Method For The Production Of N,N-Dimethylacetamide (Dmac)

Abstract

A process for preparing N,N-dimethylacetamide (DMAC) by continuously reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a basic catalyst, wherein MeOAc is used in the form of a methanolic solution which is obtained as a by-product in the preparation of polyTHF by transesterifying polyTHF diacetate with methanol.

1 - 21 . (canceled) 
     
     
         22 . A process for preparing N,N-dimethylacetamide (DMAC) comprising the step of continuously reacting methyl acetate (MeOAc) with dimethylamine (DMA) in the presence of a basic catalyst, wherein said MeOAc is in the form of a methanolic solution obtained as a by-product in the preparation of polyTHF via transesterification of poyTHF diacetate with methanol. 
     
     
         23 . The process according to  claim 22 , wherein said reaction is carried out at a temperature in the range from 80 to 140° C. 
     
     
         24 . The process according to  claim 22 , wherein said reaction is carried out at an absolute pressure in the range from 3 to 30 bar. 
     
     
         25 . The process according to  claim 22 , wherein said methanolic MeOAc solution comprises from 70 to 85% by weight of MeOAc, from 14.8 to 25% by weight of methanol from 0.1 to 1.5% by weight of dimethyl ether, from 0.1 to 3.5% by weight of tetrahydrofuran (THF), and from 0 to 0.01% by weight of water. 
     
     
         26 . The process according to  claim 22 , wherein said methanolic MeOAc solution comprises from 75 to 82% by weight of MeOAc, from 17.6 to 22% by weight of methanol, from 0.2 to 1.2% by weight of dimethyl ether, from 0.2 to 1.5% by weight of THF, and from 0 to 0.003% by weight of water. 
     
     
         27 . The process according to  claim 22 , wherein said catalyst is sodium methoxide. 
     
     
         28 . The process according to  claim 27 , wherein said catalyst is in the form of a methanolic solution. 
     
     
         29 . The process according to  claim 22 , wherein said catalyst is present in the range of from 0.0002 to 0.09 mole per mole of MeOAc. 
     
     
         30 . The process according to  claim 22 , wherein said reaction is carried out in a jet loop reactor. 
     
     
         32 . The process according to  claim 30 , wherein said jet loop reactor comprises an insert tube and a nozzle located at the bottom of said jet loop reactor. 
     
     
         32 . The process according to  claim 22 , comprising the additional step of neutralizing said catalyst present in the reactor effluent after the reaction and before distillative workup by reacting said catalyst with a protic acid or by decomposing said catalyst with water. 
     
     
         33 . The process according to  claim 32 , wherein said protic acid is phosphoric acid. 
     
     
         34 . The process according to  claim 32 , comprising the additional step of removing the organic product mixture after neutralization with a protic acid and before distillative workup by evaporating said organic product mixture from salts present after the reaction. 
     
     
         35 . The process according to  claim 22 , comprising the additional step of continuously distillatively working-up reaction effluent in a column A, wherein methanol and any other low boilers are initially removed overhead in column A, followed by feeding the bottom effluent of column A to a column B, wherein DMAC is removed via a side draw, and wherein said DMAC has a purity of greater than or equal to 99.7% by weight. 
     
     
         36 . The process according to  claim 35 , wherein said DMAC is removed in column B via a liquid side draw which is disposed in the rectifying section of column B. 
     
     
         37 . The process according to  claim 35 , wherein the top effluent of column B comprises DMAC and is recycled back into column A. 
     
     
         38 . The process according  claim 35 , wherein the bottom effluent of column B is separated into a column C, wherein the top effluent of column B is recycled into column A, and wherein said top effluent comprises DMAC and methanol. 
     
     
         39 . The process according to  claim 35 , wherein the top effluent of column A comprises methanol and is purified in a column D. 
     
     
         40 . The process according to  claim 22 , wherein the DMAC prepared has a purity of greater than or equal to 99.7% by weight, a water content of less than or equal to 200 ppm, and a Pt/Co color number less than or equal to 10. 
     
     
         41 . The process according to  claim 22 , wherein the DMAC prepared has an acid content calculated as acetic acid of less than or equal to 80 ppm. 
     
     
         42 . The process according to  claim 22 , wherein said process is carried out in a plant wherein DMF can also be prepared from carbon monoxide and DMA.