Method for synthesizing fluoro-polypxylene

A technology of parylene and p-xylene, applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry and other directions, can solve problems such as difficulty in realizing industrialization, no literature reports, etc., and achieve stable yield, short synthesis route, Effects suitable for mass production

Inactive Publication Date: 2005-11-16
SHANGHAI RECORD PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

U.S. Patent US6284993, US5536892.Tetrahedrom.Letters, Russian Patent RU2032654, Japanese Patent JP2003089679, document 42 (21), 3555-3557.Polym.Chem, 33 (3) 359-363 (English) 1995 all reported 1,1, 9, the synthetic method of 9-tetrafluoroparylene and octafluoroparylene, but there is no synthetic method of 1,2,9,10-tetrafluoroparylene at present, and because the above-mentioned synthetic method It is difficult to realize industrialization, so it is an urgent problem to find a new method to realize industrialized production of tetrafluoroparylene

Method used

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  • Method for synthesizing fluoro-polypxylene
  • Method for synthesizing fluoro-polypxylene

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Experimental program
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Effect test

Embodiment 1

[0021] Add 48.4g (0.2mol) of raw materials p-dichlorotoluene and 200ml dimethyl sulfoxide into a 500mL three-necked flask, add 29g (0.5mol) of potassium fluoride, then add catalyst tetrabutylammonium chloride 0.01mol, heat to 140 ℃ reaction for 6 hours, after the reaction is completed, slowly add 100ml of water and 100ml of toluene after cooling down to room temperature, continue to stir for 30 minutes, then separate the reaction mixture, separate the organic phase, and extract the aqueous phase twice with 100ml of toluene*2, Combine the organic phases, wash the organic phase once with saturated sodium bicarbonate solution and saturated brine, dry over anhydrous sodium sulfate, remove toluene by rotary evaporation, and distill under reduced pressure to obtain the product p-chlorofluorotoluene.

[0022] Add Pd / C / Al8.0g (5% Pd / C6g mixed with 2g Al powder) into a 500mL three-necked flask, then add 200mL of toluene, stir for 5 minutes, cool to -5°C in an ice-water bath, and then ad...

Embodiment 2

[0024] Add 62g (0.2mol) of α-perhalogenated p-xylene and 200ml dimethyl sulfoxide into a 500mL three-necked flask, add 52.2g (0.9mol) of potassium fluoride, then add a catalytic amount of tetrabutylammonium chloride, heat React at 150°C for 8 hours. After the reaction is finished, after cooling down to room temperature, slowly add 100ml of water and 100ml of toluene, continue to stir for 30 minutes, then separate the reaction mixture, separate the organic phase, and extract the aqueous phase twice with 100ml of toluene*2, combine the organic phase, organic The phase was washed once with saturated sodium bicarbonate solution and saturated brine, dried over anhydrous sodium sulfate, toluene was removed by rotary evaporation, and the product p-difluoro-chlorotoluene was obtained by distillation under reduced pressure.

[0025] Add Pd / C / Al8.0g (5% Pd / C6g mixed with 2g Al powder) into a 500mL three-necked flask, then add 200mL of toluene, stir for 5 minutes, cool to -5°C in an ice-...

Embodiment 3

[0027] Add 48.4g (0.2mol) of raw materials p-dichlorotoluene and 200ml dimethyl sulfoxide into a 500mL three-necked flask, add 40g (0.7mol) of potassium fluoride, then add 2.5g of catalyst tetrabutylammonium chloride, and heat to 170 ℃ reaction for 4 hours, after the reaction is completed, slowly add 100ml of water and 100ml of toluene after cooling down to room temperature, continue to stir for 30 minutes, then separate the reaction mixture, separate the organic phase, and extract the aqueous phase twice with 100ml of toluene*2, Combine the organic phases, wash the organic phase once with saturated sodium bicarbonate solution and saturated brine, dry over anhydrous sodium sulfate, remove toluene by rotary evaporation, and distill under reduced pressure to obtain the product p-chlorofluorotoluene.

[0028] Add 8.0g Ni / C / Zn (5% Ni / C6g mixed with 2g Zn powder) into a 500mL three-necked flask, then add 200mL dimethyl sulfoxide, stir for 5 minutes, cool to -5°C in an ice-water bath...

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Abstract

A process for synthesizing the poly-p-fluoroxylene from P-xylene includes controlling the reaction point whiel chlorinating to obtain P-2,2-chlorotoluene or p-2,3-chlorotoluene, fluorinating to obtain p-2-Cl-fluorotoluene or p-2,2-fluoro-chlorotoluene, and catalytic cyclizing polymerization to obtain 1,2,9,10-tetrafluoro-poly-p-xylene or 1,1,2,2,9.9,10,10-octofluoro-poly-p-xylene.

Description

technical field [0001] The invention relates to a synthetic method of a class of fluorine-containing polymers, in particular to a synthetic method of tetrafluoro and octafluoroparylene. Background technique [0002] Fluorinated parylene is a promising fluoropolymer. In recent years, such compounds have attracted much attention in the fields of microelectronics, electronic components, medical devices and other fields because of their good insulation, high temperature resistance and strong oxidation resistance. U.S. Patent US6284993, US5536892.Tetrahedrom.Letters, Russian Patent RU2032654, Japanese Patent JP2003089679, document 42 (21), 3555-3557.Polym.Chem, 33 (3) 359-363 (English) 1995 all reported 1,1, 9, the synthetic method of 9-tetrafluoroparylene and octafluoroparylene, but there is no synthetic method of 1,2,9,10-tetrafluoroparylene at present, and because the above-mentioned synthetic method It is difficult to realize industrialization, so finding a new method of te...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C23/18
Inventor 张芳江
Owner SHANGHAI RECORD PHARM CO LTD
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