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A method for preparing cross-linked polyacrylonitrile separation membrane by ultraviolet irradiation

A technology of polyacrylonitrile and separation membrane, which is applied in semi-permeable membrane separation, chemical instruments and methods, and membranes. Mild, good mechanical strength effect

Active Publication Date: 2017-11-07
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When preparing a cross-linked separation membrane, the conventional method needs to heat the casting solution for a long time, or soak the membrane material in the cross-linking agent solution for a long time, the preparation efficiency is low, and the structure is difficult to control; or the membrane strength can be improved by partial cross-linking. The uncrosslinked part of the film with this structure is easy to lose, the strength is limited, and it is not resistant to solvents.

Method used

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  • A method for preparing cross-linked polyacrylonitrile separation membrane by ultraviolet irradiation

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Experimental program
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Effect test

Embodiment 1

[0021] 1) Weigh 4.24g acrylonitrile, 0.286g allyl methacrylate, dissolve in 50g dimethyl sulfoxide, then add 0.07g initiator azobisisobutyronitrile and 0.04g chain transfer agent cysteine Hydrochloride, sealed with nitrogen protection, reacted in a water bath at 60°C for 4 hours, precipitated in ethanol, washed with ethanol and water for 3 times, dried in a vacuum oven at 60°C for 6 hours, and obtained the initial product;

[0022] 2) Weigh 0.4g of the initial product and dissolve it in 4.6g of dimethylsulfoxide, and add 10mg of cross-linking agent 3,6-dioxa-1,8-octanedithiol and 15mg of photoinitiator benzoin dimethyl ether to form Scraping liquid, use a 200μm spatula to scrape the film on the glass plate, and immediately put in 10μW / cm 2 After irradiating with ultraviolet light for 300s, the glass plate was transferred to water for phase inversion to form a film. Finally, soak and wash the obtained membrane with water for more than 12 hours to remove impurities such as unre...

Embodiment 2

[0024] 1) Weigh 4.24g of acrylonitrile and 0.143g of allyl methacrylate respectively, and dissolve them in 50g of dimethyl sulfoxide. Then add 0.07g of initiator azobisisobutyronitrile and 0.04g of chain transfer agent cysteamine hydrochloride, seal nitrogen protection, react in a water bath at 60°C for 4h, precipitate in ethanol, and use ethanol and water Washed three times respectively, and dried in a vacuum oven at 60°C for 6 hours to obtain the primary product;

[0025] 2) Weigh 0.4g of the initial product and dissolve it in 4.6g of dimethylsulfoxide, and add 5mg of cross-linking agent 3,6-dioxa-1,8-octanedithiol and 15mg of photoinitiator benzoin dimethyl ether to form Scraping liquid, use a 200μm spatula to scrape the film on the glass plate, and immediately put in 300μW / cm 2 Irradiate under UV light for 30s. Then the glass plate was transferred to water for phase inversion to form a film. Finally, soak and wash the obtained membrane with water for more than 12 hours,...

Embodiment 3

[0027] 1) Weigh 4.24g of acrylonitrile and 0.143g of allyl methacrylate respectively, and dissolve them in 50g of dimethyl sulfoxide. Then add 0.07g of initiator azobisisobutyronitrile and 0.04g of chain transfer agent cysteamine hydrochloride, seal nitrogen protection, react in a water bath at 60°C for 4h, precipitate in ethanol, and use ethanol and water Washed three times respectively, and dried in a vacuum oven at 60°C for 6 hours to obtain the primary product;

[0028] 2) Weigh 0.4g of the initial product and dissolve it in 4.6g of dimethyl sulfoxide, and add 5 mg of cross-linking agent (thioglycolic acid)-1,4-butylene diester and 15 mg of photoinitiator benzoin dimethyl ether to form a scraping solution , scrape the film on the glass plate with a 200μm spatula, and immediately put in 100μW / cm 2 Irradiate under UV light for 150s. Then the glass plate was transferred to water for phase inversion to form a film. Finally, soak and wash the obtained membrane with water for...

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Abstract

The invention discloses a method for preparing a cross-linking polyacrylonitrile separation membrane through ultraviolet radiation. The cross-linking polyacrylonitrile separation membrane is prepared by dissolving acrylonitrile and allyl methacrylate in dimethylsulfoxide, adding an initiator and a chain transfer agent, conducting sealing and nitrogen protection, making the mixture react for 2-6 hours in a water bath kettle with the temperature of 50-70 DEG C, conducting precipitation separation in ethyl alcohol, washing the precipitate with ethyl alcohol and water, putting the precipitate in vacuum to be dried into a primary product, dissolving the primary product in dimethylsulfoxide, adding a cross-liking agent and a light initiator to form membrane wiping liquid, conducting membrane wiping on a glass plate through a scraper of 200 micrometers, and placing the glass plate to be irradiated by ultraviolet light for 30-300 seconds. The method has the advantages that raw materials are easy to obtain, operation is easy, the energy consumption is low, efficiency is high, and modification can be easily conducted. The obtained acrylonitrile cross-linking membrane is excellent in mechanical property and high in solvent resistance. Due to the adoption of the method, copolymerization and modification can be easily conducted on the cross-linking polyacrylonitrile separation membrane and functional monomers to form a hydrophilic or functional acrylonitrile cross-linking separation film, and the cross-linking polyacrylonitrile separation membrane can be recycled after being regenerated and is not likely to cause secondary pollution.

Description

technical field [0001] The invention relates to a method for preparing a cross-linked polyacrylonitrile separation membrane by ultraviolet radiation. Background technique [0002] With the promotion of the application of membrane separation technology in food, medicine, biology, water treatment, etc., the requirements for the stability and separation performance of the membrane are also continuously increasing. Addition of supports and chemical cross-linking are routine methods to improve membrane stability. When preparing a cross-linked separation membrane, the conventional method needs to heat the casting solution for a long time, or soak the membrane material in the cross-linking agent solution for a long time, the preparation efficiency is low, and the structure is difficult to control; or the membrane strength can be improved by partial cross-linking. The uncrosslinked part of the film with this structure is easy to lose, the strength is limited, and it is not resistan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/42B01D67/00
CPCB01D67/0006B01D71/42B01D2323/02B01D2323/30B01D2323/345
Inventor 费正东王涛范萍陈枫杨晋涛钟明强
Owner ZHEJIANG UNIV OF TECH