Self-binding acid integrated production method of n,n-dimethylchloroethylamine and tetramethylethylenediamine

A technology of tetramethylethylenediamine and dimethylchloroethylamine, which is applied in the field of co-production of important intermediates N,N-dimethylchloroethylamine and tetramethylethylenediamine, which can solve industrial production problems The limited significance of benzene, the high toxicity of benzene as a solvent, etc., achieve the effect of safe reaction, simple post-processing operation, simple and clean process

Active Publication Date: 2021-04-16
恒光新材料(江苏)股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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-binding acid integrated production method of n,n-dimethylchloroethylamine and tetramethylethylenediamine
  • Self-binding acid integrated production method of n,n-dimethylchloroethylamine and tetramethylethylenediamine
  • Self-binding acid integrated production method of n,n-dimethylchloroethylamine and tetramethylethylenediamine

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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] The yield of N,N-dimethylchloroethylamine in step (4) was 17.6%, and the yield of tetramethylethylenediamine was 80.9%.

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Abstract

The invention discloses a self-binding acid integrated production method of N,N-dimethylchloroethylamine and tetramethylethylenediamine, which comprises the following steps: 1) reacting with dimethylamine aqueous solution and dichloroethane Raw materials, adding an acid-binding agent with an equimolar amount of dimethylamine to the reaction raw materials for heating reaction, the heating reaction temperature is 30-90°C, the reaction pressure is 1-3MPa, and the reaction time is 3-8h; 2), the step 1) The resulting reaction product is post-treated to obtain an aqueous solution of N,N-dimethylchloroethylamine and tetramethylethylenediamine and dichloroethane; N,N-dimethylchloroethylamine and tetramethyl The aqueous solution of ethylenediamine is subjected to vacuum rectification, thereby respectively obtaining N,N-dimethylchloroethylamine as a light component and tetramethylethylenediamine as a heavy component. The method of the present invention is adopted to co-produce tetramethylethylenediamine while producing N,N-dimethylchloroethylamine.

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 Patents(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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