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A kind of preparation method of perfluoro-2-methyl-2-pentene

A methyl, pentene technology, applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problem of low perfluoro-2-methyl-2-pentene content, strong catalyst water absorption, and catalyst Toxic problems, to achieve the effect of low cost, simple separation, high reaction efficiency

Active Publication Date: 2021-05-18
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method reported in the literature has the disadvantages of long reaction time and strong water absorption of the catalyst.
[0008] The method reported above has many disadvantages, such as the low content of perfluoro-2-methyl-2-pentene, or the catalyst is highly toxic, easy to absorb moisture, or has high requirements for equipment, etc.

Method used

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  • A kind of preparation method of perfluoro-2-methyl-2-pentene

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Experimental program
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Effect test

Embodiment 1

[0032] Add 1# catalyst (see Table 1 for composition) 12.0g, 20.0g of potassium carbonate and 66.7g of acetonitrile in 1L autoclave that internal cooling coil pipe is housed, N 2 Vacuumize the reaction kettle after 3 times, and pass 1000g of hexafluoropropylene gas at a constant speed at 50±2°C. After the gas is passed, the temperature is raised to 70°C. After 8 hours of reaction, the reaction is stopped, and the materials in the reaction kettle are released from the bottom of the reaction kettle. The product and the catalyst solvent system were immiscible, and 960 g of the lower layer reaction product was obtained by liquid separation operation, and the content of perfluoro-2-methyl-2-pentene in the product was analyzed by gas chromatography to be 99.6%.

Embodiment 2

[0034]Add 2# catalyst (see Table 1 for composition) 25.0g in 1L autoclave that internal cooling coil is housed, potassium carbonate 30.0g and acetonitrile 1000.0g, N 2 After replacing the reactor for 3 times, vacuumize, and pass 1000g of hexafluoropropylene gas at a constant speed at 50±2°C. After the gas is passed, the temperature is raised to 110°C. After 5 hours of reaction, the reaction is stopped, and the materials in the reactor are released from the bottom of the reactor. The product and the catalyst solvent system were immiscible, and 941 g of the lower layer reaction product was obtained by liquid separation operation, and the content of perfluoro-2-methyl-2-pentene in the product was analyzed by gas chromatography to be 99.4%.

Embodiment 3

[0036] Add 3# catalyst (see Table 1 for composition) 12.5g in 1L autoclave that internal cooling coil is housed, potassium carbonate 30.0g and acetonitrile 100.0g, N 2 Vacuumize the reaction kettle after 3 times, pass 1000g of hexafluoropropylene gas at a constant speed at 50±2°C, heat up to 80°C after the gas is passed through, stop the reaction after 7 hours of reaction, and release the materials in the reaction kettle from the bottom of the reaction kettle. The product and the catalyst solvent system were immiscible, and 908 g of the lower layer reaction product was obtained by liquid separation operation, and the content of perfluoro-2-methyl-2-pentene in the product was analyzed by gas chromatography to be 99.8%.

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Abstract

The invention discloses a preparation method of perfluoro-2-methyl-2-pentene. In the presence of a catalyst and an alkaline substance, hexafluoropropylene is reacted in a solvent to obtain perfluoro-2-methyl-2-pentene. 2-pentene, the mass ratio of the hexafluoropropylene to the catalyst is 20 to 100:1, the mass ratio of the hexafluoropropylene to the solvent is 1 to 15:1, and the mass ratio of the hexafluoropropylene to the basic substance is 10 to 100:1. 100:1, the reaction temperature is 40-150°C, and the reaction time is 3-12 hours. The invention has the advantages of environmental protection, low cost, simple process, high reaction selectivity and the like.

Description

technical field [0001] The invention relates to the technical field of perfluoroolefin compounds, in particular to a preparation method of perfluoro-2-methyl-2-pentene. Background technique [0002] Hexafluoropropylene dimer has two isomers, one is the kinetic isomer perfluoro-4-methyl-2-pentene, and the other is the thermodynamic isomer perfluoro-2-methyl- 2-pentene. Perfluoro-2-methyl-2-pentene (1,1,1,3,4,4,5,5,5-nonafluoro-2-(trifluoromethyl)pent-4-ene) is a perfluoroalkene compound , with a boiling point of 50.5°C, it is a colorless liquid at normal temperature and pressure. Perfluoro-2-methyl-2-pentene has two reactive sites, a fluorine atom directly connected to a carbon-carbon double bond and a carbon-carbon double bond, which makes perfluoro-2-methyl-2-pentene Alkenes are easily used as intermediates to synthesize surfactants, fabric treatment agents or paper treatment agents, etc.; because they do not contain chlorine, they will not damage the atmospheric ozone l...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C21/18C07C17/281
CPCC07C17/281C07C21/18
Inventor 姜澜陈振华王金明徐锋代现跃
Owner JUHUA GROUP TECH CENT
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