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Flexible free-standing carbon molecular sieve@graphene composite membrane and preparation method thereof

A graphene composite and carbon molecular sieve technology, applied in separation methods, chemical instruments and methods, membrane technology, etc., can solve problems such as poor thermal and chemical stability, poor mechanical strength, and reduced interlayer spacing, and achieve soft texture.

Active Publication Date: 2017-01-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the existence of pure GO separation membranes: 1. Poor thermal and chemical stability, it is easy to cause irreversible reduction to reduce the interlayer distance and greatly reduce the flux; 2. The structure of the ultra-thin separation layer is difficult to control and has poor mechanical strength. Thickened flux decreases rapidly; 3. The requirements for the support are high, and any defects on the surface will have a great impact on the selectivity of the GO membrane. Therefore, the existing preparation technology cannot be prepared with stable performance. Pure GO membranes, especially gas separation membranes

Method used

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  • Flexible free-standing carbon molecular sieve@graphene composite membrane and preparation method thereof
  • Flexible free-standing carbon molecular sieve@graphene composite membrane and preparation method thereof
  • Flexible free-standing carbon molecular sieve@graphene composite membrane and preparation method thereof

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Effect test

Embodiment 1

[0035] Graphite oxide was added into N,N-dimethylformamide, and ultrasonically dispersed to obtain a 3 mg / mL graphene oxide dispersion. The polyimide prepolymer polyamic acid was added into N,N-dimethylformamide to prepare a 1wt.% PAA solution.

[0036] Preparation of carbon molecular sieve precursor polymer@graphene oxide composite film by solvent evaporation method: mix the graphene oxide dispersion and PAA solution at a volume ratio of 3:1, add it to a polytetrafluoroethylene vessel, and place it horizontally on a constant temperature platform. Evaporated at 50°C for 24 hours to obtain a PAA@graphene oxide composite film. After the PAA@graphene oxide composite film was vacuum-dried at 70 °C for 12 h, it was peeled off from the polytetrafluoroethylene vessel.

[0037] The obtained self-supporting PAA@graphene oxide composite membrane was placed in a carbonization furnace under a nitrogen atmosphere from room temperature at a rate of 3°C / min to 600°C for 1 hour to obtain a f...

Embodiment 2

[0039] Graphite oxide was added into dimethyl sulfoxide and dispersed ultrasonically to obtain a 3 mg / mL graphene oxide dispersion. Add polyaryletherketone into dimethyl sulfoxide to prepare a 5wt.% PEK-C solution.

[0040] Preparation of carbon molecular sieve precursor polymer@graphene oxide composite film by solvent evaporation: mix the graphene oxide dispersion and PEK-C solution at a volume ratio of 15:1, add it to a glass watch glass, and place it horizontally on a constant temperature platform. Evaporate at 100°C for 48 hours to obtain PEK-C@graphene oxide composite film. After the PEK-C@graphene oxide composite film was vacuum-dried at 100 °C for 24 h, it was peeled off from the glass watch glass.

[0041] The obtained self-supporting PEK-C@graphene oxide composite membrane was placed in a carbonization furnace, under an argon atmosphere, from room temperature at a rate of 5°C / min to 700°C, and kept at a constant temperature for 1h to obtain a flexible self-supporting...

Embodiment 3

[0043] Graphite oxide was added into N-methylpyrrolidone and dispersed ultrasonically to obtain a 2 mg / mL graphene oxide dispersion. Add polyaryletherketone to N-methylpyrrolidone to prepare a 15wt.% polyaryletherketone solution.

[0044] Preparation of carbon molecular sieve precursor polymer@graphene oxide composite film by solvent evaporation: mix graphene oxide dispersion and polyaryletherketone solution at a volume ratio of 60:1, add it to a stainless steel vessel, and place it horizontally on a constant temperature platform. Evaporate at 150°C for 12 hours to obtain a polyaryletherketone@graphene oxide composite film. After vacuum-drying the polyaryletherketone@graphene oxide composite film at 150°C for 24 hours, it was peeled off from the stainless steel vessel.

[0045] The obtained self-supporting polyaryletherketone@graphene oxide composite film was raised from room temperature to 550°C at a rate of 3°C / min in a carbonization furnace in a helium atmosphere, and the ...

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Abstract

The invention relates to a flexible free-standing carbon molecular sieve@graphene composite membrane and a preparation method thereof. The flexible free-standing carbon molecular sieve@graphene composite membrane is formed by alternative assembling of graphene and a carbon molecular sieve, has a structure imitating a shell pearl layer and is soft in texture, bendable and independent of any solid support. The flexible free-standing carbon molecular sieve@graphene composite membrane is prepared by high-temperature carbonization of a carbon molecular sieve precursor polymer@oxidized graphene composite membrane formed by alternative assembling of oxidized graphene and a carbon molecular sieve precursor polymer. The flexible free-standing carbon molecular sieve@graphene composite membrane and the preparation method thereof have the advantages that the shortcomings that a carbon molecular sieve membrane is crisp and fragile and needs to depend on a rigid porous support are overcome, and the shortcoming that an oxidized graphene membrane is poor in stability is avoided; the preparation method is simple in technology and wide in applicable range, and the flexible free-standing carbon molecular sieve@graphene composite membrane is high in chemical stability and excellent in gas separation performance.

Description

technical field [0001] The invention relates to a structure and a preparation method of a flexible self-supporting carbon molecular sieve@graphene composite membrane, in particular to a carbon molecular sieve@graphene composite membrane for gas separation and a preparation method thereof. Background technique [0002] Membrane separation technology has technical advantages such as convenience, high efficiency, cleanliness, and energy saving, and has important applications in the fields of chemical industry, energy, environment, biology, and medicine. One of the keys to membrane separation technology is the development of new, high-performance membrane materials. Since its appearance in the 1980s, carbon molecular sieve membrane, as a high-performance inorganic membrane material, not only has good thermal and chemical stability and mechanical properties of inorganic membrane materials (such as: ceramic membrane materials, etc.), but also exhibits Due to its excellent gas per...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D71/02B01D71/68B01D71/50B01D71/36B01D71/34B01D71/42B01D71/12B01D67/00B01D53/22
CPCB01D53/22B01D67/0079B01D69/12B01D71/021B01D71/12B01D71/34B01D71/36B01D71/42B01D71/50B01D71/68
Inventor 王春雷王同华张生义李琳项楠郑天赋孙亚明
Owner DALIAN UNIV OF TECH