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Perfluor dioxole-modified fluorine-containing polymer

A dioxole, polymer technology, applied in offensive equipment, explosives, non-explosive/non-thermal agent components, etc., can solve the problems of limited application, inability to meet military industry, low glass transition temperature, etc.

Inactive Publication Date: 2015-03-25
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance composite materials at home and abroad use VDF / CTFE random copolymer (trade name F2314) with a copolymerization ratio of 1:4 as a structural binder, but the glass transition temperature is not higher than 50°C, which limits its high temperature treatment. Aspects of application
[0004] Chinese patent CN101186668A introduces a preparation method of fluorine-containing rubber for coatings. The main polymerization monomer is 50-80% chlorotrifluoroethylene and 20-50% vinylidene fluoride under the action of an organic initiator and a fluorine-containing emulsifier. Emulsion polymerization is carried out, and the polymers obtained by polymerization have different intrinsic viscosities and excellent solubility, but the glass transition temperature is less than 50°C, which cannot meet some special applications in the military industry
[0005] U.S. Patent Publication No. 2752331 and Chinese Patent Publication No. 102585077A focus on the P(VDF-CTFE) copolymer with low CTFE content. Although the resulting polymer has higher dipole density and energy density, the film it forms has very Fast discharge rate and low loss, but its glass transition temperature is relatively low. At room temperature, the solubility of esters and ketones is not ideal

Method used

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  • Perfluor dioxole-modified fluorine-containing polymer
  • Perfluor dioxole-modified fluorine-containing polymer
  • Perfluor dioxole-modified fluorine-containing polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] In a 50L stainless steel reaction kettle with a stirrer, add 30L of deionized water, blow nitrogen and oxygen three times, evacuate until the oxygen content is less than or equal to 25ppm, add 60g of fluorine-containing emulsifier ammonium perfluorooctanoate, 400ml of liquid paraffin (liquid at room temperature), Start stirring at a speed of 200 rpm, raise the temperature to 60°C, and add 85% chlorotrifluoroethylene, 8% vinylidene fluoride and 7% PDD mixed monomer to 2.0 MPa.

[0048] After the system is stable, add 9g of potassium persulfate, 3g of sodium sulfite, 15g of sodium acetate, and 30g of ethanol to start the polymerization reaction. At the same time, continuously add mixed monomers to keep the pressure of the reactor at 3.5 MPa until the solid content of the emulsion in the reactor reaches 30% to stop the reaction.

[0049] Recover the unreacted monomer, release the polymer emulsion, filter paraffin and other impurities, seal and freeze the obtained emulsion ...

Embodiment 2

[0051] In a 50L reactor, add 30L of deionized water, blow nitrogen and deoxygenate three times, evacuate until the oxygen content is less than or equal to 25ppm, add 60g of fluorine-containing emulsifier sodium perfluorooctanoate, 400ml of liquid paraffin (liquid at room temperature), and start stirring at a speed of 200rpm , heat up to 55°C, add 85% chlorotrifluoroethylene, 14.9% vinylidene fluoride and 0.1% PDD mixed monomer to 2.0MPa, after the system is stable, add 4g potassium persulfate and 5 ammonium persulfate composite initiators, 3g partial weight Sodium sulfite, 25g sodium acetate, 10g diethyl malonate, start the reaction. Polymerization begins. Simultaneously add mixed monomer constantly and keep reactor pressure 3.5MPa, stop reaction until emulsion solid content reaches 30% in the reactor, reclaim unreacted monomer, emit polymer emulsion, filter paraffin and other impurity, the emulsion that makes is in Seal and freeze in a frozen alcohol tank at -40°C, then thaw...

Embodiment 3

[0053] Repeat the steps described in Example 1, just add 12g potassium permanganate initiator and 12g oxalic acid, and simultaneously 85% chlorotrifluoroethylene, 5% vinylidene fluoride and 10% PDD mixed monomer. The results are listed in Table 1.

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Abstract

The invention belongs to the field of organic chemistry and relates to a perfluor dioxole-modified fluorine-containing polymer. A general formula of the perfluor dioxole is as shown in the specification, wherein R and F represent RF or ORF; RF is C1-C5 linear or branched perfluoroalkyl; X1 and X2 are independently used as F or CF3; and a fluorine-containing olefin monomer accounts for 80-99.1% of mass of a copolymerized monomer. According to the polymer disclosed by the invention, the glass-transition temperature is greater than 65 DEG C; the particle size is smaller than 120mum; the intrinsic viscosity is greater than 1.0dl / g; the polymer can be completely dissolved into common esters and other strong polar solvents; the problems that the glass-transition temperature of F23 fluorine polymers at present is relatively low and the like are solved; and the polymer can be widely applied to the military industry, and can be used as a binder for a polymer-bonded explosive and a binder for current collector metal for cells.

Description

technical field [0001] The invention belongs to the field of organic polymer compounds, and in particular relates to a vinylidene fluoride copolymer and a preparation method thereof. Background technique [0002] Fluoropolymers have many excellent properties that hydrocarbon polymers do not have, such as low surface tension and friction coefficient, excellent heat resistance, oxidation resistance, and chemical resistance. Polyvinylidene fluoride chlorotrifluoroethylene (P(VDF-CTFE)) is a kind of fluoropolymer. P(VDF-CTFE) with low CTFE content has high dipole density and energy density, and the formed film has a very fast discharge rate and low loss, which makes the application of P(VDF-CTFE) more realistic significance. P(VDF-CTFE) with high CTFE content is mainly used as a binder for polymer bonded explosives and a binder for battery collector metals, and is widely used in military, national defense, and aerospace system industries. [0003] Fluorine rubber VDF-CTFE (l:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/24C08F214/22C08F234/02C08F2/28C08F2/38C06B23/00
Inventor 王先荣李斌余金龙张廷建兰军常映军
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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