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Method for preparing heptafluoroisobutyronitrile through gas-phase fluorocyaniding

A technology of heptafluoroisobutyronitrile and gas phase, which is applied in chemical instruments and methods, cyanogen halide reaction preparation, organic chemistry, etc., can solve the problems of polluting the environment, difficulty in recycling and low yield of heptafluoroisobutyronitrile, etc. To achieve the effect of reducing pollution

Pending Publication Date: 2021-11-23
CHEM & CHEM ENG GUANGDONG LAB +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above-mentioned route has the following defects: (1) a large amount of solvents and fluorinated reagents are used, which are difficult to recycle and utilize, and will produce a large amount of liquid waste and solid waste, which will seriously pollute the environment; (2) adopt Batch process, and the yield of heptafluoroisobutyronitrile is low

Method used

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  • Method for preparing heptafluoroisobutyronitrile through gas-phase fluorocyaniding
  • Method for preparing heptafluoroisobutyronitrile through gas-phase fluorocyaniding
  • Method for preparing heptafluoroisobutyronitrile through gas-phase fluorocyaniding

Examples

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Effect test

Embodiment 1

[0060] Preparation of fluorination catalyst: according to the mass percent content of chromium ion (trivalent or / and tetravalent or / and pentavalent chromium ion) and cobalt element is 90% and 10%, chromium chloride and cobalt chloride are dissolved In water, add precipitant ammonia water at 60°C, control the pH of the solution between 7 and 9, make it fully precipitate under stirring conditions, then age for 10-24 hours, filter the formed slurry, and wash with deionized water until Neutral, then dry at 150°C for 10-24 hours to obtain a solid, crush the above-mentioned solid, press and shape to obtain a catalyst precursor, and then roast the catalyst precursor at 450°C for 10-24 hours in a nitrogen atmosphere, Activate with a mixed gas of hydrogen fluoride and nitrogen with a molar ratio of 1:2 for 10-24 hours, and oxidize for 10-24 hours at 300°C with a mixed gas atmosphere of nitrogen dioxide and nitrogen with a molar ratio of 1:10. Partially or completely converting trivalen...

Embodiment 2

[0063] The same operation as in Example 1, the difference is that "according to the mass percentages of chromium ions (trivalent or / and tetravalent or / and pentavalent chromium ions) and cobalt elements are 90% and 10%, the chlorine Dissolve chromium chloride and cobalt chloride in water" to "dissolve chromium chloride and magnesium chloride in water according to the mass percentages of chromium ions and magnesium elements being 90% and 10%. The reaction results are as follows: the conversion rate of hexafluoropropylene is 97.3%, and the selectivity of heptafluoroisobutyronitrile is 95.6%.

Embodiment 3

[0065] The same operation as in Example 1, the difference is that "according to the mass percentages 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 " be 90% and 10% according to the mass percent content of chromium ion (trivalent or / and tetravalent or / and pentavalent chromium ion) and iron element, chlorine Chromium chloride and ferric chloride dissolved in water". The reaction results are as follows: the conversion rate of hexafluoropropylene is 98.7%, and the selectivity of heptafluoroisobutyronitrile is 97.4%.

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Abstract

The invention relates to a method for preparing heptafluoroisobutyronitrile through gas-phase fluorocyaniding, and belongs to the field of chemical synthesis. Hexafluoropropylene is used as a raw material, in the presence of a fluorination catalyst, hexafluoropropylene, hydrogen fluoride and X-CN are subjected to a gas phase catalytic reaction to obtain heptafluoroisobutyronitrile, unreacted hexafluoropropylene, hydrogen fluoride and X-CN in a product flow are circulated to a reactor filled with the fluorination catalyst for continuous reaction, and when X-CN is F-CN, the raw material HF can be zero. The method has the characteristics of easily available initial raw materials, high activity of the fluorination catalyst and long service life, and only the main product heptafluoroisobutyronitrile and the possible byproduct HX are extracted from the whole system by adopting a continuous cycle process technology, so that the zero emission standard is achieved.

Description

technical field [0001] The invention relates to a method for preparing heptafluoroisobutyronitrile by gas-phase cyanidation. In particular, it relates to using hexafluoropropylene as a raw material, in the presence of a fluorination catalyst, and hydrogen fluoride and a pseudohalogen X-CN (X=F, Cl, Br, I or -CN) to undergo a gas-phase catalytic cyanidation reaction to prepare heptafluoroiso At the same time, the heptafluoroisobutyronitrile generated by continuous extraction is adopted by a recycling process, and the unreacted hexafluoropropylene, HF, and X-CN continue to circulate in the system until it is converted into heptafluoroisobutyronitrile from the system. Mining, wherein when X-CN is F-CN, the raw material HF can be zero. Background technique [0002] Among the many synthetic routes of heptafluoroisobutyronitrile, the liquid-phase fluorination of hexafluoropropylene with ethanedinitrile or cyanogen chloride in the presence of alkali metal fluoride salts is an impo...

Claims

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Application Information

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IPC IPC(8): C07C253/04C07C253/34C07C255/10B01J27/132B01J27/138
CPCC07C253/04C07C253/34B01J27/132B01J27/138C07C255/10
Inventor 张呈平庆飞要郭勤权恒道
Owner CHEM & CHEM ENG GUANGDONG LAB
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