assesses Get. s, 1946 ‘ ' is ,. 12,409,056 ." TATES PATENT. QFFICE SOAP COMPOSITION Herbert KennetEMcClain, Wyoming, ‘Ohio, as signor to The Procter and Gamble Company, Ivorydale; Ohio, a corporation oi’ Ohio No Drawing. Application'August 22, 1944, Serial No. 550,671 8 Claims. (Cl. 252-368) v 1 w This invention relates to the stabilization of ' soap or soap products, and more particularly'to soap. the prevention or retardation of the development It is an object of the present invention‘ to im prove ‘the quality of soap prgducts’ especially ’ ' According to my invention polyethylene poly of1 rancldity and customary accompanying dis‘3° “mm 2 those products containing a proportion of rosin amines of the formula 6 ' HzN-CzI-k- (HN-CaI-Ia) rum wherein a: is a whole number of 1 or more e?ec-_ with respect to their keeping quality as evidenced tively prevent or retard to a desired degree the by their tendency to become rancid or discolor. development of rancidity in Soap Products and It is known that many soap products wi11 d1s_ 10 especially those which contain a proportion of color and develop a rancid‘ odor on aging and rosin soap and which are readily susceptible to that this property is especially characteristic of the development of rancidity. Of the polyeth soap products prepared from fats which them_ ylene polyamines referred to, those in which the selves are susceptible to the development of ram Value 0f 11 is from 1 t0 5 are Particularly Well cidity. These undesirable changes in the soap is suited for use in the practice of the invention. product are in part due to conditions of storage 0! outstanding value as preservatives are dieth and handling, but in the main the development of rancidity is more pronounced in products which have become contaminated during process- ylene triamine, triethylene tetrhmine and tetra ethylene pentamine, that is, those polyamlnes having $ Values of 1', 2 and 3 respectlvely- Com ing with a small amount of an agent, such as 20 mercial mixtures of these various amines may copper for example, which will promote rancidity. ‘ 11130116 employed with good e?ect. I Many preservatives have been suggested for In the range of ordinary Conditions, I ?nd that use in the prevention or retardation of the de- > an amount of the polyethylene polyamine Which velopment of rancidity in such soaps, and their will give good results will be from about 0.02 per e?ectiveness has been well established. _ 25 cent to about 0.1 per cent of the weight of the Recently, because of fat shortages, it has be- _ ' BOBJJ- Amounts above and below this range, come necessary to suplement normal fat requlrehowever, Such 95 0-005 per cent to 1 Per cent of ments for soap manufacture with rosin and the the Weight of the 582p will show greservative use of this material has intr action also and may uced problems in rancidlty which have not hgrietofore been en- 30 countered. For example, it has been noted that soap products in particle form such as ?akes, spray dried granules, etc., having a. relatively large surface area per unit weight and a rel'a- _ employed if esil'ed In producing the stable soap Products of the plil'esent inhvlention theenpgrestervative isd added?to8 e SOB-P any 00m! 811 manner uring iuguzg crutchingt'or othielrlniixing operatioriawheret-1 .t e preserva ive w uniformly dis ribute , tlvely low moisture content and prepared from 35 thl‘?ughvut. the: entire soap mass. Distribution . fat mixtures containing rosin, develop undesired maybe esslsted by dissolving the mine in ?-e?r- , rancidity and accompanying discoloration much tier, but _I havefound that this is unnecessary faster than do similar products prepared from and that effective distribution may be brought comparable rat formulas containing no rosin. “PM in the same manner that 1.5 used m ‘115' The amount of rosin does not appear critical. 40 "13311? perfume orAggleleruilngreldlegtsltmuglh' Small amounts such as 1 per cent to 2 per cent 231mee?gg‘pbgg’lss'thorouémye g’rgfxgy $260,313; will enhance the development of rancidity in Soap, the i mm is converted into the desired the soap products prepared from such mixtures, product form and larger amounts W111 have eveln greater ef“ 45 The effective preservative action of the polyeth i’ect. I have discovered further that such soap ylene polyammes is noted in soap products of Products containing rosin Soap are not Smt'_a'b1y . all kinds, but, as previously pointed out, their preserved against the development 0f ralmldity outstanding value lies in their use in granular by agents which have been e?ectively used heretype soap products containing a proportion of tofore in ordinary soap products. As a. matter 50 rosin soap. of fact, I have obtained evidence indicating that The following examples wil1 illustrate the man. some of the preservatives which are e?‘ective in ner in which my invention may be practiced, but retarding the development of rancidity in ordiit is to be understood that the invention is not to nary soap granules and ?akes, for example, acbe limited to the speci?c conditions recited tually promote the development of rancidity in 55 therein. ' 2,409,056 3 4 of which a minor proportion is rosin soap and; as a rancidity and discoloration inhibitor, a poly ethylene polyamine of the formula Example 1.