thus, regardless of whether partial or complete neutralization is effected, it is usually vdesirable 20 to subject the neutralized or partially neutralized mass to the action of an electric field. This can be accomplished by reinserting the electrode' structure in the tank 2| and establishing the fields therein so as to coalesce and quickly remove the water or other vaqueous solution. A superior ides, although any other base may be employed « product is produced if such foreign substances as desired. For example, alkaline earth metal bases may be used, or the carbonate or bicarbon 30 ate of any desired metal or metal equivalent may be used in this capacity. The neutralizing agent is suitably mixed with the reaction mass, as by being stirred or otherwise agitated either manu are removed in a short period of time, as herein before mentioned. 'I'he electric field utilized in conjunction with the neutralizing step may be of an alternating or pulsating type, as previously described. ' With certain materials it is desirable to use the oscillatory system illustrated, though ally or mechanically by meansnot shown. Insome‘instances it is possible to neutralize to it will be understood that the utility of the process is not dependent upon the use of su'ch a field ofv 35 the desired -degree in a single s_tep. In this in high frequency oscillating potential. stance the inorganic and the organic acids pres- _ If a poly-stepneutralizing process is utilizedv this electric treating step can be performed either ent are neutralized to the desired point by the addition of the proper amount o‘f neutralizing 40 agent. In this instance the resulting product may be removed through the pipe 40 or _it may be allowed to settle for a time in the tank 2 I. Usual ly, however, it is desirable -again to subject the ' v neutralized or partially neutralized mass to the action of an electric ñeld as will be hereinafter described. ' A - In other instances it is desirable to vary this procedure, and, instead of‘neutralizing the olly acidic mass to its ñnal degree in one operation as is -performed in the common process of manu facturing sulphonated oils, to conduct the neu between the time that the respective neutralizing steps are taken or afte? the desired degree of neutralization has been obtained by this poly- _ step neutralizing process. It should be understood that I am not limited to the particular apparatus shown. If desired the tank l0 can be dispensed with and the sul phonating agent and washing. medium added di rectly to the tank 2| during the time that the ' electrode is not positioned therein. So also it is possible to perform the neutralizing step in a container separate from the tank 2|. So also, if 50 desired, the electrical treatment of the neutral tralization in two or more steps. For example, ized or partially neutralized product can be ei- it may be desirable to neutralize in the ñrst step » fected by the use of an entirely separate- electric only the strong acidic hydrogen that is due to the treater similar to that indicated by the numeral 20. Furthermore, while it is usually desirable to Cil :A sulphuric acid and the organic sulpho-bodies present in the mass. Such a procedure would utilize the invention in conjunction with a batch thus permit the settling of mineral sulphates. ‘ process, it will be apparent that my process is water andA other similar aqueous or water-soluble equally applicable to the preparation of sulpho material before completing the neutralization in fatty bodies by continuous processes and the use of the word "mass” in the appended claims is not 60 one or more subsequent steps., In this Way the presence of rexcessive amounts of such inert and to beconstrued as limiting same to a batch proc frequently undesirable substances can be avoided. ess. - ' The subsequent neutralizing step or steps would I claim as my invention: _be used for the purpose of neutralizing the prod- . 1. An improvement in the process of manu uct to any desired degree, e. g., _until a water facturing sulpho-fatty bodies, which improve _soluble oil is obtained. The product can be car- - ment includes the steps of: intimately contacting ried to the point of complete neutralization if de the reaction organic fattybody to be sulpl'ionated sired, or neutralization may _stop short thereof, depending upon the product to be produced. If and a. sulphonating agent to form an acidic reac tion'mass; mixing said acidic reaction mass with an aqueous washing medium; separatingat least out, it has been found very desirable to subject the . a part of said aqueous Washing medium by ap semi-finished product to the action of an electric plying to the'mixture an electricñeld; Withdraw