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Method for preparing functional fluorine-bearing monomer by vertical-tube type catalytic reaction

A functional, standpipe-type technology, applied in the field of preparation of functional fluorine-containing monomers, can solve the problems of reduced service life and mechanical properties of exchange membrane materials, so as to eliminate energy waste, improve utilization rate, and avoid environmental pollution Effect

Active Publication Date: 2010-05-26
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The direction of development of chlor-alkali ion exchange membrane is to improve ion conductivity, reduce cell voltage, and save energy. The known method is to increase the ion exchange capacity of sulfonic acid resin, but simply passing through high resin ion exchange capacity will cause the exchange membrane material to be mechanically damaged. Reduced performance, reduced service life

Method used

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  • Method for preparing functional fluorine-bearing monomer by vertical-tube type catalytic reaction
  • Method for preparing functional fluorine-bearing monomer by vertical-tube type catalytic reaction
  • Method for preparing functional fluorine-bearing monomer by vertical-tube type catalytic reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0043]The vertical pipe reactor that is equipped with circulating cooling / heating system, temperature control system and is filled with gac catalyst is vacuumized inside the system by the decompression system at the top, (the inner diameter of the vertical pipe reactor is 160mm, and the length is 3500mm, Hastelloy material) filled with nitrogen for three times until the oxygen content is controlled below 10ppm, vacuumed to -0.1MPa, closed the pressure reducing valve, adjusted the temperature of the circulating water to keep the internal temperature of the reactor at 0°C, from the lower part of the tubular reactor Slowly add tetrafluorosultone (molecular formula: FO 2 SCF 2 COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:5, and the residence time of the liquid materials in the reactor is controlled by a feed flowmeter to be 10min to maintain continuous feed and discharge. The product with the designed structure...

Embodiment 2

[0046] A vertical tube reactor equipped with a circulating cooling / heating system and a temperature control system filled with activated carbon, macroporous molecular sieves, and a mixed catalyst with a mass ratio of porous alumina of 1:1:1 was used to pump the inside of the system through the top decompression system. Vacuum, (the inner diameter of the standpipe reactor is 180mm, the length is 4000mm, made of Hastelloy alloy) filled with nitrogen and replaced three times until the oxygen content is controlled below 10ppm, vacuumed to -0.1MPa, closed the pressure reducing valve, and adjusted the circulating water The temperature inside the reactor was controlled at 3°C, and perfluoro 5-acyl fluoride-4-methyl-3-oxa-pentanesulfonyl fluoride (molecular formula: FO 2 SCF 2 CF 2 OCF (CF 3 )COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:7, and the residence time of the liquid materials in the reactor is controlled...

Embodiment 3

[0049] A vertical tube reactor equipped with a circulating cooling / heating system and a temperature control system filled with activated carbon and a mixed catalyst with a mass ratio of porous alumina of 2:1 will vacuumize the inside of the system through the top decompression system, (vertical tube type The inner diameter of the reactor is 200mm, the length is 4100mm, and the Hastelloy material) is filled with nitrogen for three times until the oxygen content is controlled below 10ppm, then vacuumed to -0.1MPa, the pressure reducing valve is closed, and the temperature of the circulating water is adjusted to control the internal temperature of the reactor. Temperature at 5°C, slowly add perfluoro 3-acyl fluoride-propanesulfonyl fluoride (molecular formula: FO 2 SCF 2 CF 2 COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:6. The residence time of the liquid materials in the reactor is controlled by a feed flowme...

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Abstract

The invention discloses a preparation method of a functional fluorine-containing monomer. The method comprises the following steps of: uniformly mixing a perfluoro-linear chain or branched chain acyl fluoride compound, trifluoroethylene sulfuric ester and anhydrous hydrogen fluoride liquid in the mole ratio of 1:1:(1-20); passing from bottom to top through a vertical-tube type reactor which is filled with a catalyst; finishing addition reaction in a short time under the action of the high specific surface area catalyst inside the reactor; and setting apart a reaction liquid product from the upper part of the vertical-tube type reactor to form a product with a general formula in formula (I). In the invention, the functional fluorine-containing monomer can be prepared continuously and efficiently with easily operated reaction equipment, conveniently controlled reaction temperature and no use of any organic solvent, and a high-purity monomer can be obtained through simple rectification. The catalyst filling in the tubular reactor is one or a mixture of active carbon, macro-porousmolecular sieve and porous aluminum oxide. The reaction can be carried out continuously inside the reactor and satisfies industrialization requirements. CF2=CF-O-Rf(I).

Description

technical field [0001] The invention belongs to the field of fluorine-containing fine chemicals, and relates to a preparation method of a class of functional fluorine-containing monomers, which are applied to the synthesis of fluorine resins with proton exchange functions. Background technique [0002] Since perfluorosulfonic acid ion exchange membranes were applied in the chlor-alkali industry and proton exchange membrane fuel cells in the 1970s, perfluorosulfonic acid ion exchange membranes have been widely used and researched in countries all over the world. The use of fluorinated or non-fluorinated ion exchange membranes in electrolyzers and fuel cells is currently known. Such ionic membranes have bonded anions and bonded cations for cation exchange. The ionic membrane divides the battery or electrolyzer into a cathode chamber and an anode chamber, through which ions can selectively pass. Although many polymers can be used as ion exchange membranes, it has been proven ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/82C07C303/02C07F9/40
Inventor 高自宏张永明秦胜魏茂祥宋学章赵淑慧
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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