--A mixture consisting of 86.7% of i combination of tallow and grease having a titer n the neighborhood of 40 and 13.3% rosin was :onverted into kettle soap in the usual way by I HzN-CzHr (HN-CzHO run, reatment with caustic soda solution. After the isual boiling and washing operations, the kettle cap was crutched, during which 0.05% by weight a: being a whole number, the said product beinc in small particle form and having a relatively If triethylene tetramine was uniformly distrib lted throughout the soap mass. A spray dried large surface area per unit weight and a rela tively low moisture content substantially corre sponding to that of ?ake and spray dried granular ioap product was prepared from this mixture in ;he usual manner, for example as disclosed in J’nited States Patent No. 1,652,900. In an ac soap products. :elerated rancidity development test involving of which a minor proportion is rosin soap and, as a rancidity and'discoloration inhibitor, from about 0.005 per cent to about 1 per cent by weight of a polyethylene polyamine of the formula 3. A soap product comprising essentially soap exposure of the spray dried product for three lays at 120° F. to the atmosphere, the product leveloped a peroxide value of 2.5. A spray dried )roduct corresponding in every way with the sam ale prepared above except that the triethylene ietramine was omitted developed a peroxide value wherein :c is a whole number from 1 to 5, the >! 58 under the same test. These peroxide -val 20 said product being in small particle form and ies, translated into results of shelf storage tests having a relatively large surface area per unit inder normal conditions, indicate that the prod~ weight and a relatively low moisture content sub ict without preservative will go rancid in one stantially corresponding to that of ?ake and spray nonth whereas the product containing the-pre dried granular soap products. 4. A soap product comprising essentially soap servative will stay fresh for many months. Example‘ 2.-A mixture of 95% of a combina of which a minor proportion is rosin soap and, as a rancidity and discoloration inhibitor, from tion of tallow and grease having a titer~in ‘the neighborhood of 40 and 5% rosin was saponifled about 0.005 per cent to about 1 per cent by weight in the kettle 'with caustic soda solution, then of diethylene triamine, the said product being in coiled and washed in the customary manner. In small particle form and having a relatively large ahe crutching operation 0.10% by weight of tri surface area per unit weight and a relatively low ethylene tetramine was uniformly distributed moisture content substantially corresponding to throughout the soap mass. Thereafterthe soap that of ?ake and spray dried granular soap prod was converted into thin ?ake form, for exam ucts. _ ple by the ?ake forming process disclosed in United‘ States Patent No. 2,295,596. In the ac 5. A soap product comprising essentially soap :elerated rancidity development test described in of which a minor proportion is rosin soap and, as a rancidity and discoloration inhibitor, from Example 1 the soap ?akes developed a peroxide value of 0.4 and remained fresh for many months Y . about 0.005 per cent to about 1 per cent by weight in a shelf storage test whereas a product corre 40 in small particle form and having a relatively of triethylene tetrarnine, the said product being sponding in every way except_that it contained no triethylene tetramine preservative developed large surface area per unit weight and a rela tively low moisture content substantially corre- - a peroxide value of 9.0 in the accelerated test r , sponding to that of ?ake and spray dried granu and became rancid in about one month in the lar soap products. shelf storagetest. _ - 45 6. A soap product comprising essentially soap Soap products prepared from fat formulas other than that shown in the example will also be 'of which a minor proportion is rosin soap and, as a rancidity and discoloration inhibitor, from improved by the addition of the polyethylene polyamine preservatives of my invention. Thus ' about 0.005 per cent to about 1 per cent by weight greases, coconut oil, cottonseed foots fatty acid. ‘ responding to that of ?ake and spray dried gran of tetraethylene pentamine, the said product the invention may be employed to advantage in '50 being in small particle form and having a.re1a the production of soap products from rosin-con-v tively large surface area per unit weight and a taining formulas including various tallows and _ relatively low moisture content substantially cor f ular soap products. , etc. I have also found in the course of my work 7. A soap product in ?ake form comprising on the invention that the mineral acid salts. for essentially soap of which a ‘minor proportion is example, the sulfates oi the polyethylene poly~ 1' rosin soap and, as a rancidity and discoloration aminesabove referred to likewise have preserva inhibitor, from about 0.02 per cent to about 0.1 tive action comparable with that of the amines ‘ per cent by weight or a polyethylene polyarnine themselves when incorporated with the soap, and 60 oi the formula the invention is to be understood as including .55 their use. The chlorides, phosphates, etc., of the amines may also be incorporated if desired. > "wherein a: is a whole number from 1 to 3. Having thus described my invention, what I' 1 8. A soap product in spray dried form com claim and desire to secure by Letters Patent is: 05 l. The process of inhibiting the development of rancidity and discoloration in a granular soap ' product prepared from a fat formula containing ’ a, minor proportion of rosin, which comprises in corporating with the soap a polyethylene poly-- 70 amine of the formula H2N'C2H4' (HN'CsHO :“NH: wherein a: is a whole number from 1 to 3. 2. A soap product comprising essentially soap prising essentially soap of which a minor propor tion is rosin soap and, as a rancidity and discol-* oration inhibitor, from. about 0.02 per cent to about 0.1 per cent'of a commercial mixture of polyethylene polyamine consisting essentially of amines of the formula HaN-CaHr (HN-CzHOrN'H: wherein a: is. a whole number from 1 to 3. HERBERT KENNETH McCLAIN.