US1560626A - Process for the manufacture of high-percentage, nondecomposable, durable soap - Google Patents

Description

Patented Nov. 10, 1925.

" NI ED S ATE PATENT ol-"r ce.

.AJJOLF WELTER, or xnarnnn-rznmnnnn, GERMANY.

raocnss roa 'rnn nanurac'runr. or man-rancnn'raes, nonnncomrosnta' DUBABLE soar.

7 K Drawing.

To all whom it may concern:

Be it, known'that I, ADOLF zen of the German Empire, residing at Krefeld-Pzeinhafen, Germany, have invented new and useful Improvements in aProcess for the Manufacture of High-Percent age, Nondecomposable, Durable Soap, of which the following is aspecification. The soap industry has endeavoured in the 10 lastfe'w years to put on the market soaps of as high a percentage of sappnification as possible, which shall not be friableand which shall be durable, in powder or solid form.

The oldest but also the most expensive process of manufacture for the said purpose consists in this that fluid soap -is cooled into slabs which are cut off in small pieces and dried until the product is capable of be ing ground. This process requires much time, heat and power. I

Another process consists A in this that more or less concentrated soap solutions are mixed with calcined soda, the reaction mass is cooled and ground. By this process, alkaline soaps are obtained which destroy the textile fibres, and in the case where .blocks are pressed from the powder so obtained, these blocks disintegrate in a short time and become simply soda decompositions. The soaps so obtained cannot be manufactured with high contents of fatty; acids. In

order to render this possible, ithasalso been tried to mix pulverized resins or stearin with calcined soda and to press the mixture, if required, into briquettes. In this manner, however, soaps are obtained which still contain a high percentage of unsaponified stearic acid or resin. v

it has, further been attempted to heat castor oil fatty acid in an iron vessel provided with a stirring mechanism and to add calcined soda slowly until everything is saponified and the carbonic acid is driven ofi'. This process can only be used for castor oil fatty acids and since these castor oil soaps have no importance whatever for washing purposes and are to expensive, this .of practical importance. .With all other fatty acids under similar circumstances, bady mixed lumpy -masses would be obtained which contain partly a strong excess ofsoda and partly free fatty acids.

WELTER, citiprocess of soap manufacture has not become Application and Ianuary S, 1923. Serial 110. $1,500.

The inventor has now found outthat if absolutely homogeneous mass is obtainedwhich becomes heated after a short time 7 and forms a completely saponified, highly concentrated soapy mass which does not containany more soda. If the double quantity of soda which is necessary for saponification is not exceeded, then the process is carried out in such a manner, that quantitively more orless water free sodium soaps and sodium" Y bicarbonate/are formed. These have no alkaline reaction and may be used for W001, silk and also for the human skin. They can alsobe suitably hardened and cooled, and after cooling easily pulverized. The most important point however is that the blocks 1 which are pressed-from the powder last indefinitely, do not burst and do not show any soda decompositions. The process is carried out in such a manner that the fatty acids arehcated in apparatuses having a stirrin device, a little above the melting point, and a molecule of calcined soda is "added to a molecule of fatty acid until everything is his mixed to form a homogeneous mass.

mass is allowed to become heated by the heat which itself generates until a sample taken does not give any unsaponified fatty acids with ether, whereupon either the mass which is still hot is formed into bands or extrusions, or the cooled mas-sis ground and the soap so obtained is put on the market either as such or pressed into briquettes or blocks.

It-is also possible to replace 'one part of soda by potash and a part of .the fatt acids by resin. It is also possible to add at dissolving means to the fatty acids, whereby the process is carried out equally well and effective washing whereby particularly means are obtained. The heating generated varies according to the 1- fats used. 'With oxidizable fatsthe' heating may be generated by simultaneous oxidation until the carbonization takes place, in which case care should be taken that the mass to be cooled shall ture of the fatty acids, the more uniform is the mixture, and the smaller is the uantity of carbonic acid which is develop in the reaction massso that only the sodium salt are formed.

ether.

Usually the finer and the more free of water the calcined soda used, the easier it is to carry the process out. It has been shown that with not too large contents of calcined soda absolutely homogeneous and completely saponified products are obtained which are capable of being ground and shaped,

which do not show any decomposition and the duration of which is unlimted.

I Example 1.

1000 kgs. of olein of an acidity number of 200 are given into a vessel provided with a stirring mechanism at a temperatureof 30 to 35 C., and 200 to 250 kgs. of well-ground calcined soda are added, whereby an entire ly homogeneous thin ulp is. obtained. When after a short stirring, the latter has become suificiently viscous so that it cannot be unmixed again, the reaction mass 'is allowed to settle on sheets of iron which are placed in drying chambers. The soapy pulp becomes then pufi'ed up during the next few hours according to the quantity of soda which is used owing to the formation of carbonic acid and produces a hard, porous, ho-

mogeneous soapy mass. This mass can be easily pulverized and dissolves easily and clearly in pure water, developing a strong lathering and high cleansing power. If only one molecule of water-free soda is used for two molecules of fatty acids, then when it is worked in small quantities a subsequent heating in driving chambers is necessary under certain circumstances for driving off the carbonic acid. In all cases, however, where a small excess of soda, and when one molecule of soda is used for one molecule fatty acid such'a strong heating is generated by the formation ofbicarbonate that comp ete saponification takes place after a short time. The end of the reaction is to be recognized by this that a sample taken being pulverized does not give any fatty acids with I Ewample 2.

