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Preparation method of D2 structure hexafluoropropylene dimer with high reaction activity

A technology of hexafluoropropylene dimer and high reactivity, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as difficult reactions, and achieve low cost The effect of low cost and simple preparation method

Inactive Publication Date: 2020-04-24
ZHEJIANG JUHUA HANZHENG NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The isomer content of the D1 structure in the currently prepared hexafluoropropylene dimer is more than 90%, and it is extremely difficult to react if this compound is used as the reaction raw material

Method used

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  • Preparation method of D2 structure hexafluoropropylene dimer with high reaction activity
  • Preparation method of D2 structure hexafluoropropylene dimer with high reaction activity
  • Preparation method of D2 structure hexafluoropropylene dimer with high reaction activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A highly reactive D2 structure hexafluoropropylene dimer is prepared according to the following method:

[0024] Add 0.01Kg of oligomerization catalyst, 0.01Kg of structural isomerization aid and 50Kg of organic solvent into the reaction kettle, stir and mix evenly, use argon to bubble for 5 minutes, then vacuumize, and cycle 3 times with argon, under vacuum condition Charge 15Kg of hexafluoropropylene at the bottom, control the temperature at 30°C, stir and react for 2 hours, after completing the reaction, cool down to 5°C, then discharge the residual hexafluoropropylene gas, separate the liquid to obtain the lower layer liquid, add it to the high-pressure reactor, and add 0.02Kg of metal Fluoride and 0.05Kg structural isomerization additive, heated to 60°C under nitrogen protection, reacted for 40 minutes, cooled to room temperature after the reaction was completed, and separated the catalyst to obtain the highly reactive D2 structure hexafluoropropylene dimerization ...

Embodiment 2

[0033] A highly reactive D2 structure hexafluoropropylene dimer is prepared according to the following method:

[0034] Add 0.08Kg of oligomerization catalyst, 0.05Kg of structural isomerization aid and 60Kg of organic solvent into the reaction kettle, stir and mix evenly, use argon to bubble for 8 minutes, then vacuumize, fill with argon for 3 times, under vacuum condition Charge 21Kg of hexafluoropropylene at the bottom, control the temperature at 35°C, stir and react for 5 hours, after completing the reaction, cool down to 8°C, then discharge the residual hexafluoropropylene gas, separate the liquid to obtain the lower layer liquid, add it to the autoclave, and add 0.06Kg of metal Fluoride and 0.25Kg structural isomerization additive, heated to 70°C under nitrogen protection, reacted for 50 minutes, cooled to room temperature after the reaction was completed, and separated the catalyst to obtain the highly reactive D2 structure hexafluoropropylene dimer body.

[0035] The ...

Embodiment 3

[0042] A highly reactive D2 structure hexafluoropropylene dimer is prepared according to the following method:

[0043] Add 0.15Kg of oligomerization catalyst, 0.1Kg of structural isomerization aid and 70Kg of organic solvent into the reaction kettle, stir and mix evenly, use argon to bubble for 10 minutes, then vacuumize, fill with argon for 3 times, and Charge 28Kg of hexafluoropropylene at the bottom, control the temperature at 45°C, stir and react for 8 hours, after completing the reaction, cool down to 10°C, then discharge the residual hexafluoropropylene gas, separate the liquid to obtain the lower layer liquid, add it to the high-pressure reactor, and add 0.12Kg of metal Fluoride and 0.5Kg structural isomerization aid, heated to 80°C under nitrogen protection, reacted for 60 minutes, cooled to room temperature after the reaction was completed, and separated the catalyst to obtain the highly reactive D2 structure hexafluoropropylene dimerization body.

[0044] The prepa...

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Abstract

The invention relates to the field of fine chemical engineering, in particular to a preparation method of a D2 structure hexafluoropropylene dimer with high reaction activity. The preparation method is simple, the preparation method comprises the following steps: firstly, preparing hexafluoropropylene into a hexafluoropropylene dimer of which the D2 content is greater than 70% under the action ofan oligomerization catalyst and a structural isomerization auxiliary agent; secondly, promoting the conversion of the hexafluoropropylene dimer of the D1 structure to the hexafluoropropylene dimer ofthe D2 structure by using metal fluoride and a structural isomerization additive through a heating and pressurizing reaction in the first step to prepare the high-reaction-activity D2 structure hexafluoropropylene dimer of which the content of the D2 structure hexafluoropropylene dimer is greater than 95%. The method is simple and feasible, is low in cost, and has a good industrial prospect.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a method for preparing a high-reactivity D2-structure hexafluoropropylene dimer. Background technique [0002] The synthesis and application of hexafluoropropylene dimer and its derivatives have been studied very early. As early as the 1960s and 1970s, there were patent reports on the synthesis of hexafluoropropylene dimer. Started the research on the synthesis and application of hexafluoropropylene dimer and its derivatives. [0003] 201811459916.8 discloses a method for preparing perfluoroisobutyryl fluoride from hexafluoropropylene trimer. The method comprises the steps of: taking oxygen and hexafluoropropylene dimer / hexafluoropropylene trimer as raw materials, and preparing it by reacting under the action of a catalyst; wherein oxygen and hexafluoropropylene dimer / hexafluoropropylene trimer The molar ratio is 1:10-10:1; the contact reaction time is 0.1s to 200s; the reaction p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/281C07C21/18B01J31/30
CPCB01J31/30C07C17/281C07C21/18
Inventor 王雄张则瑜段仲刚周强楼良弟
Owner ZHEJIANG JUHUA HANZHENG NEW MATERIAL
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