S'l AT ES PATENT OFFICE.

MAURICE AISEN, OF NEW YORK, N'- Y., ASSIG'NOR TO GRAIN SOAPS CORPORATION, OF DOVER, DELAWARE, A CORPORATION OF DELAWARE.

PROCESS OF MAKING SOAP AND DETERGENT.

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Specification of Letters Patent. Pate t d N 1920 lt'o llrawing. briginal application filed November 20, 1919, Serial No. 339,406. Divided and this application filed October 7, 1920. Serial No. 415,272.

To all whom it may concern."

tie it known that l MAURICE AIsnN, a citizen of the United gtates, residing at New York city, in the county of New York and Edtate of New York, have invented new and useful improvements in Processes of Making Soaps and Detergents, of which the followllti Ell.

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ing is a specification. 4

This invention relates to processes of making soap by means of hydrolyzing starches or proteids either by action of heat or by acid and heat combined, and treating the hydrolyzed product with caustic alkalis in a medium of anhydrous sodium or potassium carbonate, or any anhydrous salt of a similar chemical character.

l-leretofore detergent compounds have been made from cereals, which are a mixture of starches (carbohydrates) ,proteins (nitrogenous matter) and glycerids of fatty acids (fats). These substances have been treated either individually, or in mixture with comparatively strong solutions of alkalis (caustic soda or caustic potash). In the case of starches or proteids the resulting combination created sodium or potassium salts of starches or proteids which are of a complea nature with a higher molecular struc ture. The cereals used have been mostly corn, oats, wheat and rice, which are heavy in starches and are. built up from a number of simpler compounds of low .molecular structure, polymerized in nature to a compound of high molecular structure.

lnmy-improved process, it do not use cereals as such, but, first, by hydrolysis of the starches and proteids, T break down their high molecular structure into compounds of the same chemical family but of low molecular structure; that is, tie-polymerize the compounds of the starches and proteids, which are of high molecular structure, into compounds of low molecular structure of substantially the same chemical character.

The advantages of this are (1) that I create new and different compounds having new and different properties; (2) I obtain a product which will fix more alkali, as each simpler compound will liX an alkali, and, by weight, will combine with more alkali; (3) the simpler compounds have a more active acid groupment, that is, the alkali being stronger combined, will hydrolyze slower and be less likely to affect fabrics mjuriously in washing; a the hydrolyzed simpler The theory of washing by means of alkalifatty acids, especially those of sodium salts ol' fatty ac1ds, 15 that when this compound is dissolved in water it hydrolyzes, The acid salts of the fatty acids are colloids of great surface activity and penetrability, which 7 separate and unloosen dirt and grease mechanlcally attached to the material to be washed, and the free sodium hydroxid chemically combines with the grease and the dub The acid salts of the fatty acid emulsifies these new formed sodium compounds which are soluble to a large extent in water; by rinsing both the solubles and insolubles are removed.

The alkali-cereal compounds heretofore used, when hydrolyzed in water for washing purposes, revert back practically to their original alkali and starch. The starch, while a colloid, has little, or practically no, surface activity or washing efficacy, and the efliclency of such alkali-cereal compound is practicallyentirely dependent u on the efficacy of the alkali contents 0 the compounds. The hydrolyzed simplified cereal compounds, utilized by my process, are very active surface colloids and also are quickly soluble in water, and therefore add greatly to the penetrability and efiiioacy of the prod not of my invention as a washing agent. Y

When an alkali is combined with the hywhen alkalizing the simpler hydrolyzed compounds with strong alkali solutions. For this purpose, I have found that anhydrous sodium carbonate, or anhydrous po= tassi'um carbonate, or any anhydroussalt of similar character, is we 1 suited to rodu'ce the desired effect; these salts will re uce the violence of the chemical action. Other means of a similar character may be used without departing from my invention. The water of the caustic alkali solution is absorbed by the anhydrous salt. Then by raising the temperature of the mass to the melt ing point of the carbonate, now hydrated, ssiponification of the hydrolyzed mass takes p ace. 4

My process may be clearly understood by the following illustrations: The cereal (say 250 pounds) is heated, preferably in a steam jacketed drier, from one and one-half to four hours at a high temperature but below the carbonization temperature (the carbonization temperature is substantially 180 centigrade), the mass being constantly stirred during the heating. By this treatment the cereal is hydrolyzed to compounds of simpled, or lower, molecular structure having a stronger acid nature than the original cereal. The higher the temperature (but below the carbonization temperature) the shorter the time it will take to hydrolyze the cereal. The change of color, from yellow to brown, indicates when the desired chemical change has been accomplished. To this hydrolyzed product I add anhydrous sodium carbonate (substantially 100 pounds) which has the effect of stopping any further conversion. When the mass has cooled, I spray into the hydrolyzed sodium carbonate mixture caustic soda (substantially to pounds of 98% strength according to degree of hydrolyzation) which has been dissolved in water (in substantially 135 pounds). The anhydrous sodium carbonate,