iield, thus. greatly decreasing the time `necessary ' ing the separated aqueous layer; at least partially to separate the removable material. An advan neutralizing the remaining oily acidic mass ;.. and such a poly-step neutralizing process is carried tage accruing from subjecting such semi-neutral subjecting said partially neutralized mass to the 75 5 , 2,110,899 ‘ action of an ‘electric field to separate aqueous- reaction with sulphuric acid or a derivative there material therefrom. of to'form an acidic reaction mass. which im _ provement includes the steps of: mixing said acidic reaction mass with an aqueous washing medium; separating at least a portion of the aqueous washing medium to leave an oily acidic 2. An improvement in the process of manu facturing sulpho-fatty bodies by adding a sul phonating agent to an organic fatty body capable of reaction with‘sulphuric acid or a derivative thereof to form an acidic- reaction mass, >which mass; partially but not completely neutralizing said oily acidic mass; subjecting theresultant product to the action of\ an electric ñeld of high improvement includes the steps of: mixing said acidic reaction mass with an aqueous washing . intensity to -coalesce at least a part of the aque 10 medium; and then subjecting the resulting mix field to quickly separate the oily portion of the acidic reaction mass from the aqueous washing layer. medium and substances associated therewith,> preventing prolonged contact rwhich V15 thereby would set up deleterious side reactions. 10 ous -material removable therefrom; allowing the electrically treated material to settle to form an aqueous layer; and removing said aqueous ture ’to the action of a high-intensity electric ` 8. An improvement in the process of manufac ‘ -turing sulpho-fatty bodies by adding a sulphonat ing agent to an organic fatty body capable of ‘3. An improvement in the process of manu facturing sulpho-fatty bodies by adding a sul phonating agent to an organic fatty body ca 20 pable of .reaction with sulphuric acid or a deriv reaction with sulphuric acid or a derivative thereof to-fo-rm an acidic reaction mass, which improvement includes the steps of: mixing said 20 acidic reaction mass with an aqueous washing ative thereof to `form an acidic reaction mass. medium; separating at least a portion of the aqueous Washing medium to leave an oily acidic which improvement includes the steps of: mixing said acidic reaction mass with an aqueous wash mass; partially neutralizing said oily acidic mass; subjecting the resultant product to the action of an electric field of high intensity; and subse quently further neutralizing the material treated ing medium; 'subjecting the washed acidic re action mass to the action >of a high-intensity electric field to coalesce`at least a part of the aqueous material; settling said coalesced material to form an aqueous layer; withdrawing the ma terial in said aqueous layer; and separately with ' by's‘aid ‘ 4. An improvement in the process of manu - reaction `with sulphuric acid or a derivative thereof to form an acidic reaction mass, which -i'acturing sulpho-fatty bodies by adding a sul phonatlng agent to an organic fatty .body ca pable of reaction with sulphuric‘acid or a deriv ative thereof to form an acidic’reaction> mass, which improvement includes the steps of: mixing improvement includes the steps of: mixing said acidic reaction mass with an aqueous Washing medium; separating at least a portion of the aqueous washing mediumA to leave an oily acidic mass; at least partially neutralizing said oily acidic mass; subjecting the resultant product to -said acidic reaction mass with an aqueous wash ing medium; immediately subjecting the mixture to the action of a high-intensity electric ñeld to coalesce at least a partfefl the aqueous material; 'the action of an electric ñeld of high intensity l40 to coalesce at least a part of the aqueous ma and` relatively> quickly separating said aqueous 5. An improvement in the process of manu . turing sulpho-fatty bodies by adding a sulphonat ing _agent to an organic fatty body capable of drawing the remainder of the reaction mass. material thus coalesced from the remainder -of the mass to prevent prolonged contact-which would set up deleterious side reactions;` electric field. 