Method for comprehensively utilizing byproducts produced in HFPO (hexafluoropropylene oxide) preparation based on oxygen oxidation method

A technology of oxygen oxidation and by-products, applied in chemical instruments and methods, acid halide preparation, acid halide preparation and other directions, can solve the problem of by-product utilization, etc., and achieve the effect of less equipment investment and strong operability

Pending Publication Date: 2019-04-26
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN201310520468.9 discloses a method for preparing hexafluoropropylene oxide by oxygen oxidation using perfluoropolyether as the backbone and acyl fluoride as the terminal solvent, but the by-products have not been effectively utilized; The product is usually disposed of by incineration

Method used

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Examples

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Effect test

Embodiment 1

[0019] Example 1: Preparation of hexafluoropropylene oxide by oxidation method with oxygen as oxidant, FC-75 as solvent, and after being recycled for 20 hours after participating in the reaction, the peroxide value measured by standard starch potassium iodide method was 3800ppm, the by-product CF 3 O(CF 2 O) n (CF(CF 3 )CF 2 O) m COF and CF 3 O(CF 2 O) n (CF(CF 3 )CF 2 O) m The content of OCOF is less than 40wt%. Irradiate with 200nm ultraviolet light for 10 seconds at room temperature (in this application, the ultraviolet light irradiation wavelength can be 100nm-400nm; the irradiation time is 5-20s, and the reaction temperature is room temperature-150℃. As long as the peroxide value is less than 5ppm) . After every 20 hours of recycling, 200nm ultraviolet light is irradiated for 10 seconds. As the cycle time increases, the amount of by-products in the solvent continues to increase. The gas mixture of carbonyl fluoride and other by-products was collected improperly during the ...

Embodiment 2

[0020] Example 2: Preparation of hexafluoropropylene oxide by oxidation method using air as oxidant, using CFC-113 as solvent, recycling for 30 hours after participating in the reaction, and using standard starch potassium iodide method to measure the peroxide value of 4200 ppm. By-product CF 3 O(CF 2 O) n (CF(CF 3 )CF 2 O) m COF and CF 3 O(CF 2 O) n (CF(CF 3 ) CF 2 O) m The content of OCOF is less than 40wt%. Irradiate with 380nm ultraviolet light for 10 seconds at room temperature. After every 30 hours of recycling, 380nm ultraviolet light is irradiated for 10 seconds. As the cycle time increases, the amount of by-products in the solvent continues to increase. In the process of ultraviolet irradiation, a mixture of carbonyl fluoride and other by-products after decomposition was collected, and the content of carbonyl fluoride was 94%. After further rectification treatment, carbonyl fluoride products with higher purity can be obtained. After 600 hours of circulation, the cont...

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Abstract

The invention belongs to the field of fluorine chemical and particularly relates to a method for comprehensively utilizing byproducts produced in HFPO (hexafluoropropylene oxide) preparation based onan oxygen oxidation method. The method comprises following steps: 1), oxygen and hexafluoropropylene are taken as raw materials, and HFPO is prepared under the action of a fluoride solvent, and the fluoride solvent is recycled; 2), when content of the byproducts in the recycled fluoride solvent is lower than 40wt%, ultraviolet irradiation is performed every 10-30 h; 3), when content of the byproducts is higher than or equal to 40wt%, water is added to the fluoride solvent, and a carboxylic acid product is obtained. On one hand, an important chemical intermediate carbonyl fluoride in the fluorine chemical can be obtained, on the other hand, the byproducts can be converted into a perfluoro surfactant or fluorine-containing fluid for further application, and therefore, the byproducts producedin the HFPO preparation process based on the oxygen oxidation method are comprehensively utilized.

Description

Technical field [0001] The invention belongs to the field of fluorine chemicals, and specifically relates to a method for preparing by-products generated in HFPO by comprehensively utilizing an oxygen oxidation method. Background technique [0002] Oxygen oxidation method to prepare hexafluoropropylene oxide is the most common process in which oxygen or air is used as an oxidant to oxidize hexafluoropropylene in a fluorinated solvent to prepare hexafluoropropylene oxide. [0003] The process of preparing hexafluoropropylene oxide by the oxygen oxidation method is divided into two methods: batch method and continuous method. The fluorine-containing solvent in the two methods is often recycled. In addition, the reaction is an oxidation reaction. The intermediates produced during the reaction are unstable and will continue to react with oxygen and hexafluoropropylene to form byproducts. Among them, the chemical structure of CF3O(CF2O)n(CF(CF3)CF2O)mCOF is relatively stable, and anoth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C59/135C07C51/58C07C51/04C07D303/08C07D301/06B01F17/44C09K23/44
CPCC07C51/04C07C51/58C07D301/06C07D303/08C09K23/007
Inventor 肖鑫冀汝南于颖
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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