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In-situ preparation method of Al(Zr)-PVDF (polyvinylidene fluoride) hybrid film

An in-situ preparation and hybrid membrane technology, which is applied in the field of membrane separation, can solve the problems of high control cost, difficult hydrolysis reaction, and limited application, and achieve the effect of low equipment requirements, remarkable hydrophilic performance, and easy operation

Inactive Publication Date: 2013-03-13
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the problems of complicated operation, difficult control of hydrolysis reaction and high cost, which limits its application in the preparation of inorganic / organic composite membranes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] First, ultrasonically dissolve 1 g of zirconium oxychloride in 100 g of N,N-dimethylformamide, then add a certain amount of 201×7 resin for ion exchange, when the Cl in N,N-dimethylformamide - OH on the resin - After the exchange is complete, the anion exchange resin in the solvent is filtered off to obtain an organic solvent sol system in which zirconium species are uniformly dispersed. The PVDF polymkeric substance of 18g is dissolved in the obtained organosol, obtains uniform, transparent casting film liquid, at 70 o After standing at C for 4 hours for degassing, scrape flat membrane at room temperature, place it in the air for 30 seconds, and then immerse it in a coagulation bath completely composed of deionized water. After soaking for 24 hours, the formed Zr-PVDF ultrafiltration membrane is re- After soaking in glycerin solution for 4h, air-dry naturally. The nanoparticles in the obtained film are uniformly distributed, and the particle diameter is 10-20nm. The...

Embodiment 2

[0022] First, ultrasonically dissolve 1.5g of zirconium oxychloride in 100g of N,N-dimethylformamide, then add a certain amount of 201×7 resin for ion exchange, when the Cl in N,N-dimethylformamide - OH on the resin - After the exchange is complete, the anion exchange resin in the solvent is filtered off to obtain an organic solvent sol system in which zirconium species are uniformly dispersed. The PVDF polymkeric substance of 18g is dissolved in the obtained organosol, obtains uniform, transparent casting film liquid, at 70 o After standing at C for 4 hours for degassing, scrape flat membrane at room temperature, place it in the air for 30 seconds, and then immerse it in a coagulation bath completely composed of deionized water. After soaking for 24 hours, the formed Zr-PVDF ultrafiltration membrane is re- After soaking in glycerin solution for 4h, air-dry naturally. The nanoparticles in the obtained film are uniformly distributed, and the particle diameter is 10-20nm. The...

Embodiment 3

[0024] First, ultrasonically dissolve 2g of aluminum chloride in 100g of N,N-dimethylformamide, then add a certain amount of 201×7 resin for ion exchange, when the Cl in N,N-dimethylformamide - OH on the resin - After the exchange is complete, the anion exchange resin in the solvent is filtered off to obtain an organic solvent sol system in which zirconium species are uniformly dispersed. The PVDF polymkeric substance of 18g is dissolved in the obtained organosol, obtains uniform, transparent casting film liquid, at 70 o After standing for 4 hours at C for degassing, scrape a flat membrane at room temperature, place it in the air for 30 seconds, and then immerse it in a coagulation bath completely composed of deionized water. After soaking for 24 hours, the formed Al-PVDF ultrafiltration membrane is re- After soaking in glycerin solution for 4h, air-dry naturally. The nanoparticles in the obtained film are uniformly distributed, and the particle diameter is 10-20nm. The con...

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Abstract

The invention discloses an in-situ preparation method of an Al(Zr)-PVDF (polyvinylidene fluoride) hybrid film. According to the method, an anion-exchange resin is introduced into an organic solvent system, an inorganic salt of Al(Zr) is adopted as a raw material, and negative ions of the inorganic salt are exchanged with OH- ions provided by the anion-exchange resin to produce an organic solvent sol system in which inorganic substances are uniformly dispersed; and then, PVDF (polyvinylidene fluoride) is dissolved in the obtained organic sol to produce a uniform and transparent film casting solution; and finally the film casting solution stands still and is subjected to film scraping and gelatinization to produce an Al(Zr)-containing PVDF composite film. The method integrates the in-situ preparation process and the phase-inversion film-forming process of nanoparticles, and solves the technical problems of the nanoparticle filling process in the prior art, such as high probability of nanoparticle aggregation and poor dispersion of hydrophilic particles in a hydrophobic polymer matrix. The composite film product has the advantages that the nanoparticles have small particle diameters and are uniformly dispersed and the hydrophilicity is greatly improved.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, in particular to a method for preparing an Al(Zr)-PVDF hybrid membrane in situ. Background technique [0002] Since 1996 Doyen W and I.Genne put ceramic ZrO 2 Since the powder is filled into polysulfone and the oxide / polymer composite membrane is prepared by the phase inversion process, the research and development of the inorganic / organic composite membrane that introduces inorganic nanoparticles into the organic membrane has become an important research direction in this field. and development trends. The inorganic / organic composite membrane not only combines the characteristics of good flexibility and film-forming performance of the organic membrane, but also the characteristics of high mechanical strength, good stability, chemical and biological erosion resistance, long service life, anti-fouling and easy cleaning of the inorganic membrane. Moreover, it makes up for the poor me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/34B01D69/14B01D67/00
Inventor 李健生王连军庞睿智陆庄羽孙秀云韩卫清刘晓东
Owner NANJING UNIV OF SCI & TECH