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Preparation method for high flux solvent-resisting organic/inorganic hybridized compound film doped with aminated graphene quantum dot

A technique of aminated graphene and hybridization, which is applied in the field of membrane separation, can solve the problems of low flux and achieve the effects of large specific surface area, improved stability and small particle size

Active Publication Date: 2017-11-14
OCEAN UNIV OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the technical problem that the nanofiltration membrane facing the aqueous solution system in the prior art is difficult to be used in the organic solution system, and the organic solvent-resistant nanofiltration membrane prepared by the phase inversion method has a low flux, and proposes a doped A method for preparing a high-throughput solvent-resistant organic / inorganic hybrid composite film of aminated graphene quantum dots (abbreviated as af-GQDs in this field), the prepared organic solvent-resistant organic / inorganic hybrid composite film has excellent Solvent resistance, and has high flux, salt rejection rate and dye removal rate, which greatly improves the performance of the membrane

Method used

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  • Preparation method for high flux solvent-resisting organic/inorganic hybridized compound film doped with aminated graphene quantum dot

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0071] The preparation and purification steps of af-GQDs nanoparticles are as follows,

[0072] Step 1: preparation of graphene oxide;

[0073] Mix a certain amount of graphite powder, concentrated sulfuric acid and sodium nitrate evenly, stir at a temperature of 5°C for 30 minutes, then add an appropriate amount of potassium permanganate, keep the temperature below 20°C, and continue stirring for 2 hours, then the temperature of the mixture Keep at 35°C, keep stirring for 5 hours, then add an appropriate amount of deionized water, raise the temperature of the mixture to 95°C, continue stirring for 40 minutes, add a large amount of deionized water to terminate the reaction, and then add an appropriate amount of hydrogen peroxide solution, at this time The color of the mixture changed from brown-black to bright yellow;

[0074] Step 2: the purification of graphene oxide;

[0075] Add dilute hydrochloric acid to the above mixture to wash and centrifuge, retain the solid, and d...

Embodiment 1

[0091] In Example 1, the difference between the aqueous phase solution and Comparative Example 1: af-GQDs were added to the aqueous phase solution.

[0092] Dissolve the small molecule diamine compound and a certain amount of af-GQDs in deionized water, the mass concentration of the small molecule diamine compound is 2.0%, the mass concentration of af-GQDs is 0.01%, and the aqueous phase monomer solution.

[0093] The oil phase monomer solution is the same as that of Comparative Example 1.

[0094] The method of embodiment 1 is as follows:

[0095] Step 1: Pour a certain amount of af-GQDs-containing aqueous phase monomer solution on the surface of the ultrafiltration basement membrane and keep it for 30 seconds, then pour out the aqueous phase and let it dry for 30 seconds.

[0096] Step 2: Pour a certain amount of oil phase monomer solution on the surface of the ultrafiltration basement membrane that has absorbed the water phase monomer and keep it for 30s, then pour off th...

Embodiment 2

[0102] The differences from Comparative Example 1 include: the addition of af-GQDs to the aqueous phase solution, and the addition of chemical crosslinking and solvent activation steps after interfacial polymerization.

[0103] The aqueous monomer solution is the same as in Example 1.

[0104] The oil phase monomer solution is the same as that of Comparative Example 1.

[0105] Hexamethylenediamine (HDA) was dissolved in isopropanol to prepare a cross-linking agent solution with a mass concentration of 10%.

[0106] The activation solvent is N,N-dimethylformamide (DMF).

[0107] The method of embodiment 2 is as follows:

[0108] Step one to step four are identical with embodiment 1;

[0109] Step 5: Put the organic / inorganic hybrid film doped with af-GQDs obtained in step 4 into a cross-linking agent to chemically cross-link for 16 hours to obtain a cross-linked modified af-GQDs-doped organic / inorganic solvent-resistant organic / inorganic film hybrid film;

[0110] Step 6:...

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Abstract

The invention discloses a preparation method for a high flux solvent-resisting organic / inorganic hybridized compound film doped with aminated graphene quantum dot, a prepared compound film and an application of the film. The preparation method for the compound film comprises the steps of interfacial polymerization reaction, chemical crosslinking and solvent activation. According to the invention, the aminated graphene quantum dot is added into an interfacial polymerization monomer solution, so that the separating property and solvent resistance of the film are obviously promoted; the film-making time is shortened in the manner of increasing the cross-linking and solvent activating time; a large quantity of amino groups are loaded on the surface of the aminated quantum dot and can react with an organic phase monomer so as to form a firm covalent bond, so that the performance of the film is promoted while the stability of the quantum dot in the film is obviously promoted. According to the invention, the preparation process is simple and the film has wide application prospect in the fields of organic solution system separation and organic solvent-containing water treatment.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and specifically relates to a method for preparing a high-throughput solvent-resistant organic / inorganic hybrid composite membrane doped with aminated graphene quantum dots (af-GQDs), the prepared composite membrane and the composite membrane. Membrane application. Background technique [0002] Nanofiltration (NF) is a separation technology between reverse osmosis (RO) and ultrafiltration (UF). With its unique separation performance, it is widely used in many fields such as water treatment, food, medicine, printing and dyeing, chemical industry, etc. . At present, commercialized nanofiltration membranes are mainly used in aqueous solution systems, but many industrial separation processes require the use of a large amount of organic solvents, which requires nanofiltration membranes to have good resistance to organic solvents. The development of high-performance organic solvent-resist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/40B01D69/12B01D67/00C01B32/184B82Y30/00B82Y40/00
CPCB01D67/0079B01D69/12B01D71/40B82Y30/00B82Y40/00C01P2004/10C01P2004/51C01P2004/60C01P2004/64C01P2004/80
Inventor 苏保卫李树轩许胜杰王振远杨珊珊李灿
Owner OCEAN UNIV OF CHINA
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