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Method for preparing hydrophilic temperature and pH dual-sensitive graphene through thiol-ene click chemistry method

A kind of ene click and hydrophilic technology, applied in chemical instruments and methods, graphene, inorganic chemistry, etc., can solve the problem of soluble in several specific organic solvents, weak interaction between organic matter and graphene, affecting the stability of graphene, etc. problems, to achieve the effect of high product quality, high yield and low cost

Inactive Publication Date: 2013-11-27
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 on graphene with temperature and pH dual sensitivity and hydrophilicity at home and abroad.

Method used

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  • Method for preparing hydrophilic temperature and pH dual-sensitive graphene through thiol-ene click chemistry method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Measure 50 mL of 98% concentrated sulfuric acid and place it in an ice-water bath to keep it at 0-5°C; add 4.0 g flake graphite and 2.0 g NaNO 3 the mixture, stir well; slowly add 12g KMnO 4 After the addition, remove the ice-water bath, stir and react at room temperature for 24 h; then add 100 mL of deionized water, raise the temperature to 90°C, and continue stirring for 1 h; lower the temperature to 55°C, then add 30mL of 30% hydrogen peroxide , continue to stir and react for 45 min; after the reaction is completed, the graphite oxide is obtained by high-speed centrifugation, filtration and repeated water washing to neutrality, and finally vacuum drying at low temperature.

[0036] Disperse 2.0 g of the above-mentioned graphite oxide in absolute ethanol, add 15 mL of KH-570 ethanol solution with a concentration of 0.15 g / ml dropwise in a water bath at 35°C, react continuously for 48 hours, centrifugally filter and wash with water until neutral , Vacuum drying at a t...

Embodiment 2

[0044] Same as Example 1, but the consumption of 4-cyanovaleric acid dithiobenzoic acid is changed from 45 mg to 50 mg in step (3), the consumption of pH sensitive monomer is changed from 2 g to 2.5 g, other Change.

Embodiment 3

[0046] Same as Example 1, but the amount of 4,4'-azo-(4-cyano)valeric acid in step (4) was changed from 15 mg to 20 mg, and the amount of temperature sensitive monomer was changed from 1.2 g to 1.9 g, the others remain unchanged.

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Abstract

The present invention relates to a method for preparing hydrophilic temperature and pH dual-sensitive graphene through a thiol-ene click chemistry method. According to the method, graphene oxide is synthesized, a chemical modification method is adopted to prepare unsaturated carbon-carbon double bond group-containing graphene oxide, a reversible addition-fragmentation chain transfer polymerization method is adopted to synthesize a temperature and pH dual-sensitive block polymer, the temperature and pH dual-sensitive block polymer is reduced into thiol group-containing temperature and pH dual-sensitive diblock polymer under a strong reduction agent effect, a thiol-ene click chemistry reaction is adopted to prepare hydrophilic temperature and pH dual-sensitive graphene oxide, and reduction is performed under a strong reduction agent to obtain the hydrophilic temperature and pH dual-sensitive graphene. The method has advantages of simple process, no environmental pollution, high product quality, high input-output ratio, low cost, wide application prospects, and the like. The obtained product can be used in the fields of lithium ion batteries, biosensors, supercapacitors, solar cells, metal ion absorption, stress sensors, hydrogen storage materials and the like.

Description

technical field [0001] The invention belongs to the technical field of new materials, and in particular relates to a method for preparing hydrophilic temperature and pH double-sensitive graphene by a thiol-ene click chemistry method. 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 reporte...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184C01B32/194
Inventor 杨正龙
Owner TONGJI UNIV
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