9. An improvement in the process of manufac terial therein; removing said coalesced material; and further neutralizing the product remaining after removal of said coalesced material. « ~ 10. An improvement in the process of manu facturing sulpho-fatty bodies byr adding a sul facturing sulpho-fatty bodies as described in phonating agent to an organic fatty body ca pable of reaction with sulphuric acid or a deriv ative thereof to form an acidic reaction mass, ñéld is of high frequency character. which improvement includesgthe steps of : mixing said lacidic reaction mass with an aqueous wash ing medium; allowing the mixture to stand in a quiescent state until a portion of the washing medium and other material preferentially soluble in water have separated; and thereafter separat ing the only portion of said washing-medium` and 45 claim 2, in which said high-intensity electric ’ 1l. An improvement in the process of manu facturing sulpho-fattyvbodies by adding a sul phonating agent to an organic fatty body capa 50 ble of reaction with sulphuric acid or a deriva tive thereoff to form an acidic reaction mass. which-improvement includes the steps of : period ically discharging a condenser in circuit with a pair of electrodes bounding a treating space to the remainder of said reaction mass by sub- ' establish an electric stress in `said treating space; jection to the action of a high-intensity electric field. 60 Y . ‘ ' 6. An improvement in the process of manufac turing sulpho-fatty bodies by adding a sulphonat ing agent to an organic fatty body capable of `reaction with sulphuric acid or a derivative there of to form an acidic reaction mass, which im 63 provement includes the steps of: mixing said mixing said acidicY reaction mass with an aque ous washing medium; and subjecting the mixture . to the action of said electric stress. ‘ 60 12. An improvement in the process of manu facturing sulpho-fatty bodies by ladding a sul phonating agent to an organic fatty body ‘capa ble of reaction with sulphuric acid or a deriva tive thereof to form an acidic reaction mass, which improvement includes the steps of : es acidic VVreaction mass with an `aqueous washing medium; separating- at least a» portion of ‘the ` tablishing an oscillatory electric field; mixing aqueous washing 'medium to leave an,_ oily acidic mass; « at least partially `neutralizing. said oily acidic mass: and subjecting the resultant prod uct to the action of an electric field` of high in tensity. , ¢ H 7. An improvement ,in the process of manufacf turing sulpho-fatty bodies by adding a sulphonat ing agent to an organic fatty body capable of i said acidic reaction mass with an aqueous wash ing medium; and subjecting- the mixture to the action 'of said oscillatory electric ileld. 13. FAn improvement in the process of manu facturing sulpho-fatty bodies as described in claim 2, in which said high-intensity electric field is established by impressing an alternating / 2,110,8'99 6 potential of commercial frequency across a pair washed maß by adding a base in insuilicient ` quantities to completely neutralize same; then separating at least a part of the aqueous material facturing sulpho-fatty bodies as described in - from the partlyAneutralized mass; thereafter -claim 2, in which said high-intensity electric'ñeld ' adding additional quantities of a base; and sube. of electrodes. 14. An improvement in the process of manu is established by impressing analternating po jecting the product- resulting‘from the second tential across a pair of electrodes-fand including neutralizing step tothe action of a high-intensity ` the step Ioi’ ’periodically impressing an oscilla tory potential of high frequency across said elec -. 10~ trodes. 15. An improvement in the process of manu electric ileld. ` v , ' - 418. A process asdeiined in claim 17 in which 'said separation step performed between said 10= neutralization steps is performed by subjecting facturing sulpho-fatty bodies as described in "the mass to the action of an electric- ileld after claim 2, in which said high-'intensity electric 'the first addition of said base and prior> to the subsequent neutralization to separate a vportion field is established by impressing a potential be 15 tween a pair of electrodes, and periodically inter--k of the first-added base prior to the subsequentA 16 rupting said potential. neutralization. 16.` An improvement in the process of manu facturing sulpho-fatty bodies as described in ' ` 19. An improvement in the process of manu- - facturing -sulpho-fatty bodies by `adding a sul claim 2,-in which said high-intensity electric , phonating agent to an organic fatty body capable 20 field is established by impressing an alternating potential between a pair of electrodes, and pe ' riodically interruptinglsaid alternating potential. 