1000 kgs. of fluid palm nut oil acid of an acidity of 250 is added in a steady stream at a temperature of 35 G. into a mixing drum having a good stirring mechanism, in which 450 to 500 kgs. of calcined soda have been previously introducedl A thin pulp is then obtained which becomes heated by the saponification which takes place, and becomes thicker and can finally be removed from the mixing vessel as an entirely homogeneous,

hard friable mass. On the following day,

- the reaction mass which has been formed is so hard'and brittle that it can be easily ground, does not feel fatty to the touch, and consists only of a mixture of soap and bicarbonate, which forms a clear solution with water and has high lathering and cleansing properties. Z p

' Example 3. 7 1000 kgs. of fluid distilled cotton oil, fatty acid (soapstock fatty acid) of an acidity number 202 are mixed in a mlxing drum havmg a strong stirring mechanism, with 400 kgs. of dried calcined soda at about 30 or 35 C. When the mass has become like a pulp and does not stick any longer, it is pressed by a screw lying at the bottom of the mixing vessel into an extrusion press and shaped either hydraulically or mechanically into extrusions of any suitable diameter. These, after a short time, by the complete saponification which vtakes place, become hard and brittle, have a good appearance and a long duration.

lln this process, it is possible by using suitable apparatus to manufacture soaps in r a continuous manner. The mode of working from the moment of the introduction of the fluid fatty acids until the outlet of the hard, saponified, saleable product, requires according to the temperature and to the kin of fatty acid, from a quarter of an hour to an hour.

Example 4,.

acid of an acidity number 255 are stirred.

together with 600 kgs. of calcined soda whichcontains 20% of water and is ground very finely into a mixing drum, whereby after a certain time the mass hardens into a dough, becomes warm afterwards and then becomes completely saponified. When the mass does .not stick any longer, it is shaped by means of an extrusion press into noodles or is ground aftercooling and pressed into blocks. The blocks which are'so obtained do not contain any more soda, but only bicarbonate and a little water. They do not burst, their duration is unlimited, and do not show any signs of decomposition even after one or more years of storage.

' Example 5.

- 1000 kgs. of fluid, distilled cotton oil, fatty acid -(soapstock fatty acid) of an acidity number 202 are mixed with 50 kgs. of turby a screw-lying at the bottom of the mixing vessel into an extrusion press, and shaped either hydraulically or mechanically into extrusions of any suitable diameter. These become hard and brittle in a short time, owing to the complete saponification that takes place, and have a good appearance and along duration. It is, of course, possible to allow the mass to cool, to' grind. it

the addition of water of no'n decomposable soap of high fatty acid content, by mixing;

at the temperature of the approximate melting point of the fatty acids, a measured quantity of water free alkaline carbonate with commercial fatty acids, said measured quantity being approximately double the quantity required for the com lete'saponification of said fatty .acid,.an said excess of alkaline carbonate being approximately the quantity necessary for the absorption by said excess of all the carbon dioxide resulting from said saponification whereby a soap is formed containing a substantial excess of the bicarbonate of said alkali and approximately no stronger alkaline impunities than said'bicarbonate of soda.

2. Aproce'ss for the manufacture without 7 the addltionof Water .of non-decomposable soa -of high fatty acid content, by mixing .wit commercial fatty acids at the temperature of the approximate melting, point: of

the fatty acids, an excess of a water free alkaline carbonate overthe normal amount required for saponification of said fatty acid, said excess'being retained in intimate mixture with said saponifying fatt acid to absorb the carbon dioxide libera by said saponification and permittin the mixture as herein noted to stand until a soap with a substantial quantity of the bicarbonate of said alkali is formed and in which only traces of the carbonate of said alkali remain. 3. .A rocess for the manufacture without the addition of water'of non-decomposable soap of high fattyacid content in powderedv or .solid form, by mixing at the temperature of the approximate melting point of'selected fatty acids, an 'excess of anhydrous alkaline carbonate over the normal amount required for saponificationof said selected fatty acids, retaining said excessin intimate mixture with said saponifying fatty, acid to absorb the carbon dioxide liberated by said saponification and: permitting the mixture as herein noted to-stand until a soap with a substantial quantity of the bicarbonate of said alkali is formed and in which onl minute traces of the carbonate of said alka i remain.

In' testimony whereof I have signed my name to this specification.

Dn. ADOLF VVELTER.