- being very avid for its water of crystallization, absorbs the greater part of the moisture, leaving a very intimately mixed product, slightly alkalined, of the hydrolyzed cereal, sodium carbonate crystals and prac-- tically dry caustic soda. The temperature of the mass is then gradually raised to the melting point of the sodium carbonate crystals (below 100 centigrade) and maintained at such temperature for substantially one hour, at which time all the cereal will have been alkalined. Then all the sodium.

carbonate crystals may be neutralized with a substantially equivalent amount of fatty acid, the amount of fatty acid used depending upon the nature of the fatty acid. The product is an eflicient detergent compound. Substantially the same result can be accomplished by a slight modification of the above illustration, as for example: into the cereal (say 250 pounds) is sprayed a dilute form (substantially 0.]. to 0.25%, figured at 100%) of hydrochloric acid, or nitric acid (substantially two pounds); then heating the mixture'three-quarters to one and onehalf hours at a temperature substantially between 150 and 160. degrees centigrade; the time and temperature can be determined by the change incolorof' the mixture from yellow to brown, depending upon'the amount of hydrolyzed action desired. To this mixture add anhydrous sodium carbonate (substantially 100 pounds). When the mass is cooled, add caustic soda dissolved in water and then subject to heat to the melting point of the sodium carbonate crystals, substantially as in the previous illustration.

By another slight modification the same result is accomplished, viz: The cereal (say 250 pounds) is hydrolyzed either as in the first or second illustration above, and when hydrolyzed anhydrous sodium carbonate (substantially 100 pounds) is added. To this mixture add fatty acids sufficient to emulsify and neutralize the sodium carbonate (100 to 200 pounds, depending upon the nature of the acid). This mixture is, dry and the sodium carbonate will produce no chemical action, or practically none, except that it emulsifies the fatty acids and incorporates in the emulsion the hydrolyzed cereal. Dissolve caustic soda (substantially 45 to 55 pounds according to degree of hydrolyzation) in water (in substantially 125 pounds) and add to the emulsified mass a sufiicient amount of this caustic soda solution to complete the saponification of the fatty acid, the quantity depending upon the nature of the fatty acid. In this modification the anhydrous sodium carbonate may be omitted, for the reasonthat the fatty and will prevent a too violent chemical reaction of the alkali and hydrolyzed cereal.

By still another modification the same result is accomplished, viz: To anhydrous sodium carbonate (say 100 lbs.) saturated with its water of crystallization from a solution of caustic soda add hydrolyzed cereal (substantially 250 lbs.), raise the temperature of the mass to the melting point of the sodium carbonate crystals (below 1 O0 centigrade) and the mass will saponify, and free caustic will be substantially absent; if a fatty acid soap is desired as a part of the mixture in the final product, add to the hydrolyzed cereal after it has been mixed with the saturated sodium carbonate a fatty acid as desired and a sufiicient quantity of the solution of caustic soda to saponify the fatty acid used.

The cereals used are preferably the flour of corn, oats, wheat, rice, etc., but any substance rich in starch may be employed.

In stating the order of mixing the ingredients, the proportions of the different ingredients and the strength of the acids and alkalis used, it must be understood that I do not limit myself to the above stated proportiohs of the ingredients, orthe order of their mixture, or the quantity or strength of the acids and alkalis employed; good results may be obtained under my process by a considerable variance from the proportions and strength of the ingredients used.

ical agents used as, as is well known to chemists, other chemical agents may be substituted to produce the same results. The ingredients and chemical agents above stated, however, I have found, in practice, to be elficient, economical and productive of a high grade detergent.

with a dilute form of ydrochloric acid and maintaining the mixture at a high tempera ture, but below'the carbonization temperature, for substantially one hour; adding anhydrous sodium carbonate in the proportion by weight substantially of one part of sodium carbonate to two and one-half parts of the cereal; adding substantially onequarter by weight of caustic soda dissolved in water and subjecting the resulting mass to a temperature of the melting point of the sodium carbonate crystals (not exceed ing 100 centigrade) for substantially one hour; and neutralizing the free carbonate crystals and caustic soda with a fatty acid. a 2. The process of making soap fr'om cereals consisting in hydrolyzing a cereal flour by means of hydrochloric acid and heat, saponifying the hydrolyzed mass by .an alkali and neutralizing any free alkali with a fatty acid.

3. The process of making soap from cereals consisting in hydrolyzing a cereal flour by'means of any mineral acid and heat, saponifying the hydrolyzed mass by an alkali and neutralizing any free alkali with a fatty acid.

MAURICE AISEN. Witnesses! F. a. am, SAMUEL S. WA'rsoN.