Method for preparing N,N-dimethylacetylamide

A technology of dimethylacetamide and methylacetamide, which is applied in the field of preparation of organic solvent N,N-dimethylacetamide, can solve the problems of high requirements for reaction conditions, high cost, and long reaction process, and avoid The effect of environmental pollution and short process

Active Publication Date: 2014-05-14
高楠
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The acetic anhydride method has defects such as high energy consumption, long reaction process, and high cost; the acetyl chloride method has problems such as high raw

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A preparation method of N,N-dimethylacetamide, weighing 10g of formaldehyde, 23g of formic acid, 5g of catalyst and 38g of water into the reactor, maintaining 60°C, stirring vigorously for 1h;

[0015] Add 24g of N-methylacetamide dropwise at a rate of 0.5d / s with a constant pressure dropping funnel, and maintain the reaction at 50°C for 2h;

[0016] The reaction solution was centrifuged at 3000 rpm for 30 minutes; filtered under reduced pressure with qualitative filter paper for 30 minutes, the resulting filtrate was distilled at -0.1MPa, 100°C for 5 hours under reduced pressure, and the fraction at 164-166°C was collected to obtain N,N-dimethylacetamide .

Embodiment 2

[0018] Yet another method for preparing N,N-dimethylacetamide. Weigh 10g of formaldehyde, 22g of formic acid, 5g of catalyst and 64g of water into the reactor, maintain 65°C, and vigorously stir for 1.5h;

[0019] Add 24g of N-methylacetamide dropwise at a rate of 0.5d / s with a dropping funnel, and maintain the reaction at 55°C for 3h;

[0020] The reaction solution was centrifuged at 3000 rpm for 30 minutes; filtered under reduced pressure with qualitative filter paper for 30 minutes, the resulting filtrate was distilled at -0.1MPa, 105°C for 6 hours under reduced pressure, and the fraction at 164-166°C was collected to obtain N,N-dimethylacetamide .

Embodiment 3

[0022] Weigh 10g of formaldehyde, 21g of formic acid, 5g of catalyst and 106g of water into the reactor, maintain 70°C, and vigorously stir for 2h;

[0023] Add 25g of N-methylacetamide dropwise at a rate of 0.5d / s with a dropping funnel, and maintain the reaction at 60°C for 4h;

[0024] The reaction solution was centrifuged at 3000 rpm for 30 minutes; filtered under reduced pressure with qualitative filter paper for 30 minutes, the obtained filtrate was distilled at -0.1MPa, 110°C for 3 hours under reduced pressure, and the fraction at 164-166°C was collected to obtain N,N-dimethylacetamide .

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Abstract

The invention discloses a method for preparing N,N-dimethylacetylamide. The method comprises the following steps: by taking formaldehyde, formic acid and N-methylacetamide as raw materials, firstly, enabling formaldehyde to react with the formic acid to form an active intermediate under a catalyst and the heating condition; secondly, enabling the generated active intermediate to react with the N-methylacetamide, so as to form the N,N-dimethylacetylamide; finally, obtaining the N,N-dimethylacetylamide from the product by the processes of centrifuging, filtering, vacuum distillation and the like. The method is short in preparation flow, and low in reaction temperature, and has the advantages of being low in temperature, environmental, and short in flow, and the problem of environmental pollution in the preparation process is avoided.

Description

[0001] technical field [0002] The invention relates to a preparation method of an organic solvent N,N-dimethylacetamide. Background technique [0003] N,N-Dimethylacetamide has the advantages of thermal stability, hydrolysis resistance and corrosion resistance, and is widely used in the synthesis of polyimide, polysulfone amide and other resins. Therefore, it has been paid more and more attention by people. [0004] At present, the preparation methods of N,N-dimethylacetamide mainly include acetic anhydride method, acetyl chloride method and acetic acid method. These methods all use acetic anhydride (or acetyl chloride or acetic acid) and dimethylamine as raw materials, and undergo a substitution reaction in the presence of a catalyst to form N,N-dimethylacetamide. The acetic anhydride method has defects such as high energy consumption, long reaction process, and high cost; the acetyl chloride method has problems such as high raw material cost and high requirements for r...

Claims

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Application Information

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IPC IPC(8): C07C233/05C07C231/08C07C231/10
Inventor 余旺旺
Owner 高楠
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