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Preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether

A polyoxyalkylene and perfluoroolefin technology, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc. Problems such as low preparation and reaction safety, to achieve the effect of improving yield, improving reaction selectivity and yield

Pending Publication Date: 2021-06-11
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of this, the purpose of this application is to provide a preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether, which solves the problem that the high number average molecular weight of peroxidized perfluoropolyoxyalkylene cannot be efficiently prepared in the existing preparation method, The problem of low yield and low reaction safety has realized the stable control and adjustment of the number average molecular weight of peroxidized perfluoropolyoxyalkylene compounds between 600 and 50,000, high reaction safety and yield, and is suitable for industrial continuous production

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  • Preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether
  • Preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether

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preparation example Construction

[0038] In view of the problems that the current preparation method cannot realize the efficient preparation of peroxidized perfluoropolyoxyalkylene compounds with high number-average molecular weight, the product yield is low, and the industrial safety and continuous production cannot be realized. In the preparation of perfluoropolyoxyalkylene peroxide, the microscopic mixing, mass transfer and heat transfer process of the reaction are greatly enhanced, the reaction time of the material in the high gravity reactor is greatly shortened, and the reaction selectivity and total yield are greatly improved , and there is no local overheating, avoiding production safety problems, and realizing continuous industrial production.

[0039] The embodiment of the present application provides a method for preparing perfluoropolyoxyalkylene peroxide and perfluoropolyether, which solves the problem that the high number average molecular weight of perfluoropolyoxyalkylene peroxide cannot be eff...

Embodiment 1

[0069] According to this embodiment figure 1 Operate as shown in the process flow chart.

[0070] f 2 / O 2 Mixed gas preparation: at room temperature, pass the fluorine-nitrogen mixed gas with a mass ratio of 20% of fluorine gas and oxygen into the gas distribution tank respectively according to the raw material ratio requirements shown in Table 1 through the respective Cortesian mass flow meters , get F 2 / O 2 mixed gas.

[0071] Peroxidized perfluoropolyoxyalkylene synthesis: tetrafluoroethylene (TFE), solvent, F 2 / O 2 The mixed gas is continuously fed into the high-gravity reactor of the self-rotating packed bed at the same time, and the tetrafluoroethylene, solvent, F 2 / O 2 The inlet flow rate of the mixed gas, and the maximum flow rate shall not exceed 1kg / h. Control the reaction pressure in the reactor to normal pressure, the reaction residence time is 30s~80s, and the supergravity level is 10g. After the tail gas flows out from the gas phase outlet above the ...

Embodiment 2-8

[0078] Embodiment 2-8 uses tetrafluoroethylene as raw material, adopts the operating procedure substantially identical with embodiment 1 to prepare peroxidized perfluoropolyoxyalkylene, and concrete reaction conditions and corresponding reaction result are shown in Table 1, wherein CF 3 When OF is the initiator, CF 3 OF / O 2 The mixed gas is prepared as follows: at room temperature, the CF 3 Fluorine-nitrogen mixed gas with a mass ratio of 20% of OF and oxygen are respectively passed into the gas distribution tank according to the raw material ratio requirements shown in Table 1 to obtain CF 3 OF / O 2 mixed gas.

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Abstract

The invention discloses a preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether, and relates to the technical field of fluorine chemical industry. The preparation method of perfluoropolyoxyalkylene peroxide comprises the step of synthesizing perfluoropolyoxyalkylene peroxide from perfluoroalkene and oxygen in a supergravity reactor. According to the preparation method, the problems that perfluoropolyoxyalkylene peroxide with high number-average molecular weight cannot be efficiently prepared, the yield is low and the reaction safety is low in the existing preparation method are solved, the number-average molecular weight of the perfluoropolyoxyalkylene peroxide compound can be stably controlled and adjusted between 600 and 50000, the reaction safety and the yield are high, and the preparation method is suitable for industrial continuous production.

Description

technical field [0001] The application relates to the technical field of fluorine chemical industry, in particular to a preparation method of perfluoropolyoxyalkylene peroxide and perfluoropolyether. Background technique [0002] Perfluoropolyether (English name PerfIuoro PoIyethers, abbreviated as PFPE) is a synthetic polymer that is liquid at room temperature, and its molecular weight distribution ranges from hundreds to hundreds of thousands. It is an industrial product with extremely superior performance and a wide range of uses, such as measurement in electrical sensors, vapor phase or liquid phase welding, protection of building materials, high temperature lubricating grease, etc., in the synthesis of anti-fingerprint agents, high-speed hard disk lubricants It has an irreplaceable advantage in the synthesis. Perfluoropolyoxyalkylene peroxide, as the precursor material of perfluoropolyether, can be converted into inert perfluoropolyether without peroxy group and active...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00B01J19/28C07C407/00C07C409/16
CPCC08G65/007B01J19/28C07C407/00C07C409/16
Inventor 周黎旸吕杨张亮亮李宏峰陈建峰王树华雷志刚初广文
Owner JUHUA GROUP TECH CENT
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