Multilayer cross-linked graphene oxide as well as preparation method and application thereof

A technology of graphene and cross-linking agent, which is applied in the field of preparation of multi-layer cross-linked graphene oxide, which can solve the problem of poor stability of multi-layer graphene oxide, complicated and special ultra-low temperature synthesis equipment, and difficulty in using multi-layer graphene oxide as a reverse osmosis membrane Problems such as the separation layer can be solved to achieve the effects of improving salt interception rate and water flux, improving stability, and making products environmentally friendly.

Active Publication Date: 2019-11-01
OCEAN UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the problems existing in the synthesis method of the above-mentioned multilayer graphene oxide, the present invention provides a method for preparing multilayer graphene oxide by using the method of assembly-crosslinking-dispersion, which solves the need for more complex special methods in the existing synthesis methods. The problem of ultra-low temperature synthesis equipment and poor stability of multilayer graphene oxide; at the same time, it solves the problem that the existing multilayer graphene oxide is difficult to use as the separation layer of reverse osmosis membrane

Method used

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  • Multilayer cross-linked graphene oxide as well as preparation method and application thereof
  • Multilayer cross-linked graphene oxide as well as preparation method and application thereof
  • Multilayer cross-linked graphene oxide as well as preparation method and application thereof

Examples

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Effect test

Embodiment 1

[0029] Add 1mg of anhydrous ethylenediamine to 100ml, 0.1mg / ml graphene oxide solution as a cross-linking agent, shake well to obtain a mixed solution, then filter the mixed solution with an ultrafiltration membrane, and filter the The ultrafiltration membrane of the product is placed in an oven, heated to 50°C and kept for 2 hours for crosslinking, and finally the ultrafiltration membrane with multi-layer crosslinked graphene oxide obtained after crosslinking is placed in deionized water for ultrasonic treatment for 20min , the ultrasonic power is 25W, and the solution obtained after ultrasonic treatment is dialyzed for 24 hours, and the molecular weight cut-off of the dialysis bag is 8000-14000Da, that is, multi-layer cross-linked graphene oxide.

[0030] Add the prepared 50mg multilayer cross-linked graphene oxide into 100ml of the aqueous phase solution in step (2) of Comparative Example 1, and the others are the same as in Comparative Example 1 to prepare a polyamide rever...

Embodiment 2

[0033] To 100ml, 0.15mg / ml graphene oxide solution, add 7.5mg of anhydrous ethylenediamine as a crosslinking agent, shake well to obtain a mixed solution, then filter the mixed solution with an ultrafiltration membrane, and then filter the mixed solution with The ultrafiltration membrane that retains the product is placed in an oven, heated to 55°C and kept for 2 hours for crosslinking, and finally the ultrafiltration membrane with multi-layer crosslinked graphene oxide obtained after crosslinking is placed in deionized water for ultrasonic treatment 40min, the ultrasonic power is 30W, and the solution obtained after ultrasonic treatment is dialyzed for 36h, and the molecular weight cut-off of the dialysis bag is 8000-14000Da, that is, multi-layer cross-linked graphene oxide.

[0034] Add the prepared 50mg multilayer cross-linked graphene oxide into 100ml of the aqueous phase solution in step (2) of Comparative Example 1, and the others are the same as in Comparative Example 1 ...

Embodiment 3

[0036]Add 5 mg of anhydrous ethylenediamine as a cross-linking agent to 100 ml, 0.15 mg / ml graphene oxide solution, shake well to obtain a mixed solution, then filter the mixed solution with an ultrafiltration membrane, and then filter the mixed solution with the intercepted The ultrafiltration membrane of the product is placed in an oven, heated to 60°C and kept for 1h for crosslinking, and finally the ultrafiltration membrane with multi-layer crosslinked graphene oxide obtained after crosslinking is placed in deionized water for ultrasonic treatment for 20min , the ultrasonic power is 40W, and the solution obtained after ultrasonic treatment is dialyzed for 48 hours, and the molecular weight cut-off of the dialysis bag is 8000-14000Da, that is, multi-layer cross-linked graphene oxide.

[0037] Add the prepared 50mg multilayer cross-linked graphene oxide into 100ml of the aqueous phase solution in step (2) of Comparative Example 1, and the others are the same as in Comparative...

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Abstract

The invention discloses a multi-layer cross-linked graphene oxide prepared by adopting an assembling-cross-linking-dispersing method. The preparation method comprises the following steps: firstly, filtering a graphene oxide aqueous solution by a filter pressing method under the action of a cross-linking agent, and then heating and cross-linking the graphene oxide; and finally, carrying out ultrasonic and dialysis treatments on the cross-linked self-assembled graphene oxide to obtain the multilayer cross-linked graphene oxide. The method has the advantages of mild conditions, no need of complexspecial ultralow temperature synthesis equipment, improvement of the stability of graphene oxide, and environmental protection. Meanwhile, the multi-layer cross-linked graphene oxide is added into the polyamide reverse osmosis membrane as a nano filling material, so that the polyamide reverse osmosis membrane has good salt rejection rate and water flux.

Description

Technical field: [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing multilayer crosslinked graphene oxide. The multilayer crosslinked graphene oxide can be added to polyamide reverse osmosis membranes as nanometer filling materials. Background technique: [0002] Graphene oxide can be regarded as an oxidized derivative of graphene. It maintains the original honeycomb sheet structure of graphene, and has a large number of functional groups such as hydroxyl, carboxyl, and epoxy on the surface and edges. These active functional groups not only endow graphene oxide with good water solubility and negative charge, but also are prone to chemical reactions, providing reaction sites for crosslinking and modification. Therefore, it has excellent mechanical properties, thermal properties, electrochemical properties and high transparency, which makes it have a broad application space in the fields of optoelectronic m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/56B01D61/02B01D61/14B01D67/00C01B32/198
CPCB01D61/025B01D61/145B01D67/0006B01D71/56C01B2204/04C01B32/198
Inventor 高学理王小娟宋娜魏怡苏保卫高从堦
Owner OCEAN UNIV OF CHINA
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