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Process for synthesizing dimethylacetamide by ethyl acetate and dimethylamine

A technology of dimethylacetamide and ethyl acetate is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of high cost, increased investment, and no industrialized reports, etc. The effect of low production cost, reduced corrosion, high industrial application value

Inactive Publication Date: 2006-07-26
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the increase in investment due to the corrosion of acetic acid, the cost of producing N,N-dimethylacetamide by this route is relatively high; the liquid-phase batch reaction process of acetic acid and dimethylamine is carried out under high temperature and high pressure conditions, and industrialized devices are also introduced. Molybdenum trioxide is used as a catalyst to reduce the reaction conditions, increase the reaction speed and increase the yield of DMAC
In addition, there are many studies on the synthesis of DMAC by the reaction of acetic acid, ammonia and methanol, and the carbonylation reaction of trimethylamine and CO, but there is no industrial report yet.

Method used

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  • Process for synthesizing dimethylacetamide by ethyl acetate and dimethylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add ethyl acetate (720g), dimethylamine (420g), molybdenum trioxide catalyst (3.6g) and tungsten trioxide catalyst (3g) into A (tank reactor), then raise the temperature to 142°C, and naturally raise the pressure to 2.0 Mpa, stirred and reacted for 24 hours, the reaction liquid was cooled and separated to remove the catalyst, and the reaction product was continuously rectified through B (rectification tower I) and C (rectification tower II) to separate dimethylamine, ethyl acetate and ethanol, and the crude distillation product The product N, N-dimethylacetamide can be obtained by rectification. Excess dimethylamine, ethyl acetate and part of ethanol circulate in the system. The conversion rate of ethyl acetate is 92.6%, and the selectivity of N,N-dimethylacetamide is ≥99%.

Embodiment 2

[0022] Add ethyl acetate (720g), dimethylamine (420g) and molybdenum trioxide catalyst (8g) into A (tank reactor), then raise the temperature to 172°C, pressurize to 2.5Mpa, stir and react for 20 hours, and the reaction solution The catalyst is separated and removed by cooling, and the reaction product is continuously rectified through B (rectification tower I) and C (rectification tower II) to separate dimethylamine, ethyl acetate and ethanol, and the crude distillation product is obtained by rectification to obtain the product N, N- Dimethylacetamide. Excess dimethylamine, ethyl acetate and part of ethanol circulate in the system. The conversion rate of ethyl acetate is 92.4%, and the selectivity of N,N-dimethylacetamide is ≥99%.

Embodiment 3

[0024] Ethyl acetate (720g), dimethylamine (420g) and tungsten trioxide catalyst (3g), molybdenum trioxide catalyst (3g) and sodium metavanidate catalyst (3g) were added to A (tank reactor), then the temperature was raised To 165°C, pressurize to 2.2Mpa, stir and react for 20 hours, the reaction liquid is cooled and separated to remove the catalyst, and the reaction product is continuously rectified to separate dimethylamine and acetic acid through B (rectification tower I) and C (rectification tower II) Ethyl ester and ethanol, the crude distillation product is rectified to obtain the product N, N-dimethylacetamide. Excess dimethylamine, ethyl acetate and part of ethanol circulate in the system. The conversion rate of ethyl acetate is 92.8%, and the selectivity of N,N-dimethylacetamide is ≥99.2%.

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Abstract

The related preparation method for DMAC comprises: using ethyl acetate and dimethylamine by mole ratio as 1: 0. 8~2 as material and at least one of tungsten trioxide, molybdenum trioxide and sodium metavanadate as catalyst to compose the product on condition of 0. 8~2. 5MPa and 80~190Deg. This invention has 92% conversion of ethyl acetate as high material utilization and product purity more than 99. 5%.

Description

Technical field: [0001] The invention relates to a process synthesis method of an important chemical product dimethylacetamide, in particular to a process method for preparing N,N-dimethylacetamide by liquid-phase reaction of ethyl acetate and dimethylamine. Background technique: [0002] N, N-Dimethylacetamide N, N-dimethylacetamide (abbreviated as DMAC) is a colorless transparent liquid with low toxicity, can dissolve a variety of inorganic compounds, and can be compatible with water, alcohol, ether, ester and aromatic compounds Miscible. It has good stability under the condition of anhydrous, acid or alkali. It is an excellent polar solvent for synthesizing natural resins. It is used in the synthesis of polyimide, polysulfone amide and other polymer compounds. It is also used in the film-forming and spinning of synthetic resins, synthetic drugs, aromatic dicarboxylic acids (such as The crystallization and purification of terephthalic acid) are widely used in synthetic m...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C233/05
Inventor 张晓阳胡志彪刘婷黄宏李倩刘京林
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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