US1018733A - Process of manufacturing anhydrids of fatty acids. - Google Patents

Description

J. WEBER. v PROCESS OF'MANUFAOTURING ANHYDRIDS OF FATTY ACIDS.

APPLICATION FILED JUNE 30, 1911.

1.1 Patented Feb. 27, 1912 mltnasses; I Imam?- I WI Q i Y HMm-M his 09650271265 UNITED ,STATES PATENT OFFICE} JOSE! WEBER, F ESSEN-ON-THE-RUHR, GEBM IJAN Y.

PROCESS or menuracrunme Amnrpnms or mm? ACIDS.

'1'0 all whom it may concern:

Be it known that 1, Jose!" Vi-men, subject of the King of Prussia, (ierman Emperor, resident of Essen-on-the-Ruhr, in the German Empire, have invented a new and useful Process of Manufacturing Anhydrids of Fatty Acids, of which the following is an exact specification.

fatty acid salt or from a mixture of salts of This invention relates to an improved process of manufacturing'anhydrids of fatty acids, especially acetic anhydrld, from a out with much less trouble by mixing a fatty acid salt or salts in a dry state with sulfur, usually in the form of powder of sulfur or flowers of sulfur, and acting on this mixture with dry chlorin, good results having been obtained by taking the materials in proportion, for example, of about 8 molecules of acetate (ofa monobasic metal) to 1 atom of sulfur, these proportions, however, not being essential. In the process of the aforesaid application the reaction took place at a 7 lowtemperaturm-say at 20 (1. or less+ carrying out the process .of the aforesaid and. at that time the carrying out ofthe .process at a'low temperature seemed to be essential. At the end of the operation of application-the product obtained by the reaction was moderately heated for some time in order to transform any fatty acid .chlorid stillpresent into anhydrid, after which the anhydridwas eventually distilled in wmw in a manner'well understood. I have found,

however, that in carrying out the process of the aforesaid application, especially with acetic anhydrid, tl e reaction on which said process is based takes place not only at the low'temperatures above mentioned (as set forth in the prior application, but that,it also takes place, and thatit is possible to Specification of Letters Patent.

Application filed June 30, 1911. --Serial No. 688,137.

I Patented Feb. 27, 1912.

higher temperatures, if the mixture of the fatty acid salt or acetate with sulfur is acted upon by chlorin in the presence of a suitable diluting or distributing substance, such for example as acetic anhydrid. The temperature upto which such reaction may take place with good results may be said to be An important advantage resulting from the carrying out of thisimprovedprocess is that it is not necessary in the present case,- as it was in the process described in the aforesaid application, to maintain during the reaction temperatures which are only ohtainable by the use of refrigerating machines. Thus in the present case, as these refrigerating machines are not required, both the process and the apparatus for carrying out the process are simplified in a high degree, and by this simplification the manufacture of fatty acid anhydrid, and particularly acetic anhydrid, on a large scale is facilitated and can be eli'ected at much lower cost than in the case of the process described in the former application.

In the drawing apparatus suitable for carrying out the improved process is illustrated.

Referring to said drawing, 2 designates a tightly closed reaction chamber or vessel into which the mixture to be acted upon has been introduced. A stirrer or means for keeping in motion the substance forming the charge is illustrated at 3. It may be operated by any suitable mechanism, such as that shown at 4-. The chlorin employed, which should be in a dry state, may be admitted at 5, and its flow regulated or varied 'as desired. as for example by means of a valve 6. The anhydrid resulting from the reaction will in this case leave the reaction vessel-through a pipe 7. which may also have 'a'valve 8 therein, by means ofwvliichwommunication with the reaction vessel may be made or cut off as required, The pipe 7 leads to the coils of a condenser 9, in which the anhydrid distilled over fromthe reaction vessel. 2 is condensed and from 'which the liquid distilled passes to a receiving-yessel 10. a t

g In order to make clear the manner in sel kilograms of carefully dried sodium which this process is practiced the following -1S given as one example: In the reactlonvesacetate are mixed with at least 16 kilograms of sulfur or flowers of sulfur andan amount fatty aci of acetic anhydrid equal to the uantity of sodium acetate used. The vesse [2 is then tightly closed and this mixture at a temperature of say 25 C., the mixture being at the same time thoroughly stirred. If desired the react-ion vessel may be exhausted before introducing the chlorin. The introduction of chlorin is so regulated that in say 5 hours at least 106% kilograms V vessel. The chlorin admitted is quickly taken up by the mixture and the pressure prevailin in the chamber 2 at the end of the reaction usually exceeds that at the beginning by only 'one tenth of an atmosphere or a little more. It is believed to be unnecessary to consider whether in this reactionthe acetic anhydrid present only acts as a diluent or distributing means, or whether its action is a catalytlc one that results in advancing the reaction.

At the end of the reaction the resulting liquid anhydrid may be distilled. substantially as in my aforesaid application. ,As in the former case it is advlsable to hold a high vacuum during distillation, as it is only with the highest degree of vacuum that the output of anhydrid will be' approximately the theoretical one, i. 204 kilograms.

What I claim is:

1. A process for the production of fatty acid anh drid, which consists in mixing a d salt with sulfur, both being in a dry state, chlorin at tem eratures up to 4050 C. in the'presence o a suitable diluent.

2. A rocess for the production of fatty acid'an ydrid, which consists in mixing a fatty acid salt with sulfur, both being in a dry state,

chlorin introduced into will have entered the reaction and; treating the mixture with and treating the mixture with chlorin at temperatures up to 4050 C. in

the presence of an anhydrid of a fatty acid.

3. A process for'the production of acetic anhydrid which consists in mixing an acetate with sulfur, both being in a dry state, and treating the mixture with chlorin at temperatures u to 40-50 C. in the presence of, acetic anhy rid.

4. A process for the production of fatty acid anhydrid, which consists in mixing a plurality of salts of the same fatty acid with sulfur, all being in a dry state, and treating the mixture with chlorin at temperatures up to 40-50 C, in the presence of a suitable diluent. g

5. A process for the production of fatty acid anhydrid, which consists in mixing a plurality of salts of the same fatty acid with sulfur, all being in a dry state, and treating the mixture with chlorin at temperatures up to 40-50 C. in the'presence of an organic acid anhydrid. V 6. A process acid anhydrid, which consists in mixing a plum lity of salts of the same fatty acid with sulfur, all being in a dry state, and treating the mixture with chlorin at temperatures-up to 4050 C. in the presence of an anhydrid of the same fatty acid. y

7. A process for the production of acetic anhydrid, which consists in mixing a lurality of acetates with sulfur, all being in a dr state, and treating the mixture with ch orin at temperatures up to 4050 C. in the presence of acetic anhydrid.

, JOSEF WEBER. a 8.

Witnesses CHAS. J. WRIGHT, ALFRED HENKEL.

for the production .of fatty

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