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Method for carrying out controllable hydrophilic modification on polyvinylidene fluoride (PVDF)

A polyvinylidene fluoride and hydrophilic modification technology, applied in the field of polymer modification, can solve problems such as complicated operation, and achieve the effects of simplified synthesis steps, good biocompatibility, and convenient industrial production.

Inactive Publication Date: 2010-08-04
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the operation is more complicated

Method used

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  • Method for carrying out controllable hydrophilic modification on polyvinylidene fluoride (PVDF)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Using PVDF 400k Synthesis of the graft copolymer PVDF-g-PDMAEMA as initiator

[0027] 0.4g of PVDF 400k Dissolve in 2mL of NMP, and then place it in an oil bath at 50°C for rapid dissolution. After it is completely dissolved, cool to room temperature and add 11.6mg FeCl 3 .6H 2 O, 22.5mg PPh 3 , 2.5mL of DMAEMA, finally add 15.2mg of VC, directly seal the tube at room temperature, put it in an oil bath at 90℃ for 15 hours, take the tube into cold water, and then precipitate the polymer in a mixture of petroleum ether and ethanol In the precipitating agent, the obtained polymer was dried in a vacuum oven at room temperature for 24 hours after filtration and repeated washing with methanol, and the grafting rate of the obtained polymer PDMAEMA was 67%.

Embodiment 2

[0028] Example 2: Using PVDF 400k Synthesis of PPEGMA graft copolymer PVDF-g-PPEGMA as initiator

[0029] 0.3g PVDF 400k Dissolve in 2mL of NMP, and then place it in an oil bath at 50°C for rapid dissolution. After it is completely dissolved, cool to room temperature and add 11.6mg (0.043mmol) of FeCl 3 .6H 2 O, 22.5mg (0.086mmol) PPh 3 , A certain amount of PEGMA (see Table 1 for specific amount), finally add 15.2mg (0.086mmol) of VC, directly seal the tube at room temperature, put it in an oil bath at 90°C for a certain period of time, then take the tube and put it into cold water. The polymer was then precipitated in a mixed precipitation agent of petroleum ether and ethanol, filtered and washed repeatedly with methanol, and the resulting polymer was dried in a vacuum oven at room temperature for 24 hours.

[0030] Table 1. The effect of different polymerization time and different ratio on the grafting rate of polymer

[0031] Entry

PEGMA / PVDF 400k

Time(h)

Graft%

1

...

Embodiment 3

[0035] Example 3: Using PVDF 71k Synthesis of PPEGMA graft copolymer PVDF-g-PPEGMA as initiator

[0036] 0.3g PVDF 71k Dissolve in 2mL of NMP, and then place it in an oil bath at 50°C for rapid dissolution. After it is completely dissolved, after cooling to room temperature, add 11.6mg (0.043mmol) of FeCl 3 .6H 2 O, 22.5mg (0.086mmol) PPh 3 , 2.5mL (8.7mmol) of PEGMA, finally add 15.2mg (0.086mmol) of VC, directly seal the tube at room temperature, put it in an oil bath at 90°C for a certain period of time, take the tube into cold water, and then polymerize Precipitate in a mixed precipitation agent of petroleum ether and ethanol, filter and repeatedly wash with methanol, and dry the obtained polymer in a vacuum oven at room temperature for 24 hours.

[0037] Table 2. The effect of different polymerization time on polymer grafting rate

[0038] Entry

[0039] It can be seen from Table 2 that extending the reaction time of AGET ATRP, the grafting rate of the polymer on PVDF contin...

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Abstract

The invention discloses a method for carrying out controllable hydrophilic modification on polyvinylidene fluoride (PVDF). The method comprises the following steps of: (1) preparing a polymerization system according to a molar ratio of monomers to polyvinylidene fluoride of (2000-15000):1 and dissolving the polymerization system in an organic solvent, wherein the polymerization system comprises monomers, the PVDF, a catalyst, a coordination agent and a reducing agent; (2) sealing under air atmosphere and carrying out AGET (Activators Generated by Electron Transfer) ATRP (Atom Transfer Radical Polymerization) polymerization catalyzed by an iron salt at 90-120 DEG C; and (3) separating an obtained polymer. In the polymerization system, the monomers are selected from one of methylacrylic acid polyethylene glycol monomethyl ether ester, methacrylic acid-N,N-dimethylamino ethyl ester or hydroxyethyl methacrylate. After the AGET ATRP reaction catalyzed by the iron salt is carried out, PVDF-g-PPEGMA (polyethylene-polypropylene glycol methacrylate), PVDF-g-PDMAEMA (poly((2-Dimethylamino)ethyl methacrylate) and PVDF-g-PHEMA (polyhydroxyethyl methacrylate) are correspondingly obtained. The invention can regulate the molecular weight of a graft polymer and the molecular weight of the PVDF through regulating the time of the polymerization reaction so as to control the size of the aperture of a PVDF film, and meanwhile, the property of the polymer can be regulated through changing the category of the monomers so as to change the property of a final PVDF film.

Description

Technical field [0001] The invention belongs to the field of polymer modification, and specifically relates to a method for controllable hydrophilic modification of polyvinylidene fluoride. Background technique [0002] Polyvinylidene fluoride (PVDF) is a new type of polymer material with excellent properties. It has excellent UV resistance, weathering resistance, excellent electrical properties, heat resistance, mechanical properties, radiation resistance and chemical stability. It is white crystalline, crystallinity is 60%~80%, fluorine content is 59.6%, density is 1.75~1.78g / cm 3 , Water absorption rate <0.04%, glass transition temperature -39℃. The embrittlement temperature is below -62°C, the crystalline melting point is about 170°C, and the thermal decomposition temperature is greater than 316°C. The processing temperature range from melting point to decomposition temperature is wide, and it can still maintain good strength under certain temperature and pressure, and t...

Claims

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Application Information

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IPC IPC(8): C08F259/08C08F4/26C08F2/00
Inventor 程振平赵涛朱秀林张丽芬张正彪周年琛
Owner SUZHOU UNIV
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