Method for preparing temperature-sensitive polyvinylidene fluoride intelligent membrane material and its product

A polyvinylidene fluoride and smart membrane technology, which is applied in the preparation of temperature-sensitive polyvinylidene fluoride smart membrane materials and its products, can solve the problems of reduced membrane flux, PNIPA swelling degree, and membrane pore changes. Raw membrane filtration level and other issues, to achieve the effect of simple process, easy industrial implementation, and prevent shedding

Inactive Publication Date: 2006-03-08
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the prior art, the method of PVDF surface modification is used to prepare PVDF smart membranes. The disadvantage is that the grafted polymers are easy to fall off. Reduce the flux of the membrane and change the filtration level of the original membrane
The phase transition method is used to prepare PVDF smart membranes. Although parameters such as PVDF membrane pore size and porosity can be controlled by conditions such as stock solution concentration, coagulation bath, and temperature, when preparing PVDF graft copolymers, the reaction conditions, grafting rate, etc. , the molecular structure and molecular weight are difficult to control, so it is very difficult to study the swelling degree of PNIPA and the change of membrane pores
The applicant's previous patent application (200410019992.9) also involves the preparation method of temperature-sensitive PVDF smart film, but this method also has the problem that the smart layer is easy to fall off.

Method used

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Examples

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preparation example Construction

[0018] The preparation method of a temperature-sensitive polyvinylidene fluoride intelligent membrane designed by the present invention uses N-isopropylacrylamide as a grafting monomer, polyvinylidene fluoride as a macromolecular initiator, and cuprous chloride As a catalyst, 4,4 dimethyl 2,2 bipyridine is used as a ligand, and the method of atom transfer free radicals is used to prepare a temperature-sensitive PVDF graft copolymer, that is, a temperature-sensitive polyvinylidene fluoride smart membrane. It includes the following steps:

[0019] 1. Add polyvinylidene fluoride with a weight ratio of 7-13% and solvent N-methyl-2-pyrrolidone into a reaction kettle equipped with a thermometer and agitator, and heat to 50°C to completely dissolve it;

[0020] 2. Then add the graft monomer N-isopropylacrylamide, the molar ratio of which to cuprous chloride is 2000:1-2500:1, fill with nitrogen for 30 minutes under stirring, and then add 0.20-0.25g of Ligand 4,4-dimethyl 2,2-bipyridi...

Embodiment 1

[0028] 1 Add 5g of PVDF and 70mL of solvent N-methyl-2-pyrrolidone into a three-necked flask equipped with a thermometer and a stirrer, and heat to 50°C to dissolve completely;

[0029] 2 Then add 10g of grafted monomer NIPA, fill with nitrogen for 30 minutes under stirring, then add 0.25g of ligand 4,4-dimethyl 2,2-bipyridine, 0.04g of cuprous chloride, stir and heat to 120°C , constant temperature reaction for 18 hours.

[0030] 3 Then wash the reaction product with pure water to obtain a light brown solid, filter it, and dry it at 80°C to obtain a temperature-sensitive PVDF smart membrane product.

Embodiment 2

[0032] 1 Put 6g of polyvinylidene fluoride (PVDF) and 60mL of solvent N-methyl-2-pyrrolidone in a three-necked flask equipped with a thermometer and a stirrer, and heat to 50°C to completely dissolve it.

[0033] 2 Then graft monomer NIPA 10g, fill with nitrogen gas for 20 minutes under stirring, then add ligand 4,4-dimethyl 2,2-bipyridine 0.20g, cuprous chloride 0.04, stir and heat to 80°C, constant temperature React for 18 hours.

[0034] 3 Same as embodiment 1

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PUM

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Abstract

This invention relates to a method for prparing temperature-sensitive polyvinylidene flourine intelligent membrane. The method is: NIPA as grafted monomer, PVDF as macromelocular initiator, cuprous chloride as catalyst,4,4 demethyl 2,2 bipyridine as ligand, using atom transfer free radical process, preparation of temperature-sensitive polyvinylidene flourine intelligent membrane comprising: in reaction kettle, adding 7-13% PVDF(WT%) and solvent N-methyl-2-pyrrolidone,heating to 50 deg. C to make it solve completely; then adding grafted monomer NIPA, its mol ratio with cuprous chloride is 2000:1-2500:1,filling nitrogen gas 30mins. at stirring, and separately adding 0.20-025g ligand 4,4-dimethyl 2,2-bipyridine and 0.04-0.06g catalyst cupous chloride, stirring and heating to 80-120deg.C,constant reaction 19-25 hrs; then washing reaction product using pure water to obtain light brown solid, filtering and 80 C degree drying to obtain finish product.

Description

technical field [0001] The invention relates to a membrane material preparation method and product technology, in particular to a temperature-sensitive and temperature-responsive N-isopropylacrylamide (NIPA) graft copolymerized with polyvinylidene fluoride (PVDF) The preparation method and products of type polyvinylidene fluoride intelligent membrane material belong to the field of functional polymer materials, and the international patent classification number is proposed to be Int.Cl 7 C08F 20 / 54. Background technique [0002] Membrane is the core of membrane technology. The chemical properties of the membrane material and the membrane structure play a decisive role in the membrane separation process. Membrane materials must have the following basic functions: good selective permeability; certain hydrophobicity or hydrophilicity; excellent chemical resistance and biodegradation resistance, which can be used for a long time without deterioration; good heat resistance; Me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F259/06C08J5/18
Inventor 陈莉王闻宇
Owner TIANJIN POLYTECHNIC UNIV
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