Synthetic method of epoxy propane hexafluoride

A synthetic method, the technology of hexafluoropropylene, applied in the direction of organic chemistry, can solve the problems of raw material waste, post-processing, poor selectivity, difficulties, etc., and achieve the effect of reducing explosions

Inactive Publication Date: 2007-05-02
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the deficiency that said method exists is that the productive rate of hexafluoropropylene oxide is low, and selectivity is poor, and by-product is many, and then causes the waste of raw material and the difficulty of aftertreatment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 300L of C to a 500L lined reactor with stirring and jacket 3 h 5 OCl, C 7 f 16 Mix the solvent (the ratio of the two is 1:2) and 80kg hexafluoropropylene, gradually heat up to 80°C, then slowly feed oxygen, the reaction starts and releases heat, the temperature rises gradually, and the reaction temperature is controlled at 100°C by cooling or heating Control the reaction pressure to be around 0.8Mpa. When the amount of oxygen introduced reaches 8.5kg, stop feeding and stir for 0.5h.

[0021] The mass ratio of hexafluoropropylene to oxygen is 9.4:1 relative to the addition amount of hexafluoropropylene diphenyl ether of 500 ppm. The mixed gas from the reactor was detected by gas chromatography, and the conversion rate of hexafluoropropylene was calculated to be 70%, and the selectivity of hexafluoropropylene oxide was 90%. After the mixed gas coming out of the reactor is separated, rectified, extracted and rectified, the high-purity hexafluoropropylene oxide with...

Embodiment 2

[0023] The operation is the same as in Example 1, except that no inhibitor is added. The mixed gas coming out of the reactor was detected by gas chromatography, and it was calculated that the conversion rate of hexafluoropropylene was 69%, and the selectivity of hexafluoropropylene oxide was 82%. After the mixed gas coming out of the reactor is separated, rectified, extracted and rectified, the high-purity hexafluoropropylene oxide with a purity of more than 99% is obtained.

Embodiment 3

[0025] Add 300L of C to a 500L lined reactor with stirring and jacket 2 f 5 OC 4 f 9 、C 7 f 16 (the ratio of the two is 1: 2) and 80kg hexafluoropropylene, the relative addition of hexafluoropropylene benzene is 500ppm, other steps and

[0026] Example 1 is the same.

[0027] The mixed gas coming out of the reactor was detected by gas chromatography, and it was calculated that the conversion rate of hexafluoropropylene was 80%, and the selectivity of hexafluoropropylene oxide was 93%. After the mixed gas coming out of the reactor is separated, rectified, extracted and rectified, the high-purity hexafluoropropylene oxide with a purity of more than 99% is obtained.

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Abstract

This invention relates to a composing preparation of sexi-fluorine epoxypropane, at the basis of oxygen oxidation method, improve selection of solvent, use two kinds of solvent to compose compound phase, raise contact concentration of raw material, it can add suppressive agent of aromatic compound into liquid phase medium to restrain producing by-product. Compound solvent consists of compound of ethers and alkanes compound, among them compound of ethers is selected from C3H5OCl, C2F5OC4F9, C5F10OC3F7 or C4H9OC3F7,alkanes compound is selected from CCl4, CF2Cl2, CF2HCl, C2F3Cl3 or C7F16.

Description

technical field [0001] The invention belongs to the field of preparation of fluorine-containing fine chemicals, and in particular relates to a method for preparing hexafluoropropylene oxide by liquid-phase oxidation of hexafluoropropylene. Background technique [0002] Hexafluoropropylene oxide (HFPO for short), also known as perfluoropropylene oxide, is the most important perfluorinated epoxy compound. The compound was first synthesized by DuPont in the late 1950s. HFPO can self-polymerize under anion triggering, or react with acyl fluoride to form perfluoroalkyl perfluorovinyl ether, and then copolymerize with tetrafluoroethylene or other fluoroolefins to prepare perfluorinated lubricants and perfluorinated lubricants with excellent performance. Heat-resistant medium, perfluorinated ion exchange resin, perfluoroplastic (PFA), perfluororubber and other organic fluorine materials. It can also react with many other substances to form compounds with tablet value. In additio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08
Inventor 张恒王汉利张永明高洪光
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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