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Polyvinylidene fluoride resin preparation method and reaction equipment

A polyvinylidene fluoride resin and reaction vessel technology, applied in the field of polyvinylidene fluoride resin preparation and reaction equipment, can solve the problems of reducing the heat transfer efficiency of the reactor, increasing the frequency of overhaul of reaction equipment, and increasing operating costs, etc.

Active Publication Date: 2019-03-12
INNER MONGOLIA WANHAO FLUOROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sticky kettle will reduce the heat transfer efficiency of the reactor, increase the frequency of overhaul of reaction equipment, and increase operating costs

Method used

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  • Polyvinylidene fluoride resin preparation method and reaction equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Add 5kg deionized water, 5g hydroxypropyl methylcellulose and 10g diethyl malonate to a 10L autoclave equipped with a liquid phase stirrer, a gas phase stirrer and an initiator feeding tube, the liquid level of the liquid phase The material outlet that has not passed the initiator feeding pipe is degassed. At 50°C, 5.5MPa and the liquid phase and gas phase agitator are turned on, add 2g of diisopropyl peroxydicarbonate along the initiator feeding pipe through a metering pump to initiate a supercritical polymerization reaction, and continuously add VDF during the reaction process The pressure of the monomer is maintained at 5-7MPa, and the reaction is terminated after 5.5 hours of reaction.

[0061] After the polymerization, the polymer slurry was washed and dried at 105° C. to obtain polyvinylidene fluoride powder.

[0062] The sieve weight of the obtained polyvinylidene fluoride powder was measured, and the results are listed in Table 1 below.

Embodiment 2

[0064] Add 5kg deionized water, 5g hydroxypropyl methylcellulose and 10g diethyl malonate to a 10L autoclave equipped with a liquid phase stirrer, a gas phase stirrer and an initiator feeding tube, the liquid level of the liquid phase The material outlet that has not passed the initiator feeding pipe is degassed. At 50°C, 5.5MPa, and the gas phase and liquid phase agitator are turned on, add 2g of diisopropyl peroxydicarbonate along the gas phase from the top of the reactor through a metering pump to initiate a supercritical polymerization reaction. The VDF monomer maintains the pressure at 5-7MPa, and the reaction ends after 4-6 hours.

[0065] After the polymerization, the polymer slurry was washed and dried at 105° C. to obtain polyvinylidene fluoride powder.

[0066] The sieve weight of the obtained polyvinylidene fluoride powder was measured by the above method, and the results are listed in Table 1 below.

Embodiment 3

[0068] Add 5kg deionized water, 5g hydroxypropyl methylcellulose and 10g diethyl malonate to a 10L autoclave equipped with a liquid phase stirrer, a gas phase stirrer and an initiator feeding tube, the liquid level of the liquid phase The material outlet that has not passed the initiator feeding pipe is degassed. At 50°C, 5.5MPa and the liquid phase agitator is turned on but the gas phase agitator is not turned on, add 2g of diisopropyl peroxydicarbonate along the initiator feeding pipe through a metering pump to initiate supercritical polymerization reaction, during the reaction Constantly add VDF monomer to maintain the pressure at 5-7MPa, and stop the reaction after 4-6 hours.

[0069] After the polymerization, the polymer slurry was washed and dried at 105° C. to obtain polyvinylidene fluoride powder.

[0070] The sieve weight of the obtained polyvinylidene fluoride powder was measured by the above method, and the results are listed in Table 1 below.

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Abstract

The invention discloses a polyvinylidene fluoride resin preparation method and reaction equipment. The method comprises the steps of adding a reaction medium, a dispersing agent and a chain transfer agent to a reaction vessel, performing degasification, and introducing an initiating agent and a vinylidene fluoride monomer so as to be subjected to polymerization reaction. In a reaction process, a gas phase and a liquid phase are stirred simultaneously. The reaction vessel comprises a stirrer for stirring the liquid phase, a stirrer for stirring the gas phase and an initiating agent charging pipeline connected with a fluid in the reaction vessel, wherein a discharging hole of the initiating agent charging pipeline is positioned below the liquid level of the reaction medium.

Description

technical field [0001] The invention relates to a method for preparing polyvinylidene fluoride resin by supercritical suspension polymerization. The method can advantageously reduce kettle sticking, improve manufacturing efficiency and reduce cost. The invention also relates to a reaction apparatus which is especially useful in the process according to the invention. Background technique [0002] Polyvinylidene fluoride (PVDF) resin mainly refers to a homopolymer of vinylidene fluoride (VDF) or a copolymer of vinylidene fluoride and other small amounts of fluorine-containing vinyl monomers. Polyvinylidene fluoride resin has the characteristics of both fluororesin and general-purpose resin. In addition to good chemical corrosion resistance, high temperature resistance, oxidation resistance, weather resistance and radiation resistance, it also has piezoelectricity, dielectric It has special properties such as thermal resistance and pyroelectricity, and is currently the second...

Claims

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Application Information

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IPC IPC(8): C08F114/22C08F2/20C08F2/38C08F2/01B01J19/18
CPCB01J19/18C08F2/01C08F2/20C08F2/38C08F114/22Y02P20/54
Inventor 梁聪强陈惠强王伟兵钱辉罗卿朱世炜徐俊文许卫忠吴君毅杜丽君
Owner INNER MONGOLIA WANHAO FLUOROCHEM
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