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Method for synthesizing N,N,N',N'-methylethylenediamine using transfer line reactor

A pipeline reactor, methylethylenediamine technology, applied in the chemical method for liquid-liquid reaction, chemical equipment and method, preparation of functional groups replaced by amino groups, etc., can solve the problem of harsh reaction conditions, catalyst recovery, and high price and other issues to achieve a good effect of safety

Active Publication Date: 2007-05-16
ZHEJIANG XINHUA CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the reaction conditions of this step are harsh, the reaction needs to be carried out under high pressure, and the raw material 2,3-dimethyl-2,3-dinitrobutane and catalyst Reynolds cobalt are expensive, and the recovery of the catalyst is also a problem

Method used

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  • Method for synthesizing N,N,N',N'-methylethylenediamine using transfer line reactor
  • Method for synthesizing N,N,N',N'-methylethylenediamine using transfer line reactor
  • Method for synthesizing N,N,N',N'-methylethylenediamine using transfer line reactor

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Embodiment 1

[0027] Embodiment 1: a kind of N, N, N', the synthetic method of N'-methylethylenediamine, reaction process is as follows:

[0028] Take 989.7g (1mol) of 1,2-dichloroethane, 410g of sodium hydroxide, 4508g (10mol) of dimethylamine, and 1950g of benzene. The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the temperature of the reactor jacket at 180°C, adjust the flow rate, divide the above raw materials into two groups and inject them into the pipeline reactor at the same time, the system pressure is 0.82Mpa, and the reaction residence time is 10 minutes. The synthetic solution was rectified, and the fraction at 119-121°C was extracted to obtain 1005 g of the product, with a yield of 86.50%.

Embodiment 2

[0029] Embodiment 2: a kind of N, N, N', the synthetic method of N'-methylethylenediamine, reaction process is as follows:

[0030] Take 989.7g (1mol) of 1,2-dichloroethane, 410g of sodium hydroxide, 3606g (8mol) of dimethylamine, and 1800g of toluene. The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the reactor jacket temperature at 150°C, adjust the flow rate, divide the above raw materials into two groups and inject them into the pipeline reactor at the same time, the system pressure is 0.68Mpa, and the reaction residence time is 8 minutes. The synthetic solution was rectified, and the fraction at 119-121°C was extracted to obtain 1018g of the product, with a yield of 87.60%.

Embodiment 3

[0031] Embodiment 3: a kind of N, N, N', the synthetic method of N'-methylethylenediamine, reaction process is as follows:

[0032]Take 989.7g (1mol) of 1,2-dichloroethane, 410g of sodium hydroxide, 2704g (6mol) of dimethylamine, and 1500g of methanol. The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the reactor jacket temperature at 120°C, adjust the flow rate, divide the above raw materials into two groups and pour them into the pipeline reactor at the same time, the system pressure is 0.46Mpa, and the reaction residence time is 12 minutes. The synthetic solution was rectified, and the fraction at 119-121°C was extracted to obtain 1048g of the product, with a yield of 90.10%.

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Abstract

The invention discloses a synthesizing method of N,N,N',N'-methyl ethanediamine, which comprises the following steps: adopting 1, 2-dichloroethane, sodium hydroxide solution and dimethylamine as raw material with the molar rate at 1.000:1.025:2.500-1.000:1.025:20.000; reacting in the pipe reactor under 0.1-2.0Mpa at 100-250 Deg C for 5-30min; setting the molar rate of 1, 2-dichloroethane and solvent at 1: 1-1: 10; rectifying the N,N,N',N'-methyl ethanediamine solution; separating dimethylamine from solvent; circulating solvent; rectifying again to obtain the product.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for synthesizing N, N, N', N'-methylethylenediamine using a pipeline reactor. Background technique [0002] N, N, N', N'-methylethylenediamine (alias: tetramethylethylenediamine) is mainly used as a biochemical reagent, epoxy resin crosslinking agent, and also an intermediate of quaternary ammonium compounds. [0003] The substance can be prepared by Eschweiler, W.-Clark, H.T synthesis method, which is also the most traditional method, that is, co-heating ethylenediamine with formaldehyde and excess formic acid can cause N-methylation reaction to generate N, N , N', N'-methylethylenediamine. [0004] h 2 NCH 2 NH 2 +4HCHO+4HCOOH→(H 3 c) 2 NCH 2 CH 2 N(CH 3 ) 2 +4CO 2 +4H 2 o [0005] Although the synthesis conditions of this method are relatively mild, the product that can be produced at normal temperature 1 is a mixture of monome...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/10C07C209/08B01J14/00
Inventor 陈国建南巍冈
Owner ZHEJIANG XINHUA CHEM