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Method for preparing fluroxene by vertical-tube type catalytic reaction

A fluoroalkenyl ether and riser-type technology, which is applied in the field of fluorine-containing fine chemicals, can solve the problems of chlorine gas and caustic soda current efficiency drop, etc., and achieve the effect of improving product purity, meeting the demand of output and improving utilization rate

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

Practice has proved that fluorine-containing ion-exchange membranes containing ion-exchange groups, especially sulfonic acid groups and carboxylic acid groups, are more suitable for use as composite ion-exchange membranes for chlor-alkali electrolyzers due to their resistance to chemical degradation. The exchange membrane of the fluorine-containing carboxylic acid layer mainly prevents the reverse migration of hydroxyl anions into the anode chamber. Once the reverse migration of hydroxyl anions enters the anode chamber, the current efficiency of chlorine gas and caustic soda will be greatly reduced.

Method used

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  • Method for preparing fluroxene by vertical-tube type catalytic reaction
  • Method for preparing fluroxene by vertical-tube type catalytic reaction
  • Method for preparing fluroxene by vertical-tube type catalytic reaction

Examples

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Effect test

Embodiment 1

[0042] The vertical tube reactor that is equipped with circulating cooling / heating system, temperature control system and is filled with activated carbon catalyst is vacuumized inside the system by the decompression system at the top, (the inner diameter of the vertical tube reactor is 170mm, and the length is 3600mm, 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, and adjusted the temperature of the circulating water to keep the internal temperature of the reactor at 1°C. From the lower part of the tubular reactor Slowly add 3-methoxycarboxypropionyl fluoride (molecular formula: CH 3 OOCCF 2COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:6, and the residence time of the liquid materials in the reactor is controlled by a feed flowmeter to be 10min to maintain continuous feeding and discharging. ...

Embodiment 2

[0045] A vertical pipe 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 2:1:1 is used to pump the inside of the system through the top decompression system. Vacuum, (the inner diameter of the vertical pipe reactor is 185mm, the length is 4100mm, made of Hastelloy alloy) filled with nitrogen and replaced three times until the oxygen content is controlled below 10ppm, then vacuumed to -0.1MPa, closed the pressure reducing valve, and adjusted the circulating water The temperature is controlled at 4°C inside the reactor, and 4-methoxymethyl fluorine-containing butyryl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:9, and the residence time of the liquid materials in the reactor is controlled by a feed flowm...

Embodiment 3

[0048] 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 2:3 will evacuate 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 6-methoxycarboxypropoxy propionyl fluoride (molecular formula: CH 3 OOCCF 2 CF 2 OCF (CF 3 )COF), trifluorovinyl sulfate, and anhydrous hydrogen fluoride are mixed liquid materials with a molar ratio of 1:1:10, and the residence time of the liquid materials in the reactor is controlled by a f...

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Abstract

The invention discloses a preparation method of fluorine-containing vinyl ether. 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, a functional fluorine-containing monomer can be prepared continuously and efficiently with no adoption of high temperature pyrolysis path, 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 reaction is 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 fluoroalkenes, which are widely used in the synthesis of fluororesins with proton exchange functions, and membrane products prepared from such fluororesins are used in the chlor-alkali industry In the electrolytic cell composite membrane diaphragm, it plays a dual role of transporting protons and preventing the reverse migration of hydroxyl radicals from the cathode chamber to the anode chamber. Background technique [0002] Since the ionic membrane electrolysis method was applied in the chlor-alkali industry in the 1970s, this technology has become the development direction of the technical transformation of old factories in the chlor-alkali industry and the development of new electrolysis devices. The use of fluorine-containing ion exchange membranes in electrolyzers is a known technology. Such ionic membranes have bonded anion...

Claims

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Application Information

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IPC IPC(8): C07C69/734C07C67/31C07C43/17C07C41/01C07C255/13C07C253/30C07C235/06C07C231/12
Inventor 张永明秦胜高自宏李勇王汉利赵淑慧
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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