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Method for simultaneously preparing dichlorohexafluorocyclopentene isomers

A technology for dichlorohexafluorocyclopentene and trichloropentafluorocyclopentene is applied in the field of simultaneous preparation of dichlorohexafluorocyclopentene isomers, and can solve problems such as being difficult to exist stably, unattractively, and difficult to find, etc. problem, to achieve the effect of stable activity and easy availability of raw materials

Active Publication Date: 2020-02-18
BEIJING YUJI SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above-mentioned known technical routes for synthesizing 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene do not possess the attractiveness of industrialization, which is attributed to the following defects: First, in the synthesis of 1 , In the technical route of 2-dichlorohexafluorocyclopentene, the yields of 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene are both zero, which is attributed to 1 The compound energy of 3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene is much larger than that of 1,2-dichlorohexafluorocyclopentene, so that in the high temperature reaction system It is difficult to exist stably in the medium; secondly, the method for synthesizing 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene by liquid phase has improved aspects of strong corrosion reduction and waste reduction. room
Because 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene are difficult to exist stably at high temperature; in addition, C(sp 2 )-Cl gas-phase fluorine-chlorine exchange reaction performance is often better than C(sp 3 )-Cl is much more difficult, so that it is difficult to find suitable raw materials to prepare 2 )-F and C(sp 3 )-Cl haloalkane
Up to now, about the use of gas-phase fluorine-chlorine exchange reaction to simultaneously prepare 1,4-dichlorohexafluorocyclopentene, 1,3-dichlorohexafluorocyclopentene and 1,2-dichlorohexafluorocyclopentene The technical route has not yet been publicly reported

Method used

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  • Method for simultaneously preparing dichlorohexafluorocyclopentene isomers
  • Method for simultaneously preparing dichlorohexafluorocyclopentene isomers

Examples

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Embodiment 1

[0030] Preparation of fluorination catalyst: Dissolve chromium nitrate in water, add precipitant ammonia water at 60°C, control the pH of the solution between 7.5 and 8.5, make it fully precipitate under stirring conditions, filter the formed slurry, and use Wash with ion water until neutral, then dry at 150°C for 12 hours to obtain chromium hydroxide. The above-mentioned chromium hydroxide and cobalt hydroxide are uniformly mixed according to the mass percentage of 95% and 5%, and press-molded to obtain a catalyst precursor, and then the catalyst precursor is roasted at 450 ° C for 10 hours under a nitrogen atmosphere. Activate at 300°C for 10 hours with a mixed gas consisting of hydrogen fluoride and hydrogen at a molar ratio of 10:1 to prepare a fluorination catalyst.

[0031] 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 temperature of the reactor is ra...

Embodiment 2

[0033] The same operation as in Example 1, except that the reaction temperature was changed to 130° C., the results are shown in Table 1.

Embodiment 3

[0035] The same operation as in Example 1, except that the reaction temperature was changed to 180°C, the results are shown in Table 1.

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Abstract

The invention relates to a method for simultaneously preparing dichlorohexafluorocyclopentene isomers. The method comprises the following steps: taking hydrogen fluoride and trichloropentafluorocyclopentene as reaction raw materials; carrying out gas-phase catalysis fluorine-chlorine exchange reaction in the presence of a fluorination catalyst to obtain the dichlorohexafluorocyclopentene isomers. By adopting the method provided by the invention, 1,2-dichlorohexafluorocyclopentene, 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene can be coproduced, wherein the single-pass yield of the 1,3-dichlorohexafluorocyclopentene and the 1,4-dichlorohexafluorocyclopentene is relatively high and the sum of the yield of the 1,3-dichlorohexafluorocyclopentene and the 1,4-dichlorohexafluorocyclopentene is greater than 57 percent; the raw materials are easy to obtain and the fluorination catalyst has stable activity, so that the method is suitable for simultaneously and continuously preparing the 1,2-dichlorohexafluorocyclopentene, the 1,3-dichlorohexafluorocyclopentene and the 1,4-dichlorohexafluorocyclopentene in a large scale in a gas phase.

Description

technical field [0001] The present invention relates to a method for simultaneously preparing 1,2-dichlorohexafluorocyclopentene, 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene, in particular to a process by The isomers of trichloropentafluorocyclopentene and hydrogen fluoride undergo a gas-phase fluorine-chlorine exchange reaction in the presence of a fluorination catalyst to simultaneously prepare 1,2-dichlorohexafluorocyclopentene, 1,3-dichloro Methods for hexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene. Background technique [0002] 1,2-dichlorohexafluorocyclopentene, 1,3-dichlorohexafluorocyclopentene and 1,4-dichlorohexafluorocyclopentene are very important intermediates that can be used to synthesize octafluorocyclopentene Alkenes, 1,2,2,3,3,4,4,5-heptafluorocyclopentane and other five-membered ring fluorides. Five-membered ring fluorides are mainly used to replace ozone-depleting substances used in the semiconductor electron...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/20C07C23/08
CPCC07C17/206C07C23/08
Inventor 张呈平张妮庆飞要权恒道
Owner BEIJING YUJI SCI & TECH
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