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Method for continuously producing N,N-diethyl formamide by one-step method

A technology of diethylformamide and diethylamine, which is applied in the preparation of carboxylic acid amides, chemical instruments and methods, separation/purification of carboxylic acid amides, etc., can solve problems such as difficulty in product separation, complex production process, and impact on product quality. , to achieve the effects of cheap and easy-to-obtain raw materials, low equipment investment, and reduced production costs

Active Publication Date: 2018-12-14
ZHEJIANG XINHUA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conversion rate of raw material diethylamine in this process is about 95%, unreacted diethylamine needs to be separated and recovered, and a small amount of diethylamine contained in the product will affect the product quality, and it needs to be stripped to be qualified. The production process is relatively complex
[0005] Reports such as Liu Xingquan (Applied Chemistry 1996, 5, 1-4) use sodium methylate as the main catalyst, propylene oxide as a cocatalyst, add diethylamine in the autoclave and pass into carbon monoxide to catalyze the synthesis of N, N-diethyl methyl Amide, the selectivity reaches 96%, but the reaction pressure is relatively high, the raw material diethylamine is completely converted, and it needs to be recycled. At the same time, there are problems with the recycling of propylene oxide, the process is complicated, and the product separation is difficult.

Method used

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  • Method for continuously producing N,N-diethyl formamide by one-step method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] as attached figure 1 For the process equipment shown, 120kg of diethylamine, 10kg of methanol and 2kg of sodium methoxide are added to a 200L Venturi jet reactor. After the nitrogen replacement is qualified, CO is introduced, and the Venturi jet reactor circulation pump is turned on. The reaction temperature is controlled at 120°C. , the reaction pressure is 1.5MPa, and after reacting for about 3 hours, the sample analysis diethylamine conversion rate is 100%, and the product selectivity is 98.9%. components, and then rectified under reduced pressure to obtain the product N,N-diethylformamide with a product content of 99.97%.

Embodiment 2

[0027] Add 120kg of diethylamine, 5kg of methanol and 1kg of sodium methoxide into a 200L Venturi jet reactor, return about 5kg of light components recovered by rectification to the reactor through the filter, and react the previous batch in the filter The catalyst left by filtration is brought into the reactor to continue to participate in the reaction. After the reactor is replaced with nitrogen, CO is introduced, and the Venturi jet reactor circulation pump is turned on. The reaction temperature is controlled at 100°C, the reaction pressure is 1.8MPa, and the reaction is about After 2.5 hours, sampling analysis showed that the conversion rate of diethylamine was 100%, and the product selectivity was 98.7%. , N-Diethylformamide, the product content is 99.96%.

Embodiment 3

[0029] Add 100kg of diethylamine, 15kg of methanol and 4kg of sodium methoxide into a 200L Venturi jet reactor, pass CO into the reactor after passing the nitrogen replacement, turn on the circulation pump of the Venturi jet reactor, control the reaction temperature to 100°C, and react The pressure was 2 MPa, and after about 2 hours of reaction, the conversion rate of diethylamine was 100% and the product selectivity was 98.8%. The reaction material is filtered through a filter at a rate of 75kg / h and cooled, and then sent to the crude product tank to be rectified. At the same time, the diethylamine feed pump and the configured methanol sodium methoxide solution pump are turned on, and the diethylamine is fed at a rate of 40kg / hour. Add the sodium methoxide and methanol into the reactor at a rate of 3:10, then feed them into the reactor at a rate of 0.15kg / h through the feed pump, while maintaining the pressure at 2MPa and the temperature at 100°C for continuous reaction , kee...

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Abstract

The invention relates to a process for continuously producing N,N-diethyl formamide by a one-step method, and belongs to the technical field of chemical engineering. According to the invention, diethylamine, carbon monoxide, methanol and sodium methoxide are used as raw materials, a reaction is carried out in a venturi injection reactor, and then the N,N-diethyl formamide is continuously producedthrough filtration and rectification. The process disclosed by the invention has the characteristics of cheap and easily available raw materials, simple process, high reaction speed, high production efficiency, good product quality, low equipment investment, less waste discharge, low production cost, suitability for continuous production, and the like.

Description

technical field [0001] The invention relates to a production process of N,N-diethylformamide, in particular to a one-step continuous production process of N,N-diethylformamide, which belongs to the technical field of chemical industry. Background technique [0002] N, N-diethylformamide CAS: 617-84-5; English name is N, N-Diethylformamide, abbreviated as DEF; molecular formula is C 5 h 11 NO; molecular weight 101.15; density 0.9049, boiling point 177-178°C, miscible with water, alcohol, ether, ketone, benzene, etc., has strong solubility, and is often used as a solvent, cleaning agent, extractant, etc. in industry. [0003] At present, the production process of DEF is mainly a two-step method of methyl formate, that is, the reaction of formic acid and methanol to prepare methyl formate, or the carbonylation of methanol and carbon monoxide to prepare methyl formate, and then the separation and purification of methyl formate and diethylamine The reaction produces N,N-diethyl...

Claims

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Application Information

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IPC IPC(8): C07C231/02C07C231/24C07C233/03C07C67/36C07C69/06
CPCC07C67/36C07C231/02C07C231/24C07C233/03C07C69/06
Inventor 刘承伟应思斌应登宇黄小鹏黄菊段小刚吴锦平方胜军刘训军贾建红徐卫中孙小林
Owner ZHEJIANG XINHUA CHEM