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Preparation method of N,N-dimethyl benzylamine

A technology of dimethylbenzylamine and dimethylamine aqueous solution, applied in the N field, can solve the problems of generation of by-products, difficult separation and purification, large production energy consumption, etc., and achieves large wastewater treatment capacity, high yield and low pollution Effect

Active Publication Date: 2017-05-31
SHANGHAI WOKAI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this method is: monochloromethane is poisonous gas, and danger is big during production, and reaction has by-product to produce, and separation and purification are difficult, and yield is not high, and its chemical reaction formula is as follows:
[0005] At present, the methods for chemically preparing N.N-dimethylbenzylamine all have certain defects, the technology is backward, the production energy consumption is large, and the pollution is serious

Method used

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  • Preparation method of N,N-dimethyl benzylamine
  • Preparation method of N,N-dimethyl benzylamine

Examples

Experimental program
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Effect test

Embodiment 1

[0018]

[0019] (1) Get 1.7mol benzyl chloride to obtain solution A;

[0020] (2) Take 1mol dimethylamine and dissolve it in an appropriate amount of water to obtain a 30wt% aqueous solution of dimethylamine to obtain solution B. Since dimethylamine is a toxic gas, dissolving it in water can facilitate the reaction and prevent gas from escaping and causing pollution;

[0021] (3) After heating the glass reaction module of the Corning microchannel G1 glass reactor to 70°C, use two feed pumps to add solution A and solution B to the microchannel reactor at the same time to mix and react. The ratio of the feed rate of the pump to control the molar ratio of benzyl chloride and dimethylamine is 1:1.7;

[0022] (4) Since the volume in the glass reaction module of the reactor is a known fixed value, the total feed rate of the two feed pumps can be adjusted to control the reaction residence time to be 30 seconds;

[0023] (5) Collect the oil-water mixture that produces, cool immedi...

Embodiment 2

[0026] (1) Get 2.0mol benzyl chloride to obtain solution A;

[0027] (2) Dissolve 0.88mol dimethylamine in an appropriate amount of water to obtain a 20wt% dimethylamine aqueous solution to obtain solution B. Since dimethylamine is a toxic gas, dissolving it in water can facilitate the reaction and prevent gas from escaping and causing pollution;

[0028] (3) After heating the glass reaction module of the Corning microchannel G1 glass reactor to 90°C, use two feed pumps to add solution A and solution B to the microchannel reactor at the same time to mix and react. The ratio of pump feeding speed controls the feeding molar ratio of benzyl chloride and dimethylamine to be 1:2.2;

[0029] (4) Since the volume in the glass reaction module of the reactor is a known fixed value, the total feed rate of the two feed pumps can be adjusted to control the reaction residence time to be 40 seconds;

[0030] (5) Collect the oil-water mixture that produces, cool immediately, leave standstil...

Embodiment 3

[0033] (1) Get 1.0mol benzyl chloride to obtain solution A;

[0034] (2) Dissolve 0.4mol dimethylamine in an appropriate amount of water to obtain a 25wt% dimethylamine aqueous solution to obtain solution B. Since dimethylamine is a toxic gas, dissolving it in water can facilitate the reaction while preventing gas from escaping and causing pollution;

[0035] (3) After heating the glass reaction module of the Corning microchannel G1 glass reactor to 60°C, use two feed pumps to add solution A and solution B to the microchannel reactor at the same time to mix and react. The ratio of pump feeding speed controls the feeding molar ratio of benzyl chloride and dimethylamine to be 1:1.6;

[0036] (4) Since the volume in the glass reaction module of the reactor is a known fixed value, the total feed rate of the two feed pumps can be adjusted to control the reaction residence time to be 25 seconds;

[0037] (5) Collect the oil-water mixture that produces, cool immediately, leave stand...

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Abstract

The invention belongs to the technical field of chemical synthesis and particularly relates to a preparation method of N,N-dimethyl benzylamine. The preparation method comprises steps as follows: (1) benzyl chloride and 20wt%-40wt% of a dimethylamine water solution in the molar ratio being 1: (1.2-2.2) are introduced into a glass module of a microchannel reactor by a feed pump to be mixed for a heating reaction; (2) a collected oil and water mixture is cooled, left to stand and separated, and an upper oil layer is the reactant, namely, N,N-dimethyl benzylamine. The method is short in reaction time and safe in reaction control and conforms to the green chemistry concept.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a preparation method of N,N-dimethylbenzylamine. Background technique [0002] N,N-Dimethylbenzylamine can be used as a dehydrogenation catalyst, preservative, an intermediate in the synthesis of 18-methyl norethindrone, a triene hornosolone, a precursor of the D ring in the total synthesis of steroid compounds, and It can be used in the synthesis of quaternary ammonium salts, catalysts for the production of new clean and dehydrohalogenated products, corrosion inhibitors, acid neutralizers, accelerators for embedding electron microscope slices, etc. It is an important organic synthesis intermediate. [0003] The existing conventional methods for preparing N,N-dimethylbenzylamine mainly include: preparing N,N-dimethylbenzylamine by reacting benzylamine with methylene chloride. Chloromethane was passed into benzylamine and heated, and the product was separa...

Claims

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Application Information

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IPC IPC(8): C07C209/08C07C211/27
CPCC07C209/08C07C211/27
Inventor 王涛柯德宏薛循育周印
Owner SHANGHAI WOKAI BIOTECH
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