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Microporous polymer film containing cross-linked super branched molecule and its prepn

A hyperbranched polymer and microporous membrane technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc. problem, to achieve the effect of good biocompatibility, long-lasting hydrophilicity, and enhanced strength

Inactive Publication Date: 2006-05-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the grafted hydrophilic groups tend to move into the membrane matrix under the force of the chain movement, the hydrophilicity of the membrane will gradually decrease with the prolongation of use time.
(3) Surface cross-linking polymerization: that is, coating the surface of the microporous membrane with a hydrophilic monomer or prepolymer (initiator can also be used at the same time) that can undergo cross-linking reaction, and then use ultraviolet light, heat or high-energy rays to initiate Polymerization, forming an ultra-thin cross-linked layer on the surface of the membrane (such as US patents 4,618,533, 5,137,633, 5,286,382, 5,629,804), but it is easy to produce the problem of membrane pore blockage caused by surface polymerization cross-linking
[0007] At present, there is no report on the preparation of hydrophilic microporous membranes by using the casting solution containing cross-linked hydrophilic polymers and the phase inversion process. In fact, this method is suitable for the preparation of hydrophilic blended polymer microporous membranes. There are few hydrophilic cross-linked polymer systems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Example 1: BTDA cross-linked G3-DPAA-NH 2 Preparation of / PES microporous membrane

[0085] 14g PES (RADEL  A100, Solvay Advanced Polymers, L.L.C), 8g amino-terminated poly(amide-amine) molecule G3-DPAA-NH synthesized by step-by-step 2 and 85ml of anhydrous DMF were stirred at 45°C for 10 hours to dissolve; 1.2g of cross-linking agent 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA, Beijing Institute of Gas and Coal Chemical Industry), was added, Stir at 40°C for 5 hours and 150°C for 5 hours for cross-linking reaction; then add 5g of PVP (K60, China Pharmaceutical Group Shanghai Chemical Reagent Company) and stir at 40°C for 10 hours; Filter through polyester filter cloth, and vacuum degas at 25°C for 5 hours to obtain a uniform and transparent casting solution. In an air environment at 30°C and a relative humidity of 90%, put the casting solution at 30°C on a clean stainless steel plate with a scraper with a blade depth of 400 μm to scrape the casting sol...

Embodiment 2

[0094] Example 2: Preparation of glutaraldehyde crosslinked G5-HPAE-OH / PVDF microporous membrane

[0095] Add 14g of PVDF (FR904, Shanghai 3F), 8g of G5-HPAE-OH synthesized by the quasi-one-step method to 70ml of DMAC, heat and stir in a water bath at 70°C for 24 hours; then add 1.2g of glutaraldehyde (GA), 70 Conduct crosslinking reaction at ℃ for 5 hours, then raise the temperature to 100℃ and crosslinking reaction for 8 hours; cool to room temperature, filter with a polyester filter cloth with a pore size of 45 μm, and vacuum degas at 25℃ for 10 hours to obtain a uniform and transparent casting film liquid. In an air environment at 25°C and a relative humidity of 70%, put the casting solution at 30°C on a clean glass plate with a scraper with a blade depth of 250 μm to scrape the casting solution into a primary liquid film with uniform thickness. After staying for 20 seconds, the liquid film was immersed in water at 25°C for 100 seconds, and then the liquid film solidified...

Embodiment 3

[0097] Example 3: Preparation of Succinic Acid Crosslinked G5-HPAE-OH / PVDF Microporous Membrane

[0098] Add 14g PVDF (FR904, Shanghai 3F), 8g one-step synthesized hydroxyl-terminated G5-HPAE-OH into 65ml NMP solvent, stir at 80°C for 35 hours to dissolve; then add 0.9g succinic acid (BDAC) (Anqinghe Xing Chemical Company) as a crosslinking agent, stirred and reacted at 140°C for 40 hours; cooled to room temperature, filtered with a polyester filter cloth with a pore size of 45 μm, and vacuum degassed for 4 hours at 25°C to obtain a uniform and transparent casting solution. In an air environment at 25°C and a relative humidity of 83%, put the casting solution at 30°C on a clean glass plate and use a scraper with a blade depth of 300 μm to scrape the casting solution into a primary liquid film with uniform thickness. After staying for 35 seconds, the liquid film was immersed in an aqueous solution containing 10% NMP at 25° C. for 200 seconds and solidified to form a film. The ...

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Abstract

The present invention is one kind of microporous polymer film containing cross-linked super branched molecule and its preparation. The hydrophilic microporous film is prepared with casting solution containing cross-linked water-base polymer and through phase conversion, and the preparation process includes the steps of: preparing casting solution, scraping film, curing in solidification bath and drying. The microporous film has excellent hydrophilicity. In the same time, owing to the interpenetration and twisting of the linear polymer inside the film on the super branched molecules and the cross-linking of super branched molecules, the super branched molecules will not dissolve and migrate from the film, resulting in high film strength. The film forming process of the present invention has low viscosity of the casting solution and easy filming.

Description

technical field [0001] The invention relates to a polymer microporous separation membrane material and its preparation technology, and specifically provides a polymer microporous membrane containing cross-linked hyperbranched molecules and a preparation method thereof. Background technique [0002] Membrane separation technology is of great significance in the fields of chemical industry, energy, environmental protection, medical treatment, and pharmaceuticals. The "membrane" is the starting point and core of membrane separation technology and the main content of membrane separation technology research and development. Membrane materials used in membrane separation technology are mainly polymer materials, such as modified cellulose, polysulfone, polyolefin, polyamide, polycarbonate, acrylic copolymer, fluoropolymer, polyimide, silicone rubber, etc. . Membranes made of these polymers are currently the most used and widely used membranes. They are used in membrane processes s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D67/00B01D69/06B01D71/78
Inventor 朱宝库魏秀珍徐又一
Owner ZHEJIANG UNIV
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