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Preparation method of 2,2,2-trifluoroethylamine

A technology of trifluoroethylamine and ethyl chloride, which is applied in two fields, can solve the problems of low yield and long reaction time, and achieve the effect of high product yield and short reaction time

Active Publication Date: 2013-11-06
XIAN MODERN CHEM RES INST
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The method has the problems of low yield and long reaction time

Method used

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Examples

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Effect test

preparation example Construction

[0016] A preferred 2,2, the preparation method of 2-trifluoroethylamine, comprises the following steps:

[0017] 1) Mix the liquid phase 1,1,1-trifluoro-2-chloroethane dissolved in glycerol with ammonia water, wherein the mixture of glycerol and 1,1,1-trifluoro-2-chloroethane The volume ratio is 2:1, the molar ratio of ammonia to 1,1,1-trifluoro-2-chloroethane is 12:1, the concentration of ammonia water is 60%wt, and then enters the pipeline reactor for reaction, and the reactants are in The flow rate in the pipeline reactor was 3.5L / h; the reaction temperature was 180°C, the pressure was 2.5MPa, and the time was 22min to obtain a mixed solution containing 2,2,2-trifluoroethylamine;

[0018] 2) The mixed solution containing 2,2,2-trifluoroethylamine is deaminated by flash evaporation under reduced pressure, and then the deammonized liquid is neutralized by adding sodium carbonate, in which sodium carbonate is mixed with 1,1,1-trifluoroethylamine The molar ratio of fluoro-2-ch...

Embodiment 1

[0024] 1) Mix the liquid phase 1,1,1-trifluoro-2-chloroethane dissolved in glycerol with ammonia water, the volume ratio of glycerol to 1,1,1-trifluoro-2-chloroethane 2:1, the molar ratio of ammonia to 1,1,1-trifluoro-2-chloroethane is 12:1, the concentration of ammonia water is 60%wt, and then enters the pipeline reactor for reaction, and the reactant is in the pipeline The flow rate in the reactor is 3.5L / h; the reaction temperature is 180°C, the pressure is 2MPa-4MPa, and the time is 22min, to obtain a mixed solution containing 2,2,2-trifluoroethylamine;

[0025] 2) The mixed solution containing 2,2,2-trifluoroethylamine is deaminated by flash evaporation under reduced pressure, and then the deammonized liquid is neutralized by adding sodium carbonate, in which sodium carbonate is mixed with 1,1,1-trifluoroethylamine The molar ratio of fluoro-2-chloroethane is 0.8:1, and the neutralized solution is rectified under reduced pressure to obtain 2,2,2-trifluoroethylamine.

[00...

Embodiment 2

[0028] 1) Mix the liquid phase 1,1,1-trifluoro-2-chloroethane dissolved in glycerol with ammonia water, the volume ratio of glycerol to 1,1,1-trifluoro-2-chloroethane 1:1, the molar ratio of ammonia to 1,1,1-trifluoro-2-chloroethane is 8:1, the concentration of ammonia water is 50%wt, and then enters the pipeline reactor to react, and the reactant is in the pipeline The flow rate in the reactor is 2.0L / h, the reaction temperature is 150°C, the pressure is 4.0MPa, and the time is 30min to obtain a mixed solution containing 2,2,2-trifluoroethylamine;

[0029] 2) The mixed solution containing 2,2,2-trifluoroethylamine is deaminated by flash evaporation under reduced pressure, and then the deammonized liquid is neutralized by adding sodium carbonate, in which sodium carbonate is mixed with 1,1,1-trifluoroethylamine The molar ratio of fluoro-2-chloroethane is 0.5:1, and the neutralized solution is rectified under reduced pressure to obtain 2,2,2-trifluoroethylamine.

[0030] After...

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PUM

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Abstract

The invention discloses a preparation method of 2,2,2-trifluoroethylamine, which comprises the following steps of: (1) mixing liquid-phase 1,1,1-trifluoro-2-chloroethane dissolved into glycerin with ammonia, wherein the volume ratio of glycerin to 1,1,1-trifluoro-2-chloroethane is 1-3:1, the molar ratio of ammonia to 1,1,1-trifluoro-2-chloroethane is 8-15:1, and the concentration of ammonia ranges from 30wt% to 100wt%; reacting in a pipeline-type reactor for 20min to 30min at 150 DEG C and 200 DEG C under the pressure of 2MPa and 4MPA so as to obtain a mixed solution containing 2,2,2-trifluoroethylamine, wherein the flowing velocity of the reactant in the pipeline-type reactor is 2.0-4.0L / h; and (2) carrying out pressure reduction, flashing and deamination on the mixed solution of 2,2,2-trifluoroethylamine, and adding the liquid subjected to deamination into sodium carbonate for neutralizing , wherein the molar ratio of sodium carbonate to 1,1,1-trifluoro-2-chloroethane is 0.5-2:1; carrying out pressure reduction and rectification on the neutralized solution to obtain 2,2,2-trifluoroethylamine. The method has the advantages of short reaction time and high product yield.

Description

technical field [0001] The invention belongs to the preparation in the field of organic chemical industry, in particular to a preparation method of 2,2,2-trifluoroethylamine. Background technique [0002] 2,2,2-Trifluoroethylamine is an important pesticide intermediate, which can be used to synthesize highly active insecticides, acaricides, ovicides, and synthetic herbicides. In the field of medicine, 2,2,2-trifluoroethylamine can be used as a pharmaceutical intermediate to prepare 1,2-substituted biguanide and its derivatives for treating diabetes. [0003] US4618718 discloses a kind of preparation method of trifluoroethylamine. The method uses 1,1,1-trifluoro-2-chloroethane to react with ammonia, in the presence of solvent N-methylpyrrolidone, under the condition of pressure 7-11Mpa, 200-220°C for 24h, 1,1, The conversion rate of 1-trifluoro-2-chloroethane was 98.7%, and the yield of 2,2,2-trifluoroethylamine was 86.8%. This method has the problems of low yield and long...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/15C07C209/08C07C209/86
Inventor 吕剑杨建明郝志军庞国川杨志强余秦伟
Owner XIAN MODERN CHEM RES INST
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