Green preparation method of polyimide gas separation membrane

A technology of gas separation membrane and polyimide, which is applied in separation methods, gas treatment, semi-permeable membrane separation, etc., to achieve the effects of increasing flux, good affinity and improving selectivity

Active Publication Date: 2017-11-24
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of green preparation method of polyimide gas separation membrane, to overcome the defective of existing polyimide membrane preparation technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of green preparation method based on polyimide gas separation membrane, comprises the steps, and described formula proportion is by weight:

[0020] A. Synthesis of water-soluble polyimide: Weigh 5 parts of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and dissolve it in 15 parts of N-methylpyrrolidone, in a nitrogen atmosphere After dissolving in the medium for 1 hour, add 5 parts of pyromellitic dianhydride, react in an ice-water bath for 3 hours, add 20 parts of benzene, reflux at 180°C for 6 hours, cool to room temperature, wash 3 times with deionized water, 150°C Oven drying to obtain hydroxyl polyimide; after dissolving 10 parts of hydroxyl polyimide in 30 parts of N,N-dimethylformamide, add 1.5 parts of p-fluorobenzoic acid and 10 parts of K 2 CO 3 , react at 56°C for 20 hours, dissolve the product in a mixed solution of methanol and dichloromethane with a volume ratio of 3:1 for recrystallization, and obtain a water-soluble polyimide;

[0021] B. Pr...

Embodiment 2

[0024] A kind of green preparation method based on polyimide gas separation membrane, comprises the steps, and described formula proportion is by weight:

[0025] A. Synthesis of water-soluble polyimide: Weigh 10 parts of 9,9-bis(3-amino-4-hydroxyphenyl)fluorene and dissolve in 30 parts of N-methylpyrrolidone, and dissolve in nitrogen atmosphere for 1h Finally, add 10 parts of phthalic dianhydride, react in an ice-water bath for 3 hours, add 20 parts of toluene, reflux at 180°C for 6 hours, cool to room temperature, wash with deionized water three times, and dry in an oven at 150°C. To obtain hydroxyl polyimide; after dissolving 10 parts of hydroxyl polyimide in 30 parts of N,N-dimethylformamide, add 2.5 parts of 4-fluorobenzenesulfonic acid and 20 parts of K 2 CO 3 , react at 56°C for 20h, dissolve the product in a mixed solution of methanol and dichloromethane with a volume ratio of 2:1 for recrystallization, and obtain a water-soluble polyimide;

[0026] B. Preparation of...

Embodiment 3

[0029] A kind of green preparation method based on polyimide gas separation membrane, comprises the steps, and described formula proportion is by weight:

[0030] A. Synthesis of water-soluble polyimide: Weigh 5 parts of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane and dissolve it in 15 parts of N-methylpyrrolidone, in a nitrogen atmosphere After dissolving in the medium for 1 hour, add 5 parts of hexafluorodianhydride, react in an ice-water bath for 3 hours, add 20 parts of xylene, reflux at 180°C for 6 hours, cool to room temperature, wash 3 times with deionized water, and dry in an oven at 150°C Dry to obtain hydroxyl polyimide; after dissolving 10 parts of hydroxyl polyimide in 30 parts of N,N-dimethylformamide, add 3.5 parts of 4-fluorobenzenesulfonic acid and 20 parts of K 2 CO 3 , react at 56°C for 20 hours, dissolve the product in a mixed solution of methanol and dichloromethane with a volume ratio of 1:1 for recrystallization, and obtain a water-soluble polyimid...

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Abstract

The invention belongs to the technical field of membrane separation and in particular relates to a green preparation method of a polyimide gas separation membrane. The membrane preparation process comprises the following process steps: (1) synthesis of water-soluble polyimide: dissolving the prepared hydroxypolyimide in N,N-dimethylformamide, adding a sulfonation or carboxylation reagent and K2CO3, reacting at the temperature of 56 DEG C for 20 hours, and dissolving a product in a mixed solution of methanol and dichloromethane for recrystallization, so as to obtain water-soluble polyimide; (2) preparation of a polyimide gas separation membrane: taking water as a solvent, dissolving the water-soluble polyimide in water to prepare a casting solution, uniformly performing knife coating on a tetrafluoroethylene plate, standing at a room temperature for 12 hours, and drying in a drying oven at the temperature of 50 DEG C for 6 hours, thereby obtaining the product polyimide gas separation membrane. According to the method disclosed by the invention, the organic solvent is replaced with water for film mulching in the film preparation process based on a green film preparation technology, so that no volatile organic vapor is produced. The prepared polyimide gas separation membrane is excellent in permeability of CO2 gas and high in separation factor of CO2/N2.

Description

technical field [0001] The invention belongs to the field of high-tech and gas separation membrane preparation, and in particular relates to a green preparation method of polyimide gas separation membrane. Background technique [0002] In recent years, due to human activities such as coal, oil, natural gas and other fossil fuel combustion and motor vehicle exhaust, the "greenhouse effect" has become increasingly serious, global warming, sea level rise, earth diseases and insect pests, endangered biological species, land drought, desertification, etc. Environmental problems are becoming increasingly prominent. CO 2 It is the main greenhouse gas, contributing as much as 76% to the greenhouse effect. Therefore, separation and recovery of CO from combustion exhaust 2 It is an important way to slow down the greenhouse effect. In addition to environmental protection requirements, CO 2 The separation of gas is also closely related to the needs of many industrial processes, suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/64B01D69/02B01D53/22
CPCB01D53/228B01D69/02B01D71/64B01D2257/504
Inventor 张春芳尹松虎刘会影崔晓晨
Owner JIANGNAN UNIV
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