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Preparation method of single-layer graphene pyridine solution

A single-layer graphite and vinylpyridine technology, applied in the field of graphene technology preparation, can solve problems such as high price, toxicity, harm to human body and environment, etc., and achieve the effects of long-term preservation, good corrosion inhibition, and uniform dispersion.

Inactive Publication Date: 2014-04-16
北京纳新天地科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Commonly used reducing agents include hydrazine hydrate, hydroquinone, sodium borohydride, reducing sugar, aluminum powder, etc., but both hydrazine hydrate and hydroquinone are highly toxic and harmful to humans and the environment; although ascorbic acid is a A highly efficient and environmentally friendly reducing agent, but its high price is not conducive to large-scale industrial production
[0005] Based on the existing technology, the preparation method of graphene aqueous solution reduced by hydroxylamine or hydrobromic acid has achieved initial success, but in some industrial applications, graphene aqueous solution cannot meet the long-term preservation of graphene-metal composite materials. Unable to meet diverse industrial uses

Method used

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  • Preparation method of single-layer graphene pyridine solution

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Experimental program
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Effect test

Embodiment 1

[0029] A kind of preparation method of monolayer graphene pyridine solution, carry out according to the following steps:

[0030] (1) Weigh 20g of natural graphite powder, put it in a 500ml reaction bottle, add 1g of calcium nitrate, 2g of potassium nitrate and 1g of sodium nitrate into it, stir well, slowly add 300g of deionized water into the reaction bottle, and control The temperature of the system is 5°C. Slowly add 0.2g of concentrated sulfuric acid with a mass concentration of 98% to the reaction bottle at a constant temperature. Control the temperature of the system not to exceed 20°C. Continue stirring. Potassium permanganate, stirring continuously, controlling the reaction temperature not to exceed 20°C, and reacting for 1 hour to obtain a graphite oxide solution.

[0031] (2) Suction filter the graphite oxide solution, wash the filter cake 4 times with dilute hydrochloric acid with a mass concentration of 2% at 35°C, and then wash 5 times with deionized water to obt...

Embodiment 2

[0035] (1) Weigh 15g of natural graphite powder, put it in a 500ml reaction bottle, add 1g of calcium nitrate, 3g of potassium nitrate and 2g of sodium nitrate to it, stir well, slowly add 350g of deionized water into the reaction bottle, and control The temperature of the system is 8°C. Slowly add 0.4g of concentrated sulfuric acid with a mass concentration of 98% to the reaction bottle at a constant temperature. Control the temperature of the system not to exceed 20°C. Continue stirring. Potassium permanganate, stirring continuously, controlling the reaction temperature not to exceed 20°C, and reacting for 30 minutes to obtain a graphite oxide solution.

[0036] (2) Suction filter the graphite oxide solution, wash the filter cake 4 times with dilute hydrochloric acid with a mass concentration of 1% at 32°C, and then wash 5 times with deionized water to obtain a graphite oxide filter cake; configure 100ml, 80g / L graphite oxide aqueous solution was placed in a 250ml Erlenmeye...

Embodiment 3

[0040] (1) Weigh 10g of natural graphite powder, put it in a 500ml reaction bottle, add 1g of calcium nitrate, 4g of potassium nitrate and 3g of sodium nitrate to it, stir well, slowly add 350g of deionized water into the reaction bottle, and control The temperature of the system is 4°C. Slowly add 5g of concentrated sulfuric acid with a mass concentration of 98% to the reaction bottle under constant temperature. Control the temperature of the system not to exceed 20°C. Continue stirring. When the temperature of the system drops to 13°C, slowly add 1g of high manganese Potassium oxide, stirring continuously, controlling the reaction temperature not to exceed 20°C, and reacting for 6 hours to obtain a graphite oxide solution

[0041] (2) Suction filter the graphite oxide solution, wash the filter cake 3 times with dilute hydrochloric acid with a mass concentration of 3% at 33°C, and then wash 4 times with deionized water to obtain a graphite oxide filter cake; configure 100ml, 1...

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Abstract

The invention discloses a preparation method of a single-layer graphene pyridine solution. According to the method, natural graphite, calcium nitrate, potassium nitrate, concentrated sulfuric acid and potassium permanganate are mixed and processed to obtain a graphite oxide solution, after the graphite oxide solution is prepared into an aqueous single-layer graphene oxide solution, hydrobromic acid is added for a reaction, an aqueous single-layer graphene solution is obtained, then pyridine is added into the aqueous graphene solution, and extraction and reduced pressure distillation are performed through an inorganic salt saturated solution to obtain the graphene pyridine solution. According to the method, the single-layer graphene pyridine solution with high single layer rate, high compositing feature and uniform dispersion is prepared finally after multiple times of ultrasonic stripping.

Description

technical field [0001] The invention relates to a preparation method in the technical field of graphene, in particular to a preparation method of single-layer graphene pyridine solution. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a planar film composed of carbon atoms in a hexagonal honeycomb lattice with sp2 hybrid orbitals. It is only one carbon atom thick. 2D materials. Graphene has always been considered as a hypothetical structure and cannot exist stably alone. Until 2004, physicists Andre Geim and Konstantin Novoselov of the University of Manchester in the United Kingdom succeeded in experimenting from graphite Graphene was isolated from the experiment, and it was confirmed that it can exist alone. The two also won the 2010 Nobel Prize in Physics for their "pioneering experiments on two-dimensional graphene materials". [0003] Graphene is currently the thinnest but also the hardest nan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/194
Inventor 王云峰李晓斐
Owner 北京纳新天地科技发展有限公司
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