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Preparation method of thermal cross-linked polymer separation membrane and application thereof

A polymer and separation membrane technology, which is applied in separation methods, semipermeable membrane separation, and dispersed particle separation, can solve problems such as yield loss and nanoporous transition layer collapse, and achieve energy saving and separation selectivity coefficient improvement. , The effect of simple synthesis process

Active Publication Date: 2022-02-25
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although asymmetric membranes with defect-free thin selective layers can also be decarboxylated and cross-linked, such heat treatment temperatures above the glass transition temperature of polyimide easily lead to the collapse of the nanoporous transition layer, resulting in a 2–4 ​​fold yield loss
High-temperature reaction conditions for decarboxylation and cross-linking make it challenging to develop stable commercial separation membranes with high selectivity coefficients

Method used

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  • Preparation method of thermal cross-linked polymer separation membrane and application thereof
  • Preparation method of thermal cross-linked polymer separation membrane and application thereof
  • Preparation method of thermal cross-linked polymer separation membrane and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Synthesis of DUPI: Add 30mmol of benzyldiamine monomer to a three-necked flask equipped with a magnetic stirrer, under nitrogen protection, add an appropriate amount of ultra-dry N-methylpyrrolidone solvent, stir until all solid powder is dissolved, then add 30mmol 4,4'-(hexafluoroisopropylidene) diphthalic anhydride, adding ultra-dry N-methylpyrrolidone solvent to obtain a homogeneous mixed solution with a mass concentration of 20 wt%, and stirring for prepolymerization for 12 hours. During this process, dianhydride and diamine undergo a condensation reaction to open the ring to form polyamic acid. Subsequently, 5-10 mL of anhydrous toluene was added to the system, and a water separator and a spherical condenser were installed on the side neck of the three-necked flask. The water generated in the imine process is removed by azeotropic distillation with toluene, and the reaction proceeds forward. After the reaction was completed, the viscous reaction product solution w...

Embodiment 2

[0047] The benzyl polyimide synthesis method and film preparation method are the same as in Example 1, except that the temperature of thermal oxygen treatment is 300° C. for 5 hours. Among them, the hydrogen permeability coefficient of this type of membrane can reach 330 Barrer, the hydrogen methane separation selectivity coefficient can reach 85, the carbon dioxide permeability coefficient can reach 200 Barrer, and the carbon dioxide methane selectivity coefficient can reach 50.

Embodiment 3

[0049] The benzyl polyimide synthesis method and film preparation method are the same as in Example 1, except that the temperature of thermal oxygen treatment is 300° C. for 10 h. Among them, the hydrogen permeability coefficient of this type of membrane can reach 330 Barrer, the hydrogen methane separation selectivity coefficient can reach 85, the carbon dioxide permeability coefficient can reach 200 Barrer, and the carbon dioxide methane selectivity coefficient can reach 50.

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Abstract

The invention provides a preparation method of a thermal cross-linked polymer separation membrane and an application thereof. According to the method, the stable covalent cross-linked polyimide film is prepared by thermal oxidation cross-linking, and the method has the advantages of mild reaction temperature, main chain integrity maintenance, excellent plasticizing resistance and the like. According to the invention, a strategy of dehydrogenation of a methyl substituent group on an oxygen-induced benzene ring is established, so that a cross-linked network is constructed in a benzyl polyimide system under a mild condition, and the cross-linked membrane has higher chain stacking density, so that the cross-linked membrane has very excellent plasticizing resistance even under a high-pressure CO2 feeding condition. The method is expected to be used in the molecular separation fields of gas separation, organic nanofiltration and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer separation membranes, and in particular relates to a preparation method and application of a heat-crosslinked polymer separation membrane. Background technique [0002] Biogas is an environmentally friendly energy produced by the fermentation of organic matter. Compared with coal, oil, shale gas and other energy sources, its green economic feasibility is superior, and it can achieve carbon "zero emission". It is of great significance to study the separation and purification of biogas with complex components. In addition, carbon dioxide (CO 2 ) and methane (CH 4 ) two components, CO 2 It not only reduces the calorific value of natural gas, but also easily corrodes the transportation pipeline. Therefore, the study of CO in biogas 2 and CH 4 It is also very important to obtain energy with high calorific value. Compared with traditional heat-driven separation processes, polymer gas separation m...

Claims

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Application Information

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IPC IPC(8): C08J3/24C08L79/08C08G73/10B01D53/22B01D69/02B01D61/02
CPCC08G73/1007C08G73/1039C08G73/1067C08J3/247B01D53/228B01D69/02B01D61/027C08J2379/08
Inventor 王正宫靳健
Owner SUZHOU UNIV
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