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A kind of preparation method of hexafluoropropylene oxide

A technology of hexafluoropropylene oxide and oxygen source, applied in the direction of organic chemistry, etc., can solve problems such as restricting technological development, generation of chlorine-containing wastewater, hidden dangers of explosion safety, etc., achieve good industrial prospects, high conversion rate, and reduce production costs Effect

Active Publication Date: 2019-04-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] According to the oxygen source used in the preparation process of hexafluoropropylene oxide, there are mainly molecular oxygen, hypochlorite, and aqueous hydrogen peroxide solution. Among them, the preparation process using molecular oxygen as the oxygen source has oxygen accumulation and potential explosion safety hazards; However, the preparation process using hypochlorite as the oxygen source has the problem of causing a large amount of chlorine-containing wastewater; using hydrogen peroxide as the oxygen source is a relatively economical and clean process route
In the preparation process using hydrogen peroxide as the oxygen source, it was found that the requirements for the reaction catalyst system were strict, and there were problems such as low conversion rate, which restricted the further technological development of this process route.

Method used

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  • A kind of preparation method of hexafluoropropylene oxide
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  • A kind of preparation method of hexafluoropropylene oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Use Mn(OTf)2 and chiral tetradentate ligands to generate catalysts in situ with a molar ratio of 1:1, and slowly pump the catalysts into the reactor (see attached figure 1 , Note, different embodiments use reaction devices with different apertures), and make it evenly attached to the inner wall of the reactor.

[0038] After mixing and pumping acetonitrile (50g) and hydrogen peroxide (50wt% 1.2mol) into one end of the tube reactor (wherein containing catalyst 0.01mol), the auxiliary agent (0.1mol) is pumped in; the other end is slowly pumped into hexafluoropropylene (1mol), the whole system is protected by nitrogen, and the reaction pressure is 0.03Mpa. Reaction at room temperature for 1.5h. After the reaction, use methyl chloride extractive distillation to obtain the product yield as shown in the table below.

[0039] In the embodiment, the chiral tetradentate organic ligand is a chiral tetradentate nitrogen organic ligand, specifically the following structural formu...

Embodiment 2

[0045] The experimental method is as in Example 1, and the auxiliary agent used is sodium carbonate, and the solvent addition is 50 g. The experimental results are shown in the table below.

[0046] Table 2. Solvent investigation

[0047] serial number

[0048] Conclusion: Better results were obtained when using acetonitrile or a mixture of acetonitrile and isopropanol.

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Abstract

The invention provides a method for preparing hexafluoropropylene oxide. Specifically, in a mixed solvent, the substrate is hexafluoropropylene, and a complex compound formed in situ of a chiral tetradentate organic ligand and a metal manganese compound is used as a catalyst. The aqueous solution of hydrogen peroxide is used as the oxygen source, and the target product—hexafluoropropylene oxide can be generated efficiently and selectively in a specific reactor with additives or no additives. The process route used in the invention is green and environment-friendly, and has high industrial application prospect.

Description

technical field [0001] The invention belongs to the field of synthesis of fine chemicals, and in particular relates to a preparation method of hexafluoropropylene oxide. Background technique [0002] Hexafluoropropylene oxide (HFPO for short) is an important fluorine-containing fine chemical and an organic intermediate for the production of important fluorine chemicals such as perfluoropolyether, perfluoroacetone, perfluoropropionyl chloride, and fluorine-containing surfactants. body. HFPO has high chemical activity and can react with various nucleophilic reagents to produce various perfluorovinyl ethers. The latter is usually used as a comonomer for melting fluororesins, fluororubbers and functional group-containing production of fluoropolymers. Because HFPO has changed the properties of fluororesins that are difficult to process, such as polytetrafluoroethylene, its market demand has been rapidly developed. HFPO can synthesize PPVE, perfluoromethyl vinyl ether PMVE and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D301/12C07D303/48
CPCC07D301/12C07D303/48
Inventor 高爽吕迎张毅张恒耘
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI