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Method for preparing poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene)

A technology of chlorotrifluoroethylene and vinylidene fluoride, which is applied in the field of hydrogenation reduction reaction, can solve the problems of fluoropolymer elimination and degradation, copper salt is difficult to remove, etc., and achieves low cost, friendly to human body and environment, simple and easy to control method operation Effect

Active Publication Date: 2012-09-19
陕西德天励成新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the previous hydrogenation system, this system has greatly improved both in terms of controllability and environmental friendliness. However, copper salts are difficult to remove in the polymer, and at the same time, the use of nitrogen-containing ligands is also easy. Causes elimination degradation of fluoropolymers

Method used

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  • Method for preparing poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene)
  • Method for preparing poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene)
  • Method for preparing poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for preparing poly(vinylidene fluoride-chlorotrifluoroethylene-trifluoroethylene) by reduction of poly(vinylidene fluoride-chlorotrifluoroethylene) comprises the following steps:

[0020] Step 1. In the three-necked flask, add poly(vinylidene fluoride-trifluoroethylene) P(VDF-CTFE), the molar composition is VDF / CTFE=80:20, and at the same time add solvent, poly(vinylidene fluoride-trifluoroethylene) The mass ratio of chlorofluoroethylene) P(VDF-CTFE) to solvent is 4.5:100. After the poly(vinylidene fluoride-trifluorochloroethylene)P(VDF-CTFE) is fully dissolved, a reducing agent is added, and the reducing agent and poly (Vinylidene fluoride-chlorotrifluoroethylene)P(VDF-CTFE)The molar ratio of Cl atoms is 3.4:1, after the reductant is dissolved by magnetic stirring, continue to stir and react at room temperature for 20 hours;

[0021] Described solvent is tetrahydrofuran;

[0022] The reducing agent is LiAlH 4 ;

[0023] Step 2: Pour the final solution obtai...

Embodiment 2

[0027] A method for preparing poly(vinylidene fluoride-chlorotrifluoroethylene-trifluoroethylene) by reduction of poly(vinylidene fluoride-chlorotrifluoroethylene) comprises the following steps:

[0028]Step 1. In the three-necked flask, add poly(vinylidene fluoride-trifluoroethylene) P(VDF-CTFE), the molar composition is VDF / CTFE=80:20, and at the same time add solvent, poly(vinylidene fluoride-trifluoroethylene) The mass ratio of chlorofluoroethylene) P(VDF-CTFE) to solvent is 3.6:100. After the poly(vinylidene fluoride-trifluorochloroethylene)P(VDF-CTFE) is fully dissolved, a reducing agent is added, and the reducing agent and poly (Vinylidene fluoride-chlorotrifluoroethylene)P(VDF-CTFE)The molar ratio of Cl atoms is 2.7:1, after the reductant is dissolved by magnetic stirring, continue to stir and react at room temperature for 20 hours;

[0029] Described solvent is dimethyl sulfoxide;

[0030] The reducing agent is LiAlH 4 ;

[0031] Step 2: Pour the final solution obt...

Embodiment 3

[0034] A method for preparing poly(vinylidene fluoride-chlorotrifluoroethylene-trifluoroethylene) by reduction of poly(vinylidene fluoride-chlorotrifluoroethylene) comprises the following steps:

[0035] Step 1. In the three-necked flask, add poly(vinylidene fluoride-trifluoroethylene) P(VDF-CTFE), the molar composition is VDF / CTFE=80:20, and at the same time add solvent, poly(vinylidene fluoride-trifluoroethylene) The mass ratio of chlorofluoroethylene) P(VDF-CTFE) to solvent is 4.5:100, after poly(vinylidene fluoride-trifluorochloroethylene)P(VDF-CTFE) is fully dissolved, add reducing agent, reducing agent and poly (Vinylidene fluoride-chlorotrifluoroethylene)P(VDF-CTFE)The molar ratio of Cl atoms is 2.2:1, after the reductant is dissolved by magnetic stirring, continue to stir and react at room temperature for 20 hours;

[0036] Described solvent is tetrahydrofuran;

[0037] The reducing agent is NaBH 4 ;

[0038] Step 2: Pour the final solution obtained in step 1 into a...

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Abstract

The invention discloses a method for preparing poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene). The method comprises the following steps of: adding poly(vinylidene fluoride-chlorotrifluoroethylene) into a three-neck bottle, adding a solvent simultaneously, adding a reducing agent after the poly(vinylidene fluoride-chlorotrifluoroethylene) is fully dissolved, and continually stirring and reacting at the room temperature for 16-24 hours; and pouring an obtained solution into a beaker filled with hydrochloric acid of which the pH is 3, stirring for 1 hour, precipitating a polymer out, repeatedly washing the obtained polymer to whiteness with methanol, and performing vacuum drying under the condition that the temperature is not higher than 60 DEG C to constant weight to obtain a target product. In the method, poly(vinylidene fluoride-trichloroethylene) or poly(vinylidene fluoride-chlorotrifluoroethylene-trichloroethylene) is synthesized by taking poly(vinylidene fluoride-chlorotrifluoroethylene) as a raw material with a one-step process; the method is easy to operate and control; an adopted reaction system has the advantages of low cost and friendliness to human bodies and environment; and the reducing agent is easy to remove from a polymer.

Description

technical field [0001] The invention relates to a new hydrogenation reduction reaction method of fluorine-containing polymers, in particular to a method for preparing poly(vinylidene fluoride-trifluoroethylene) by reduction of poly(vinylidene fluoride-trifluoroethylene) P(VDF-CTFE) P(VDF-TrFE) or poly(vinylidene fluoride-chlorotrifluoroethylene-trifluoroethylene)P(VDF-CTFE-TrFE) method. Background technique [0002] Polyvinylidene fluoride (PVDF) and its copolymer with trifluoroethylene (P(VDF-TrFE)) have excellent dielectric, ferroelectric, piezoelectric and other properties. Since it was reported in the 1900s, PVDF and its copolymers have been widely used in electrical insulation, microelectronic devices, sensors and other fields. In order to realize the application of such materials in energy storage capacitors, in 1998, Professor QM Zhang of Pennsylvania State University used the electron radiation method (Science.1998, 280, 2101-2104.), in P(VDF-TrFE) crystal The intr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/22C08F214/24C08F8/04
Inventor 张志成朱智刚
Owner 陕西德天励成新材料科技有限公司
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