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The preparation method of polyvinylidene fluoride

A technology of polyvinylidene fluoride and vinylidene fluoride, which is applied in the field of preparation of polyvinylidene fluoride, can solve the problems of product yellowing, chemical resistance reduction, and processing difficulties, and achieve mild process conditions, high production efficiency, and uniform molecular weight Effect

Active Publication Date: 2019-03-29
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In addition, the patent FR2259114 uses acetone as the chain transfer agent, the patent US4360652 uses isopropanol as the chain transfer agent, and CN101218264B uses dimethyl ether, halogenated hydrocarbons and alkanes as the chain transfer agent, but the PVDF obtained by using these chain transfer agents still has a wide range. Molecular weight distribution, its molecular weight distribution coefficient is usually between 4-20
A large amount of high molecular weight components leads to processing difficulties, and a large amount of low molecular weight components leads to yellowing of products and reduced mechanical properties and chemical resistance
[0010] And from the content disclosed in the above patent documents, we can also know that none of the documents involve product characteristics such as polymerization time, yield, and particle size of polyvinylidene fluoride; even in CN101218264B, a comparison of polymerization time, average particle size, and solid content is given. data, but except for the aggregation time, the rest of the data have not improved significantly, so it can be seen that the existing technology has not made any substantial improvement to the overall production efficiency

Method used

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  • The preparation method of polyvinylidene fluoride
  • The preparation method of polyvinylidene fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a 100L horizontal reactor, add 60L of deionized water, 2g of initial chain transfer agent ethyl acrylate, and 100g of an aqueous solution of 20% perfluorocarboxylate polyether ammonium salt, evacuate and remove oxygen until the oxygen content is ≤30ppm is qualified. Then the temperature of the polymerization kettle is raised to 60° C., by adding vinylidene fluoride monomer to the pressure of 3.0 MPa in the kettle, then use a metering pump to quickly inject 100 g of the initial organic initiator solution (15% diisopropyl Hydrogen peroxide), start polymerization, keep temperature, pressure constant, after 10min, inject at a constant speed with metering pump, 1500g10% chain transfer agent solution (regulator is ethyl propionate) and 300g 15% add trigger Dosage solution, 2h finished. During the polymerization reaction, keep the temperature and pressure of the kettle constant, and stop the reaction when a certain amount of reaction is reached. Coagulation, washing, dryi...

Embodiment 2

[0035] The difference from Example 1 is that the initial chain transfer dose is changed to 5 g, and the additional chain transfer dose is changed to 3000 g of 5% chain transfer agent solution.

Embodiment 3

[0037] The difference from Example 1 is that the added chain transfer agent is changed to ethyl acetate.

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Abstract

The invention belongs to the technical field of organic synthesis and particularly relates to a preparation method of PVDF. Vinyl fluoride, deionized water, initial chain transfer agents and a dispersing agent are added to a reaction kettle, evacuation and deoxygenization are performed, the temperature is raised to 20 DEG C to 150 DEG C, the kettle is refilled with vinylidene fluoride monomers until the pressure in the kettle is 1.0-6.0 MPa, and an initial chain transfer agent is added; polymerization reaction is started, the kettle is refilled with another chain transfer agent and a replenishing initiator, and after the reaction, the finished product is obtained after the obtained polymer emulsion is subjected to condensation, washing, drying and granulation. According to the preparation method of the PVDF, two kinds of chain transfer agents are firstly used in the polymerization process, a production technology of the PVDF with controllable molecular weight and distribution of the molecular weight for narrow size distribution is provided, and the technological conditions are mild and easy to control; the molecular weight of the product obtained by polymerization is uniform, the distribution is narrow, and the production efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of polyvinylidene fluoride. Background technique [0002] Polyvinylidene fluoride (PVDF) is a fluorine-containing thermoplastic engineering plastic with chemical corrosion resistance, aging resistance and excellent mechanical processing properties. It is processed into various products through extrusion, injection, molding and other molding processes. It is widely used In the manufacturing industry, electronics industry and water treatment industry and other fields. [0003] In view of the increasingly widespread application of PVDF, people's demand for PVDF is increasing, and the attention paid to the yield of PVDF is getting higher and higher; in addition, in terms of product performance, especially in the molding process, uneven heating, Wide molecular weight distribution and easy decomposition of small molecular substances will caus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F114/22C08F2/38C08F2/30
CPCC08F2/30C08F2/38C08F114/22
Inventor 王汉利李秀芬唐妮杜延华韩瑞芹许克
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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