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A kind of preparation method of sulfonated reduced graphene oxide

A graphene and sulfonation technology, applied in graphene, chemical instruments and methods, carbon compounds, etc., can solve safety problems and other problems, and achieve the effects of avoiding safety problems, mild reaction conditions, and broad application prospects

Active Publication Date: 2019-04-02
NANJING UNIV OF INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, there are certain safety issues in the preparation of sulfonated graphene by diazotization reaction.

Method used

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  • A kind of preparation method of sulfonated reduced graphene oxide

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Embodiment 1

[0020] The preparation method of sulfonated reduced graphene oxide of the present invention is as follows:

[0021] (1) Weigh 0.1 g of graphene oxide, dissolve in 100 mL of deionized water, and sonicate for 2 hours;

[0022] (2) Adjust the pH value of the solution to 8 with sodium hydroxide, sonicate for 2 hours, and transfer the above graphene oxide solution to a four-necked flask;

[0023] (3) Weigh 1g of hydrazine hydrate, add it into a four-necked flask, and react at 60°C for 15 hours;

[0024] (4) After suction filtration and deionized water washing, 20 mL of methanol was added to prepare a reduced graphene oxide methanol solution.

[0025] (5) Weigh 0.1 g of sodium metal, add it to the reduced graphene oxide methanol solution, and stir for 2 hours.

[0026] (6) Weigh 0.1 g of epichlorohydrin, add it to the solution after the reaction in step (5), heat to 30 °C, stir for 10 hours, and rotate to evaporate at 30 °C to obtain powder I.

[0027] (7) Weigh 0.1 g of p-aminob...

Embodiment 2

[0030] The preparation method of sulfonated reduced graphene oxide of the present invention is as follows:

[0031] (1) Weigh 0.2 g of graphene oxide, dissolve in 200 mL of deionized water, and sonicate for 2 hours;

[0032] (2) Adjust the pH value of the solution to 10 with ammonia water, sonicate for 2 hours, and transfer the above graphene oxide solution to a four-necked flask;

[0033] (3) Weigh 2.5 g of ammonium thiosulfate, add it into a four-necked flask, and react at 80 °C for 12 hours;

[0034] (4) After suction filtration and deionized water washing, 50 mL of methanol was added to prepare a reduced graphene oxide methanol solution.

[0035] (5) Weigh 0.1 g of sodium metal, add it to the reduced graphene oxide methanol solution, and stir for 4 hours.

[0036] (6) Weigh 0.31 g of epichlorohydrin, add it to the solution after the reaction in Step 5, heat to 50 °C, stir for 6 hours, and then rotatively evaporate at 50 °C to obtain powder I.

[0037] (7) Weigh 0.57 g o...

Embodiment 3

[0041] The preparation method of sulfonated reduced graphene oxide of the present invention is as follows:

[0042] (1) Weigh 1 g of graphene oxide, dissolve it in 200 mL of deionized water, and sonicate for 2 hours;

[0043] (2) Adjust the pH value of the solution to 10 with ammonia water, sonicate for 4 hours, and transfer the above graphene oxide solution to a four-necked flask;

[0044] (3) Weigh 5g of ammonium thiosulfate, add it into a four-necked flask, and react at 90°C for 5 hours;

[0045] (4) After suction filtration and deionized water washing, 50 mL of methanol was added to prepare a reduced graphene oxide methanol solution.

[0046] (5) Weigh 5 g of sodium metal, add it to the reduced graphene oxide methanol solution, and stir for 6 hours.

[0047] (6) Weigh 0.5 g of epichlorohydrin, add it to the solution after the reaction in step (5), heat to 60 °C, stir for 5 hours, and then rotatively evaporate at 60 °C to obtain powder I.

[0048] (7) Weigh 0.6 g of p-am...

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Abstract

The invention discloses a preparation method of sulfated reduciton-oxidation graphene. According to the method, reduciton-oxidation graphene is taken as a raw material, a sulfated group is introduced by a ring-opening reaction of an epoxy group, and the sulfated reduciton-oxidation graphene is prepared. The sulfated group is introduced by the ring-opening reaction of the epoxy group, the reaction condition is mild, safe, stable and reliable, the safety problem of a diazotization reaction is avoided, and the sulfated reduciton-oxidation graphene has a wide application prospect as a humidity-sensing sensor material.

Description

technical field [0001] The invention relates to a preparation method of a sulfonated reduced graphene oxide material with moisture-sensitive properties. Background technique [0002] Portable, stable, reliable and low-cost humidity sensors play a pivotal role in national defense, industry, agriculture, medicine, aerospace, and weather monitoring. The physical and chemical properties of the moisture-sensitive material itself are the key factors affecting its moisture-sensitive performance. At present, the materials for preparing humidity-sensitive sensors mainly include: organic polymers, ceramics, metal oxides and their composites, etc. These materials have parameters such as sensitivity, response time-recovery time, and hysteresis, which cannot meet the increasingly stringent requirements of the rapid development of science and technology for sensors. Therefore, the research and development of humidity-sensitive materials with superior performance such as high sensitivity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/194
CPCC01B2204/22C01P2004/03
Inventor 张超智柏源陈斌
Owner NANJING UNIV OF INFORMATION SCI & TECH