17. An- improvement _in the process of manu? facturing sulpho-fatty bodies by adding a‘sul 25 phonating agent to `an organic fatty body capa ble of reaction with sulphuric acid or a deriva tive thereof to form a reaction mass, which irn provement includes the steps of: mixing said >reaction mass with an aqueous washing medium; of reaction with sulphuric acid or a derivative 20 thereof to form an acidic reaction mass, which .improvement includes the steps of t mixing said acidic reaction mass fwith an- aqueous washing medium; subjecting the washed acidic reaction mass to the action of an electric ñeld to separate 25 at least a part of the aqueous material; at least _ partially> neutralizing the resulting oily reac-= tion mass; and subjecting the resulting product to the action of an electric field of high intensity. 30 separating at :least »a portion- of said aqueous so WILLIAM WoELFuN. washing medium; then partly neutralizing the CERTIFICATE V0F coRaEcTIoN.r Patent No.' 2,110,899. March 15, 1958-. I WILL IAM WOELFLIN . It is hereby certified -that error appears in the printed specification of the above numbered patent requiring correction as follows: IPage. 2, first_ column, line 16, for "matterial" read naterial; page 5, first column, ~line56, claim 5, for "only" read oily; and that the said Letters Patent should be readwith these corre ations' therein, that theA vsame may conform to the record of the case in the Patent Office.. Signed' and sealed this 10th day of l'iay, A._ D. 1958.. (Seal.) ~ Henry Van Arsdale,.- _ y Acting Commissioner of Patents. / 2,110,8'99 6 potential of commercial frequency across a pair washed maß by adding a base in insuilicient ` quantities to completely neutralize same; then separating at least a part of the aqueous material facturing sulpho-fatty bodies as described in - from the partlyAneutralized mass; thereafter -claim 2, in which said high-intensity electric'ñeld ' adding additional quantities of a base; and sube. of electrodes. 14. An improvement in the process of manu is established by impressing analternating po jecting the product- resulting‘from the second tential across a pair of electrodes-fand including neutralizing step tothe action of a high-intensity ` the step Ioi’ ’periodically impressing an oscilla tory potential of high frequency across said elec -. 10~ trodes. 15. An improvement in the process of manu electric ileld. ` v , ' - 418. A process asdeiined in claim 17 in which 'said separation step performed between said 10= neutralization steps is performed by subjecting facturing sulpho-fatty bodies as described in "the mass to the action of an electric- ileld after claim 2, in which said high-'intensity electric 'the first addition of said base and prior> to the subsequent neutralization to separate a vportion field is established by impressing a potential be 15 tween a pair of electrodes, and periodically inter--k of the first-added base prior to the subsequentA 16 rupting said potential. neutralization. 16.` An improvement in the process of manu facturing sulpho-fatty bodies as described in ' ` 19. An improvement in the process of manu- - facturing -sulpho-fatty bodies by `adding a sul claim 2,-in which said high-intensity electric , phonating agent to an organic fatty body capable 20 field is established by impressing an alternating potential between a pair of electrodes, and pe ' riodically interruptinglsaid alternating potential. 17. An- improvement _in the process of manu? facturing sulpho-fatty bodies by adding a‘sul 25 phonating agent to `an organic fatty body capa ble of reaction with sulphuric acid or a deriva tive thereof to form a reaction mass, which irn provement includes the steps of: mixing said >reaction mass with an aqueous washing medium; of reaction with sulphuric acid or a derivative 20 thereof to form an acidic reaction mass, which .improvement includes the steps of t mixing said acidic reaction mass fwith an- aqueous washing medium; subjecting the washed acidic reaction mass to the action of an electric ñeld to separate 25 at least a part of the aqueous material; at least _ partially> neutralizing the resulting oily reac-= tion mass; and subjecting the resulting product to the action of an electric field of high intensity. 30 separating at :least »a portion- of said aqueous so WILLIAM WoELFuN. washing medium; then partly neutralizing the CERTIFICATE V0F coRaEcTIoN.r Patent No.' 2,110,899. March 15, 1958-. I WILL IAM WOELFLIN . lïzishereby certified that error appears in the printed specification dftheabovennmberedpatentrequiringcorrectionasfbllows: Page 2, first _ column, line 16, for "matterial" read naterial; page 5, first column, .line- 56, claim 5,for“on1y"readoily; and thatthesaid Letters Patent should be readwith these corre ations' therein, that theA vsame may conform to the record of the case in the Patent Office.. Signed' and sealed this 10th day of l'iay, A._ D. 1958.. (Seal) ~ Henry Van Arsdale,.- _ y Acting Commissioner of Patents.