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Preparation method of high-throughput graphene oxide/polyimide mixed matrix membrane material

A technology of mixed matrix membrane and polyimide matrix, which is applied in the field of preparation of high-throughput graphene oxide/polyimide mixed matrix membrane materials, can solve the problems of poor temperature resistance, poor plasticization resistance, and poor separation performance. Limit and other issues, to achieve the effect of high operating temperature, stable chemical structure, and broad application prospects

Active Publication Date: 2018-01-09
UNIV OF SCI & TECH LIAONING +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The invention provides a method for preparing a high-throughput graphene oxide / polyimide mixed matrix membrane material. The prepared mixed matrix gas separation membrane material has the characteristics of excellent permeation and separation performance and stable chemical structure, and solves the existing problems. Polymer separation membrane materials have limited separation performance, poor plasticization resistance, and poor temperature resistance.

Method used

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  • Preparation method of high-throughput graphene oxide/polyimide mixed matrix membrane material

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Embodiment 1

[0039] First, aminated graphene was prepared according to conventional methods. Add a certain amount of aminated graphene and N,N-dimethylacetamide into a 250mL three-necked round-bottomed flask, and vibrate for 2 hours under the action of ultrasonic waves. Then, 0.01 mol of bis(3-hydroxy-4-aminophenyl)diphenylmethane was added, and reacted at 40° C. for 16 hours under mechanical stirring and nitrogen protection. After cooling down to room temperature, add 0.01mol 4,4'-(hexafluoroisopropylidene) diphthalic anhydride (6FDA), and continue to stir at room temperature for 18 hours to form a viscous aminated graphene / polyamic acid mixed solution. The solid content was 15% by weight. The solution was uniformly coated on a clean glass plate, and dried in a far-infrared drying oven at 80° C. and 150° C. for 6 hours respectively to obtain a composite material film. The content of aminated graphene in the composite film is 0.1wt%.

[0040] The composite material film containing 0.1wt...

Embodiment 2

[0042] First, aminated graphene was prepared according to conventional methods. Add a certain amount of aminated graphene and N,N-dimethylacetamide into a 250mL three-necked round-bottomed flask, and vibrate for 2 hours under the action of ultrasonic waves. Then, add 0.01mol 9,9-bis(4-aminophenyl)fluorene and 0.01mol 9,9-bis(3-amino-4-hydroxyphenyl)fluorene, and react at 70°C for 12 Hour. After cooling down to room temperature, add 0.02mol 4,4'-(hexafluoroisopropylidene) diphthalic anhydride (6FDA), and continue to stir at room temperature for 18 hours to form a viscous aminated graphene / polyamic acid mixed solution. The solid content was 15% by weight. The solution was uniformly coated on a clean glass plate, dried at 40°C for 24 hours, then removed, and then dried in a far-infrared oven at 80°C and 150°C for 6 hours to obtain a composite film. The content of aminated graphene in the composite material is 0.5wt%.

[0043] The composite material film containing 0.5wt% amin...

Embodiment 3

[0045] The preparation method of the composite material film in this embodiment is the same as in Example 2, and the difference from Example 2 is that the composite material film containing 0.5wt% aminated graphene is placed in a heating furnace, and nitrogen gas is fed into the gas flow rate. 100ml / min, the furnace temperature is raised to 250°C at 2°C / min, then raised to 550°C at 1°C / min, and maintained at this temperature for 1 hour, and the graphene oxide / polyimide mixture is obtained after natural cooling Matrix membrane material.

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Abstract

The invention relates to a preparation method of high-throughput graphene oxide / polyimide mixed matrix membrane material. The high-throughput graphene oxide / polyimide mixed matrix membrane material isprepared by the steps of introducing graphene oxide into a polyimide matrix subjected to thermotropic rearrangement reaction through an in-situ method to prepare a composite material membrane, and processing the composite material membrane for at least 0.1h under inert atmosphere. The prepared mixed matrix gas separation membrane material has the characteristics of excellent seepage separation performance and stable chemical structure and can solve the inadequate problems of limited separation performance, poor anti-plasticizing capability, poor temperature tolerance and the like of the existing polymer separation membrane material.

Description

technical field [0001] The invention relates to the technical field of gas separation membrane materials, in particular to a preparation method of a high-throughput graphene oxide / polyimide mixed matrix membrane material. Background technique [0002] Compared with traditional separation technology, gas membrane separation technology has the advantages of low energy consumption, no pollution and simple equipment, etc. It is widely used in the fields of natural gas purification, hydrogen recovery, oxygen enrichment, nitrogen enrichment and organic vapor recovery. So far, the gas separation membrane materials that have been commercialized are mainly polymer membrane materials. However, the separation membranes prepared by these polymer membrane materials either have high gas selectivity but low permeability, such as polysulfone, polyethersulfone, polyimide or polyetherimide membrane materials; or High gas permeability and low selectivity, such as silicone rubber membrane mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/64B01D71/02B01D67/00
Inventor 鲁云华肖国勇李琳王同华胡知之侯旻辰郝继璨陈琳
Owner UNIV OF SCI & TECH LIAONING
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