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Polyvinylidene fluoride preparation method

A technology selected from polyvinylidene fluoride, which is applied in the field of preparation of fluorine-containing polymers, can solve the problems of high system pressure, high reaction risk, and long time consumption, and achieve the effect of reducing the reaction temperature

Active Publication Date: 2014-11-19
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former because the initial reaction temperature is lower than the decomposition temperature of the initiator, the reaction speed is too slow and takes too long; the latter has a high system pressure and a high risk of reaction. In addition, the reaction rate can only be partially improved and cannot be fundamentally solved.
Therefore, the main problem faced by the traditional method is how to successfully apply the highly active peroxide initiator to the suspension polymerization of vinylidene fluoride, so that the system can be carried out safely and quickly.

Method used

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  • Polyvinylidene fluoride preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0031] In a 5L vertical stainless steel jacketed and stirred polymerization reactor, the nitrogen was evacuated 5 times to detect that the oxygen content in the reactor was lower than 20ppm, and the system was filled with nitrogen to slightly positive pressure, and the temperature of the system was controlled at -2°C. Perfluoro(2-ethoxy)propionyl chloride (CF 3 CF 2 OCF 2 CF 2 COCl) trifluorotrichloroethane solution 100ml (concentration is 6%), stirring speed is 200rpm. Slowly add 12.27 g of a pre-configured mixed solution of NaOH and 30% hydrogen peroxide to the system, which contains 0.8 g of NaOH and 2.27 g of 30% hydrogen peroxide. Control the temperature of the system at -10°C and stir for 0.5h. 2.7 L of deionized water dissolved in 3.1 g of isopropylcyclopentane and 4.1 g of methylcellulose cooled at 2°C was passed into the system. The stirring speed was increased to 600 rpm, and 600 g of liquid monomer vinylidene fluoride was introduced into the system. The temper...

Embodiment 2

[0033] In a 5L vertical stainless steel jacketed and stirred polymerization reactor, the nitrogen was evacuated and replaced 5 times to check that the oxygen content reached the standard, so that the system pressure was slightly positive, and the system temperature was controlled at -5°C. into the dissolved F(CF 2 CF 2 OCF 2 ) 4 COCl trifluorotrichloroethane solution 100ml (concentration: 15%), the stirring speed is 200rpm. Slowly add 12.27 g of a pre-configured mixed solution of NaOH and 30% hydrogen peroxide to the system, which contains 0.8 g of NaOH and 2.27 g of 30% hydrogen peroxide. The system was stirred at -5°C for 1 h. 2.7 L of deionized water dissolved in 3.1 g of isopropylcyclopentane and 4.1 g of methylcellulose cooled at 2°C was passed into the system. The stirring speed was increased to 600 rpm, and 600 g of liquid monomer vinylidene fluoride was introduced into the system. The temperature was raised to 20°C within half an hour for the reaction, and the re...

Embodiment 3

[0035] In a 5L vertical stainless steel jacketed and stirred polymerization reactor, the nitrogen was evacuated and replaced 5 times to check that the oxygen content reached the standard, so that the system pressure was slightly positive, and the system temperature was controlled at 0°C. into the dissolved CF 2 CF 2 COCl trifluorotrichloroethane solution 100ml (concentration: 3.5%), stirring speed is 200rpm. Slowly add 12.27 g of a pre-configured mixed solution of NaOH and 30% hydrogen peroxide to the system, which contains 1.12 g of KOH and 2.27 g of 30% hydrogen peroxide. The system was stirred at -5°C for 1 h. 2.7 L of deionized water dissolved in 3.1 g of isopropylcyclopentane and 4.1 g of methylcellulose cooled at 2°C was passed into the system. The stirring speed was increased to 600 rpm, and 600 g of liquid monomer vinylidene fluoride was introduced into the system. The temperature was raised to 30°C within half an hour for the reaction, the temperature was raised t...

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Abstract

The present invention relates to a polyvinylidene fluoride preparation method, which comprises: introducing an acyl halide solution dispersed in a fluorine-containing organic solvent into a reaction kettle, adding a mixed solution comprising an inorganic alkali solution and hydrogen peroxide, carrying out a stirring reaction for 30-120 min at a temperature of -10-10 DEG C, carrying out in situ synthesis to obtain an initiator, introducing an aqueous solution of a dispersing agent, a vinylidene fluoride monomer and a chain transfer agent, carrying out a stirring reaction for 4-12 h at a temperature of 10-30 DEG C to prepare polyvinylidene fluoride, and carrying out filtering, washing, drying and crushing after completing the reaction to obtain the powdery product which is polyvinylidene fluoride resin powder. The powdery polyvinylidene fluoride resin has characteristics of good thermal stability, good physical property, good mechanical property, simple reaction process and easy control, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing fluorine-containing polymers, in particular to a method for preparing polyvinylidene fluoride. Background technique [0002] Polyvinylidene fluoride (PVDF) resin mainly refers to a homopolymer of vinylidene fluoride or a copolymer of vinylidene fluoride and a small amount of other fluorine-containing vinyl monomers. PVDF resin has the characteristics of both fluororesin and general-purpose resin. In addition to chemical corrosion resistance, high temperature resistance, oxidation resistance, weather resistance, and radiation resistance, it also has special properties such as piezoelectricity, dielectricity, and pyroelectricity. It is currently the second largest output of fluorine-containing plastics. big product. The preparation methods of PVDF resin include emulsion polymerization, suspension polymerization and solution polymerization. Among them, emulsion polymerization and suspension polymerization ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F114/22C08F4/34C08F2/20
Inventor 王寅飞郑炳发黄凯金
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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