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Self-acid-binding integrated production method for N,N-dimethyl chloroethylamine and tetramethylethylenediamine

A technology of tetramethylethylenediamine and dimethylchloroethylamine is applied in the field of co-production preparation of important intermediates N,N-dimethylchloroethylamine and tetramethylethylenediamine, and can solve the problem of benzene production. Solvent toxicity is high, the significance of industrial production is limited, etc., to achieve the effect of high total yield, reaction safety, and high industrial application value

Active Publication Date: 2018-12-14
恒光新材料(江苏)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Benzene is highly toxic as a solvent, and this method has limited significance for industrial production

Method used

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  • Self-acid-binding integrated production method for N,N-dimethyl chloroethylamine and tetramethylethylenediamine
  • Self-acid-binding integrated production method for N,N-dimethyl chloroethylamine and tetramethylethylenediamine
  • Self-acid-binding integrated production method for N,N-dimethyl chloroethylamine and tetramethylethylenediamine

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Experimental program
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Effect test

Embodiment 1

[0047] Embodiment 1, a kind of technique of producing N,N-dimethylchloroethylamine and co-production of tetramethylethylenediamine. Taking dichloroethane and 33% dimethylamine aqueous solution as starting materials, the following steps are carried out successively:

[0048] (1) Synthesis:

[0049] Add 67.5g dimethylamine aqueous solution (0.5mol, mass concentration is 33%), 148.5g dichloroethane (1.5mol) and 58g acid-binding agent tetramethylethylenediamine (0.5mol) in 500ml autoclave, will After replacing the reactor with nitrogen for 3 times, fill it with nitrogen to 1.5MPa, start stirring, raise the temperature to 35°C for reaction, and the reaction time is 5h, and the resulting reaction solution is collected.

[0050] (2) Separation:

[0051] The reaction solution in step (1) was allowed to stand, separated into layers, and the water layer was set aside (the water layer was composed of water, tetramethylethylenediamine hydrochloride and other components), and the organic...

Embodiment 2-6

[0068] Embodiment 2-6, change the reaction pressure in embodiment 1 into 3MPa, all the other are equal to embodiment 1;

[0069] The yield of N,N-dimethylchloroethylamine in step (2) is 23.2%, and the yield of tetramethylethylenediamine is 75%.

[0070] In step (4), the yield of N,N-dimethylchloroethylamine was 23.0%, and the yield of tetramethylethylenediamine was 75.1%.

Embodiment 2-7

[0071] Embodiment 2-7, change the mol ratio of dimethylamine and dichloroethane in embodiment 1 into 1:1, all the other are equal to embodiment 1;

[0072] The yield of N,N-dimethylchloroethylamine in step (2) is 18%, and the yield of tetramethylethylenediamine is 80.8%.

[0073] In step (4), the yield of N,N-dimethylchloroethylamine was 17.6%, and the yield of tetramethylethylenediamine was 80.9%.

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Abstract

A self-acid-binding integrated production method for N,N-dimethyl chloroethylamine and tetramethylethylenediamine is disclosed. The method includes 1) adding an acid binding agent the mole of which isequal to that of dimethylamine into an aqueous dimethylamine solution and dichloroethane which are adopted as reaction raw materials, and performing a reaction under heating, with the heating reaction temperature being 30-90 DEG C, the reaction pressure being 1-3 MPa, and the reaction time being 3-8 h; and 2) subjecting a reaction product of the step 1) to after-treatment to obtain dichloroethaneand an aqueous solution of N,N-dimethyl chloroethylamine and tetramethylethylenediamine, and subjecting the aqueous solution of N,N-dimethyl chloroethylamine and tetramethylethylenediamine to rectification under vacuum to obtain the N,N-dimethyl chloroethylamine as a light component and the tetramethylethylenediamine as a heavy component. The method can be used for coproduction of the tetramethylethylenediamine and the N,N-dimethyl chloroethylamine.

Description

technical field [0001] The invention belongs to the fine chemical industry, and relates to a coproduction preparation method of important intermediates N,N-dimethylchloroethylamine and tetramethylethylenediamine. Background technique [0002] N,N-Dimethylchloroethylamine, the molecular formula is C 4 h 10 ClN, widely used in medicine, pesticides, surfactants and dyes and other industries; Tetramethylethylenediamine, the molecular formula is C 6 h 16 N 2 , commonly used as biochemical reagents and epoxy resin crosslinking agent, its structural formula is as follows: [0003] [0004] The preparation of N,N-dimethylchloroethylamine mainly adopts the following methods: [0005] Method 1: Patent CN107445847 reports a chlorination reaction with N,N-dimethylethanolamine as raw material with thionyl chloride, and the temperature is controlled at 10-15°C to obtain the finished product N,N-dimethylchloroethylamine salt salt. The process steps are simple and the yield is hig...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/15C07C211/10C07C209/08C07C209/86
CPCC07C209/08C07C209/86C07C211/15C07C211/10
Inventor 张超魏梦怡张华张琪丁东升
Owner 恒光新材料(江苏)股份有限公司
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