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Method for preparing hydrophilic graphene with pH sensitivity

A hydrophilic and graphene technology, applied in the direction of graphene, nanotechnology, nanocarbon, etc., can solve the problems of environmental pollution, solubility in several specific organic solvents, and low stability of graphene, and achieve simple process, The effect of high yield

Inactive Publication Date: 2013-09-18
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent CN102145882A reports a method for preparing water-soluble graphene. The method is to first oxidize graphite into graphite oxide; Water-soluble graphene, but this method is based on the water-soluble graphene prepared by the π-π conjugation mechanism between the aromatic water-soluble small molecule Coomassie brilliant blue and graphene, so the interaction between organic matter and graphene is weak, It will inevitably affect the stability of graphene in aqueous solution
Chinese patent CN101844762A has reported a preparation method of hydrophilic graphene, which is to oxidize flake graphite by Hummers method to obtain graphite oxide, then disperse the obtained graphite oxide in deionized water, and perform ultrasonic treatment to make graphite oxide peel off Form a single-layer graphene oxide sheet, and then add hexamethylenetetramine to react to obtain a graphene dispersion that is stably dispersed in water, but the graphene prepared by this method has low stability in aqueous solution and is prone to Aggregate deposition
Chinese patent CN101863465A reports a method for preparing graphene that can be dispersed in organic solvents. This method uses bulky dendritic substituents to functionalize graphene oxide, so that the obtained graphene oxide can be dispersed in most organic solvents. After hydration After trap reduction, the obtained graphene still maintains excellent organic solvent dispersion properties, but the graphene prepared by this method can only be dissolved in several specific organic solvents, and a highly toxic solvent was used in the preparation process— Thionyl chloride has the problem of environmental pollution
So far, there are no public literature reports and patent applications about pH-sensitive and hydrophilic graphene at home and abroad.

Method used

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  • Method for preparing hydrophilic graphene with pH sensitivity
  • Method for preparing hydrophilic graphene with pH sensitivity
  • Method for preparing hydrophilic graphene with pH sensitivity

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 40.4 mg 4-cyanopentanoic acid dithiobenzoic acid (CTP), 10.2 mg 4,4'-azo-(4-cyano)valeric acid (V-501) into a 25 mL single-necked bottle ( Make the molar ratio of CTP to V-501 4:1), and add 0.5 mL of dioxane to dissolve it completely; after dissolving 2.01 g of dimethylaminoethyl methacrylate (DMAEMA) in 6 mL of deionized water , adjust the pH to 4 and add it to a one-necked bottle, place it in a water bath with a magnetic heating stirrer under nitrogen protection, raise the temperature to 70°C and react for 9 h, after the reaction is completed, cool the reaction bottle to room temperature and ventilate to the atmosphere for 30 min. Then the product was dialyzed in deionized water with a pH of 4.5 for 3 days (the molecular weight cut-off of the dialysis bag was 1000), and then freeze-dried for 48 h to obtain a hydrophilic polymer PDMAEMA.

[0027]Add 100 mg of graphite oxide (iGO) and 10 mL of anhydrous N,N-dimethylformamide into a 50 mL round-bottomed flask, and ul...

Embodiment 2

[0031] Same as Example 1, but the consumption of 4-cyano-4-(thiobenzoyl) valeric acid in the first step of the reaction is changed from 40.4 mg to 50.3 mg, and the consumption of dimethylaminoethyl methacrylate is changed from 2.01 g becomes 2.51 g, N-3-aminopropylmethacrylamide hydrochloride, 4-cyano-4-(thiobenzoyl)valeric acid) and 4,4'-azo-( The molar ratio of 4-cyanovaleric acid) was changed from 100:1:0.25 to 88:1:0.2, and the others remained unchanged.

Embodiment 3

[0033] Same as Example 1, but the amount of 4,4'-azo-(4-cyanovaleric acid) in the first step of the reaction was changed from 10.2 mg to 20.3 mg, and in the system dimethylaminoethyl methacrylate, 4- The molar ratio of cyano-4-(thiobenzoyl)valeric acid to 4,4'-azo-(4-cyanovaleric acid) was changed from 100:1:0.25 to 88:1:0.5, and the others remained unchanged .

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Abstract

The invention belongs to the technical field of novel materials and particularly relates to a method for preparing hydrophilic graphene with pH sensitivity. The method comprises the following steps of: firstly, synthesizing a hydrophilic polymer PDMAEMA by a reversible addition-fragmentation transfer polymerization process; secondly, carrying out isocyanic acid esterification on the surface of a graphene oxide; by a grafting reaction between the hydrophilic polymer PDMAEMA and the isocyanic-acid-esterified graphene oxide, obtaining hydrophilic graphene oxide iGO-PDMAEMA with pH sensitivity; and finally reducing the hydrophilic graphene oxide iGO-PDMAEMA with pH sensitivity to the hydrophilic graphene with pH sensitivity. The method has the characteristics of being simple in technology, high in yield, pollution-free to environment, and the like; the prepared hydrophilic graphene can be uniformly and stably dispersed in an aqueous solution for a long time and has pH sensitivity.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a method for preparing hydrophilic pH-sensitive graphene. Background technique [0002] Graphene is a new type of two-dimensional planar nanomaterial discovered in 2004. It is a kind of sp 2 A single-layer two-dimensional honeycomb graphite crystal composed of hybridized carbon atoms has excellent mechanical, electrical and thermodynamic properties. Since its discovery, graphene has attracted the attention of many researchers around the world. It is currently the most active research object in the fields of materials science and condensed matter physics. It has shown great promise in the fields of electronics, information, energy, materials, and biomedicine. Broad application prospects. However, graphene with a complete structure has a large aromatic conjugated structure. Although it has been reported in the literature that a single layer of graphene can exist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y40/00C01B32/184
Inventor 杨正龙徐晓黎
Owner TONGJI UNIV
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