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Method for synthesizing 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination

A technology of trifluoromethyl and methyl propionitrile is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc. Environmental pollution and other problems, to achieve the effect of short synthesis route and high single-pass yield

Pending Publication Date: 2022-02-25
CHEM & CHEM ENG GUANGDONG LAB +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above route has the following defects: (1) the route is lengthy; (2) batch method, the synthesis efficiency is low; (3) a large amount of solvents are used, which are difficult to recycle and utilize, and will produce a large amount of liquid waste, which will seriously pollute the environment; (4) The total yield of 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propionitrile is low, only 50.8%

Method used

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  • Method for synthesizing 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination
  • Method for synthesizing 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination
  • Method for synthesizing 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination

Examples

Experimental program
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Effect test

Embodiment 1

[0061] Preparation of fluorine-halogen exchange catalyst: according to the mass percentage content of chromium ions (trivalent or / and tetravalent or / and pentavalent chromium ions) and cobalt elements are 90% and 10%, chromium chloride and chlorinated Cobalt is dissolved in water, and the precipitant ammonia water is added at 60°C, and the pH of the solution is controlled between 7 and 9, so that it is fully precipitated under stirring conditions, and then aged for 10-24 hours, the formed slurry is filtered, and deionized water is used. Wash to neutrality, then dry at 150°C for 10-24 hours to obtain a solid, pulverize the above-mentioned solid, press and shape to obtain a catalyst precursor, and then calcinate the catalyst precursor at 450°C for 10-24 hours under a nitrogen atmosphere. Activation at 300°C with a mixture of hydrogen fluoride and nitrogen with a molar ratio of 1:2 for 10-24 hours, and oxidation at 300°C with a mixture of chlorine trifluoride and nitrogen with a mo...

Embodiment 2

[0064] The same operation as in Example 1, the difference is that "according to the mass percentage content of chromium ions (trivalent or / and tetravalent or / and pentavalent chromium ions) and cobalt elements are 90% and 10%, the chlorine Chromium chloride and cobalt chloride are dissolved in water” to “dissolve chromium chloride and magnesium chloride in water according to the mass percentage of chromium ions and magnesium elements of 90% and 10%”. The reaction results are as follows: the conversion of isobutyronitrile is 100%, the selectivity of 2-chloro-3,3,3-trifluoro-2-(trifluoromethyl)propionitrile is 59.5%, the selectivity of 2-chloro-3, 22.0% selectivity for 3,3-trifluoro-2-(monochlorodifluoromethyl)propionitrile, 2-chloro-3,3,3-trifluoro-2-(trichloromethyl)propionitrile The selectivity was 12.1% and the selectivity for 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propionitrile was 6.4%.

Embodiment 3

[0066] The same operation as in Example 1, the difference is that "according to the mass percentage content of chromium ions (trivalent or / and tetravalent or / and pentavalent chromium ions) and cobalt elements are 90% and 10%, the chlorine Chromium and cobalt chloride are dissolved in water" to "according to the mass percentage content of chromium ions (trivalent or / and tetravalent or / and pentavalent chromium ions) and zinc elements are 90% and 10%, the chlorine Chromium and zinc chloride dissolve in water". The reaction results are as follows: the conversion of isobutyronitrile is 100%, the selectivity of 2-chloro-3,3,3-trifluoro-2-(trifluoromethyl)propionitrile is 62.1%, the selectivity of 2-chloro-3, The selectivity of 3,3-trifluoro-2-(monochlorodifluoromethyl)propionitrile was 28.7%, and the selectivity of 2-chloro-3,3,3-trifluoro-2-(trichloromethyl)propionitrile The selectivity was 8.7% and the selectivity for 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propionitrile was 0.5%....

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Abstract

The invention discloses a method for preparing 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination. In the presence of a fluorine-halogen exchange catalyst, 2-R1-3, 3, 3-trifluoro-2-(trifluoromethyl) propionitrile (R1 is H, Cl, Br or I) is used as a raw material and is subjected to gas-phase catalytic fluorination reaction with hydrogen fluoride and halogen simple substances to obtain 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile, and the raw material 2-R1-3, 3, 3- trifluoro-2-(trifluoromethyl)propionitrile can be synthesized through a series of gas phase reactions by taking octafluoroisobutylene or saturated or unsaturated nitrile as an initial raw material. The method is mainly used for preparing the 2, 3, 3, 3-tetrafluoro-2-(trifluoromethyl)propionitrile in a gas phase manner. The preparation method has the advantages of short route, high single-pass yield, high catalyst activity and no generation of liquid waste.

Description

technical field [0001] The invention relates to a method for synthesizing 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propionitrile by gas-phase catalytic fluorination, in particular to a method of using 2-R 1 -3,3,3-Trifluoro-2-(trifluoromethyl)propionitrile (R 1 A method for obtaining 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propionitrile through gas-phase catalytic fluorination reaction with hydrogen fluoride and halogen element using H, Cl, Br or I) as raw materials, and simultaneously providing raw material 2-R 1 - A method for the synthesis of 3,3,3-trifluoro-2-(trifluoromethyl)propionitrile. Background technique [0002] Chinese patent CN111825569A reported the synthesis of 2,3,3,3-tetrafluoro-2 using hexafluoropropylene as the starting material through a four-step reaction of liquid-phase oligomerization, liquid-phase esterification, liquid-phase amination and liquid-phase dehydration. -(trifluoromethyl) propionitrile, specifically as follows: (1) liquid phase oligomeriz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/26C07C255/10B01J23/86
CPCC07C253/26B01J23/864C07C255/10
Inventor 张呈平董利唐泽华权恒道
Owner CHEM & CHEM ENG GUANGDONG LAB
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