Preparation method of D2 structure hexafluoropropylene dimer

A technology of hexafluoropropylene dimer and hexafluoropropylene, which is applied in the field of chemical technology, can solve the problems of high degree of dissociation and easy aggregation of fluoride anions, and achieve the effect of improving overall performance, reducing the degree of dissociation, and realizing dispersion

Pending Publication Date: 2022-01-14
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%, while the preparation method of the D2 structure hexafluoropropylene dimer is less, and the fluorine anion has a large degree of dissociation, which is easy to aggregate and does not participate in Isomerization reaction, so the catalytic system of isomerization needs to be further improved

Method used

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  • Preparation method of D2 structure hexafluoropropylene dimer
  • Preparation method of D2 structure hexafluoropropylene dimer
  • Preparation method of D2 structure hexafluoropropylene dimer

Examples

Experimental program
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Effect test

preparation Embodiment 1

[0043] (1) Add 5g of 3-mercaptopicolinic acid, 3g of vinyl borate pinacol ester, 150g of acetonitrile, add 2g of sodium ethoxide into a closed autoclave, heat up and stir to 50°C, pressure is 0.8MPa, and react for 100min to obtain Auxiliary A;

[0044] (2) Then directly mix the auxiliary agent A with 25 g of potassium fluoride for 10 hours, the molar ratio of the auxiliary agent A to potassium fluoride is 1:1, and distill off the acetonitrile under reduced pressure to obtain the isomerization catalyst 1.

preparation Embodiment 2

[0046] (1) Add 12g of 3-mercaptopicolinic acid, 6g of vinylboronic acid pinacol ester, 220g of acetonitrile into a closed high-pressure reactor, add 6g of sodium ethoxide, heat up and stir to 65°C, pressure is 2.0MPa, and react for 150min to obtain Auxiliary A;

[0047] (2) Then directly mix Auxiliary A with 36 g of potassium fluoride for 20 hours, the molar ratio of A and potassium fluoride is 1:1.5, and distill off acetonitrile under reduced pressure to obtain isomerization catalyst 2.

Embodiment 1

[0049] (1) Oligomerization reaction

[0050] Cesium fluoride was calcined at 400°C for 10 hours, ground into powder and added to the autoclave together with anhydrous acetonitrile, stirred and mixed evenly, then bubbled with argon for 5 minutes, then vacuumed, and argon was circulated for 3 times. Fill 20g of hexafluoropropylene under the conditions, control the temperature at 30°C, pressure at 0.8MPa, stir the reaction for 2 hours, and the stirring speed at 50r / min, cool down to 10°C after the reaction is completed, and then discharge the residual hexafluoropropylene gas, Liquid obtains lower floor liquid; Join in the autoclave;

[0051] (2) Isomerization reaction

[0052] Add 0.5g of isomerization catalyst 1 into the autoclave, raise the temperature to 100°C under the protection of nitrogen, and react for 60 minutes. After the reaction is completed, cool to room temperature and separate the catalyst to obtain the highly reactive D2 structure hexafluoro Propylene dimer.

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Abstract

The invention relates to the technical field of chemical processes, in particular to a preparation method of a D2 structure hexafluoropropylene dimer. According to the preparation method of the D2 structure hexafluoropropylene dimer, 5-bromine-6-sulfydryl pyridine and vinyl trifluoroborate are subjected to a sulfydryl-alkene reaction, the prepared auxiliary is added into metal fluoride, the valence state of metal can be stabilized, the catalytic activity can be improved, and high dispersion of active components in a fluorine-containing catalyst is achieved.

Description

technical field [0001] The invention relates to the technical field of chemical technology, in particular to a preparation method of a D2 structure hexafluoropropylene dimer. Background technique [0002] Because the fluorine atoms replace the hydrogen atoms in the molecule, the hexafluoropropylene dimer has good thermal and chemical stability; and because it contains double bonds, it can be further reacted to prepare various fluorine-containing derivatives. These derivatives It can be used as pharmaceuticals, pesticide intermediates, fluorine-containing surfactants, water and oil repellent additives, fluorine-containing polymer monomers, solvents, and inert liquids. Therefore, it is of great practical significance to study the development and utilization of hexafluoropropylene dimer and its derivatives. [0003] The applicant's previous application, CN201911361617.5, relates to the field of fine chemicals, and specifically relates to a method for preparing a high-reactivit...

Claims

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Application Information

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IPC IPC(8): C07C17/358C07C21/18C07C17/281
CPCC07C17/358C07C17/281C07C21/18
Inventor 张军良周强岳亚伟段仲刚刘明生林久明
Owner ZHEJIANG JUHUA HANZHENG NEW MATERIAL
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