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Preparation method of continuous production of diethylformamide

A technology of diethylformamide and a production method is applied in the preparation of carboxylic acid amides, the preparation of organic compounds, chemical instruments and methods, etc., and can solve the problems of fire, large reactors, increased separation energy consumption and material consumption, etc., Achieve the effect of high yield, simple industrial scale-up and low material consumption

Active Publication Date: 2014-07-16
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These defects will result in the need to use larger reactors, and are prone to extreme hazards such as fire, separation energy consumption and material consumption increase

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method for continuous production of diethylformamide, in a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and then converted into diethylformamide by amidation reaction , the finished product diethylformamide is obtained through refining.

[0028] The reaction conditions are: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, and the liquid phase space velocity is 15.0h -1 , the reaction temperature is controlled at 80°C, and the reaction pressure (gauge pressure) is normal pressure ~0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of aluminum oxide, magnesium oxide and zirconium oxide.

[0029] The heterogeneous catalyst is strip-shaped with a maximum length of 2 mm.

[0030] The water content of diethylamine is 0.2 wt%.

[0031] The methanol content in methyl formate was 0.1 wt%.

[0032] Measure export product, diethylamine conversion rate is ...

Embodiment 2

[0034] A preparation method for continuous production of diethylformamide, in a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and then converted into diethylformamide by amidation reaction , the finished product diethylformamide is obtained through refining.

[0035] The reaction conditions are as follows: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, the liquid space velocity is 10.0h-1, the reaction temperature is controlled at 60°C, and the reaction pressure (gauge pressure) is normal pressure~0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of titanium oxide and calcium oxide.

[0036] The heterogeneous catalyst is spherical, with a maximum length of 3 mm.

[0037] The water content of diethylamine is 0.1wt%.

[0038] The methanol content in methyl formate was 0.05 wt%.

[0039] Measure the export product, the diethylamine conversion rate is 99.5%, and t...

Embodiment 3

[0041] A preparation method for continuous production of diethylformamide, in a closed tubular reactor filled with a heterogeneous catalyst, diethylamine and methyl formate are mixed and then converted into diethylformamide by amidation reaction , the finished product diethylformamide is obtained through refining.

[0042] The reaction conditions are: the molar ratio of diethylamine to methyl formate is 1.0~1.1:1.0, and the liquid phase space velocity is 5.0h -1 , the reaction temperature is controlled at 50°C, and the reaction pressure (gauge pressure) is normal pressure ~0.2MPa. The chemical composition of the heterogeneous catalyst is: a mixture of aluminum oxide, magnesium oxide and zirconium oxide.

[0043] The heterogeneous catalyst is spherical with a maximum length of 1.5mm.

[0044] The water content of diethylamine is 0.4wt%.

[0045] The methanol content in methyl formate was 0.08 wt%.

[0046] Measure the export product, the diethylamine conversion rat...

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Abstract

The invention relates to a method for producing diethylformamide. The invention relates to a preparation method for continuous production of diethylformamide, which comprises the following steps: mixing diethylamine and methyl formate, converting to diethylformamide through an amidation reaction, and refining to obtain the finished product diethylformamide; wherein the mol ratio of diethylamine to methyl formate is 1.0-1.1: 1.0, space velocity of the liquid phase is 1.0-20.0h<-1>, the reaction temperature is controlled at 10-80 DEG C, and the reaction pressure (gauge pressure) is between normal pressure and 0.2MPa. The method has the advantages of high yield, because that high mol ratio of methyl formate to diethylamine is not required, diethylamine conversion rate is high, and the material consumption of whole process is little. The preparation method makes DEF production to serialization, so that the production efficiency of the process is increased, and the investment and production cost can be greatly reduced.

Description

Technical field: [0001] The present invention relates to a kind of production method of diethylformamide. Background technique: [0002] N, N-Diethylformamide (DEF), the English name is N, N-Diethylformamide, abbreviated as DEF; the molecular formula is C 5 h 11 NO; molecular weight is 101.15; density is 0.9049, boiling point is 177~178°C, it is a colorless and transparent polar organic solvent with low density and high boiling point, miscible with water, alcohol, ether, ketone, benzene, etc., and has strong solubility It can dissolve many organic polymers, such as polyacrylonitrile, urethane prepolymer, PVC, vinylidene chloride-vinyl chloride copolymer, polyvinyl formal, polyimide and other polymers, so DEF can be used as an industrial solvent to replace N,N-dimethylformamide (DMF), and its toxic and side effects are far less than DMF. In addition, DEF also has potential application value in the field of fiber synthesis and pharmaceutical synthesis. [0003] Liu Xingqua...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/03C07C231/02
Inventor 宋国全肖强杨理闫广学
Owner MAIQI CHEM CO LTD
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