Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing N,N-dimethylacetylamide

A technology of dimethylacetamide and formaldehyde, which is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high requirement of reaction conditions, high cost, long reaction process, etc., and avoid environmental problems. Pollution, short process effect

Active Publication Date: 2015-06-17
高楠
View PDF2 Cites 0 Cited by
  • Summary
  • 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 material costs and high requirements for reaction conditions; the acetic acid method has defects such as high energy consumption, long reaction process, and high cost

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] 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;

[0014] 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;

[0015] 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

[0017] 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;

[0018] 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;

[0019] 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

[0021] 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;

[0022] 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;

[0023] 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 .

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

technical field [0001] The invention relates to a preparation method of an organic solvent N,N-dimethylacetamide. Background technique [0002] 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. [0003] 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 reaction c...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/05C07C231/08C07C231/10
Inventor 余旺旺
Owner 高楠
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com