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Preparation method of octafluorocyclopentene

A technology of octafluorocyclopentene and chloroheptafluorocyclopentene, which is applied in the field of preparation of octafluorocyclopentene by fluorination, can solve the problems of difficult recycling of fluorinated reagent reaction solvents, environmental pollution, etc., and achieve novel routes , reduce pollution and achieve zero pollution effect

Active Publication Date: 2017-09-22
BEIJING YUJI SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above-mentioned prior art has the following defects: First, the three routes are all liquid-phase fluorination methods, which require the use of a large amount of solvents, and the excess fluorination reagents and reaction solvents are difficult to recycle, resulting in a large amount of waste liquid, which will cause serious pollution to the environment

Method used

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  • Preparation method of octafluorocyclopentene
  • Preparation method of octafluorocyclopentene
  • Preparation method of octafluorocyclopentene

Examples

Experimental program
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Embodiment 1

[0035] Preparation of fluorination catalyst: according to the mass percentages of chromium and magnesium as 90% and 10%, dissolve chromium chloride and magnesium chloride in water, add an appropriate amount of precipitant ammonia water at 60°C, and control the pH of the solution to 7.5- 8.5 range, make it fully precipitate under stirring conditions, filter the formed slurry, wash with deionized water until neutral, and then dry at 150°C for 12 hours to obtain the precursor of the catalyst. The precursor of the above catalyst was press-molded, and then calcined at 450°C for 10 hours under a nitrogen atmosphere, and then activated at 300°C for 10 hours with a mixed gas composed of hydrogen fluoride and hydrogen at a molar ratio of 10:1,

[0036] A fluorination catalyst is prepared.

[0037] A tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm was filled with 10 ml of the above-prepared fluorination catalyst. The reactor of the first ...

Embodiment 2

[0042] The same operation as in Example 1, except that 1,2-dichlorohexafluorocyclopentene was changed to an equivalent amount of 1,4-dichlorohexafluorocyclopentene, and the reaction temperature was changed to 290°C, the result See Table 2.

[0043] Table 2

[0044]

[0045] Note: F5-123 is 1,2,3-trichloropentafluorocyclopentene; F5-124 is 1,2,4-trichloropentafluorocyclopentene.

Embodiment 3

[0047] The same operation as in Example 1, except that 1,2-dichlorohexafluorocyclopentene was changed to an equivalent amount of 1,3-dichlorohexafluorocyclopentene, and the reaction temperature was changed to 290°C, the result See Table 3.

[0048] table 3

[0049]

[0050] Note: F5-123 is 1,2,3-trichloropentafluorocyclopentene; F5-124 is 1,2,4-trichloropentafluorocyclopentene.

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Abstract

The invention discloses a preparation method of octafluorocyclopentene, comprising the steps of a, in the presence of a fluorination catalyst, subjecting 1,4-dichlorohexafluorocyclopentene or / and 1,3-dichlorohexafluorocyclopentene or / and 1,2-dichlorohexafluorocyclopentene to gas catalytic fluorination with anhydrous hydrogen fluoride to obtain the intermediate 1-chloroheptafluorocyclopentene; b, in the presence of a fluorination catalyst, subjecting the 1-chloroheptafluorocyclopentene to gas catalytic fluorination with anhydrous hydrogen fluoride to obtain octafluorocyclopentene. The preparation method can produce octafluorocyclopentene with zero pollution; first-step reaction and second-step reaction are performed through a circulating system such that materials can react fully and can be utilized fully, pollution is relieved greatly, and zero-pollution production is achieved.

Description

technical field [0001] The present invention relates to a kind of preparation method of 1,2,3,3,4,4,5,5-octafluorocyclopentene, especially a kind of dichlorohexafluorocyclopentene and anhydrous hydrogen fluoride as raw materials, in Under the action of a fluorination catalyst, the first step of fluorination to obtain 1-chloro-2,3,3,4,4,5,5-heptafluorocyclopentene, and the second step of fluorination to obtain octafluorocyclopentene . Background technique [0002] Octafluorocyclopentene is a new type of environmentally friendly fluorine-containing compound, which does not destroy the atmospheric ozone layer (ODP value is 0), and has little effect on the greenhouse effect (GWP 100 =2), is considered to be the most promising new generation of semiconductor etching and cleaning gas, and can also be used as photochromic fluorescent probe compound molecular fragments for high-density holographic optical storage, in other fluorine-containing fine chemicals and high There are also...

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C23/08B01J23/26
CPCB01J23/26C07C17/20C07C2523/26C07C23/08
Inventor 刘冬鹏庆飞要张呈平张妮权恒道
Owner BEIJING YUJI SCI & TECH
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