Method for efficiently producing chlorinated graphene

A technology of chlorinated graphene and graphene powder, applied in the field of high-efficiency production of chlorinated graphene, can solve the problems of less research on chlorine-doped graphene, complicated operation, limited application, etc. Good repeatability and uniform chlorine doping effect

Inactive Publication Date: 2015-10-21
XIAMEN KNANO GRAPHENE TECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the non-metallic elements doped in graphene include nitrogen, boron, phosphorus, sulfur, chlorine, etc., but there are few studies on chlorine-doped graphene. Wu et al. prepared chlorine-doped graphene using electron cyclotron resonance technology. , but this method has extremely high requirements on equipment and complicated operation, which limits its further application
(Justin Wu, Liming Xie, Yangguang Li, Hailiang Wang, Yijian Ouyang, Jing Guo, and Hongjie Dai. Controlled chlorine plasma reaction for noninvasive graphene doping [J]. J.Am.Chem.Soc.,2011,133:19668- 19671.) Li et al. used photocatalysis to covalently adsorb chlorine radicals and carbon atoms on graphene to prepare chlorine-doped graphene. However, this method is complicated to operate and cannot be used for mass production.
(Bo Li, Lin Zhou, Di Wu, Hailin Peng, Kai Yan, Yu Zhou, and Zhongfan Liu. Photochemical chlorination of graphene [J]. ACS Nano, 2011,5(7): 5957-5961.) Jin Huile et al. Combustion of magnesium strips activates chloromethane to generate dichlorocarbene, which then self-assembles into chlorine-doped graphene, which can be used as a cathode catalyst material in an oxygen reduction electrode, but the The method requires multiple separations, precipitations, and washings of the product, resulting in a large amount of carbon tetrachloride and chloroform waste liquid. The post-treatment is more complicated, and if it is not handled properly, there will be highly toxic phosgene.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Weigh 100g of graphene powder and put it into a chlorination reaction kettle. After the reaction kettle is locked and sealed, the graphene powder is heated. The heating temperature is set at 60°C, and the stirring device is turned on to stir the graphene powder. , so that the graphene powder fills the entire reactor, close the exhaust valve of the reactor (the valve is connected to the chlorine gas recovery device), open the vacuum valve, and vacuumize the reactor. The vacuum pressure is 0.1MPa, and the heating and vacuuming time is 30min. After the moisture in the graphene powder is completely drawn out, close the vacuum valve, stop vacuuming, and heat the graphene powder again. When the temperature reaches 300°C, open the exhaust valve, open the chlorine gas inlet valve, and let in chlorine gas. The flow rate is 450~550 mL / min, and the reaction time is 4~8h. After the reaction, close the chlorine inlet valve, close the chlorine recovery valve, feed nitrogen ...

Embodiment 2

[0016] Example 2: Weigh 100g of graphene powder and put it into the chlorination reaction kettle. After the reaction kettle is locked and sealed, the graphene powder is heated. The heating temperature is set at 60°C, and the stirring device is turned on to stir the graphene powder. , so that the graphene powder fills the entire reactor, close the exhaust valve of the reactor (the valve is connected to the chlorine gas recovery device), open the vacuum valve, and vacuumize the reactor. The vacuum pressure is 0.1MPa, and the heating and vacuuming time is 30min. After the moisture in the graphene powder is completely drawn out, close the vacuum valve, stop vacuuming, and heat up the graphene powder again. When the temperature reaches 450 °C, open the exhaust valve, open the chlorine gas valve, and let in chlorine gas. The flow rate is 450~550 mL / min, and the reaction time is 3~5h. After the reaction, close the chlorine inlet valve, close the chlorine recovery valve, feed nitrogen ...

Embodiment 3

[0017] Example 3: Weigh 100g of graphene powder and put it into the chlorination reaction kettle. After the reaction kettle is locked and sealed, the graphene powder is heated. The heating temperature is set at 60°C, and the stirring device is turned on to stir the graphene powder. , so that the graphene powder fills the entire reactor, close the exhaust valve of the reactor (the valve is connected to the chlorine gas recovery device), open the vacuum valve, and vacuumize the reactor. The vacuum pressure is 0.1MPa, and the heating and vacuuming time is 30min. After the moisture in the graphene powder is completely drawn out, close the vacuum valve, stop vacuuming, and heat the graphene powder again. When the temperature reaches 600°C, open the exhaust valve, open the chlorine gas inlet valve, and let in chlorine gas. The flow rate is 450~550 mL / min, and the reaction time is 1~3h. After the reaction, close the chlorine inlet valve, close the chlorine recovery valve, feed nitroge...

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PUM

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Abstract

The invention discloses a method for efficiently producing chlorinated graphene. The method comprises the following steps that graphene powder is heated, so that a part of moisture is removed, vacuumizing is conducted until moisture of the graphene powder is completely removed, and the graphene powder continues to be heated; the graphene powder and chlorine react at a certain temperature, and a chlorinated graphene powder material is obtained; the chlorinated graphene powder material is treated with nitrogen, free chlorine adsorbed on the surface of the chlorinated graphene powder is removed, and pure chlorinated graphene powder is obtained. Negative electricity exists among the chlorinated graphene powder prepared according to the method due to the action of a chlorine functional group, and the chlorinated graphene powder is fluffier and easier to scatter in use due to the action that like charges repel; in addition, the number of steps of the preparation method is small, the productivity is high, the technology is simple, and large-scale industrial production is easy to achieve.

Description

technical field [0001] The invention relates to a graphene preparation technology, in particular to a method for efficiently producing chlorinated graphene, which is suitable for mass production of chlorinated graphene. Background technique [0002] Graphene is a new two-dimensional carbon nanomaterial composed of a single layer of carbon atoms, which has a high specific surface area, excellent electrical conductivity, thermal conductivity and mechanical properties, and because of its special energy band structure and photoelectric properties It has broad application prospects in composite materials, functional materials, power materials, sensors and other fields. However, pure graphene still has defects in many applications, and element doping of pure graphene is an effective method to improve the defects of graphene. After being doped with elements, the energy band structure of graphene will change, resulting in significant changes in its electrical, optical and magnetic ...

Claims

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Application Information

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IPC IPC(8): C01B31/00
Inventor 赵立平江龙迎林丽萍
Owner XIAMEN KNANO GRAPHENE TECH CORP
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