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Intercalation agent for rapidly stripping graphite for mass production of high-quality graphene

A technology for exfoliating graphite and graphene, applied in graphene, inorganic chemistry, organic chemistry and other directions, can solve problems such as unfavorable graphene exfoliation, complex preparation process, affecting intercalation, etc., to improve exfoliation efficiency and product quality, avoid layer The effect of inter-stacking and lowering the reaction temperature

Active Publication Date: 2018-10-12
GUANGZHOU SPECIAL PRESSURE EQUIP INSPECTION & RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this preparation technology, the preparation process of the composite intercalation agent uses a high-boiling surfactant, which is not conducive to the subsequent drying treatment and affects the quality of graphene; at the same time, the preparation process is more complicated due to the ultrasonic intercalation and then ball milling, and Long-term ultrasonic treatment will not only affect the intercalation, but also cause the intercalation agent to fall off from the interlayer, which is not conducive to the exfoliation of graphene, resulting in low yield and low quality of prepared graphene
[0005] The prior art also discloses a method for preparing graphene, which also uses the method of first intercalation and then ball milling, and uses strong oxidizing acids and other oxidizing agents as intercalation agents, and the expansion agent is also oxidizing Substances, this method is essentially no different from the redox method to prepare graphene, not only does not reduce the defect degree of graphene, but also is more complicated than the redox method preparation process
[0006] According to the above, the intercalants used in the preparation of graphene by ball milling are mainly strong oxidizing acids or other oxidizing agents or high-boiling surfactants used in the preparation process, resulting in low yield and low quality of prepared graphene.

Method used

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  • Intercalation agent for rapidly stripping graphite for mass production of high-quality graphene
  • Intercalation agent for rapidly stripping graphite for mass production of high-quality graphene
  • Intercalation agent for rapidly stripping graphite for mass production of high-quality graphene

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Embodiment 1

[0037] The intercalant used for the rapid exfoliation graphite of high-quality graphene mass production of the present embodiment comprises transition metal halide salt, nitrogen source material and organic solvent that mass ratio is 1:1:2, wherein, described transition metal halide salt is ferric chloride, the nitrogen source substance is urea, and the organic solvent is isopropanol.

[0038] The method in which the intercalation agent is used to exfoliate graphite to prepare graphene specifically includes: pouring 1g of expanded graphite into a dry ball mill jar, then mixing 10g of ferric chloride, 10g of urea, and 20g of isopropanol into the ball mill The ball mill jar is covered with zirconia beads; the ball mill jar is symmetrically fixed on the planetary ball mill, the speed is adjusted to 700rpm, and the ball mill is continued for 48h; after ball milling, the graphite intercalation compound and the intercalation agent are separated by high-speed centrifugation at 10000rp...

Embodiment 2

[0042] The intercalant for the rapid exfoliation of graphite used in the mass production of high-quality graphene in this embodiment includes a transition metal halide salt, a nitrogen source substance, and an organic solvent with a mass ratio of 1:1:10, wherein the transition metal halide salt copper chloride, the nitrogen source substance is urea, and the organic solvent is ethanol.

[0043] The method that the intercalation agent is used for exfoliating graphite to prepare graphene specifically includes: pouring 1g of 300 mesh flake graphite into a dry ball mill jar, then mixing 5g cupric chloride, 5g urea, and 50g absolute ethanol and pouring Put it into a ball mill jar so that it is not covered with zirconia beads. Fix the ball mill tank symmetrically on the planetary ball mill, adjust the speed to 500rpm, and continue ball milling for 48 hours; after ball milling, use 10,000rpm high-speed centrifugation to separate the graphite intercalation compound from the intercalati...

Embodiment 3

[0047] The intercalant for the rapid exfoliation of graphite used in the mass production of high-quality graphene in this embodiment includes a transition metal halide salt, a nitrogen source substance and an organic solvent with a mass ratio of 10:1:2, wherein the transition metal halide salt It is ferric chloride hexahydrate, the nitrogen source substance is urea, and the organic solvent is ethylene glycol.

[0048] The method that the intercalation agent is used to exfoliate graphite to prepare graphene specifically includes: pouring 1g graphite powder into a dry ball mill jar, then mixing 50g ferric chloride hexahydrate, 5g urea, and 10g ethylene glycol Pour it into the ball mill jar to make it covered with zirconia beads; fix the ball mill jar symmetrically on the planetary ball mill, adjust the speed to 400rpm, and continue ball milling for 48 hours; after ball milling, use 10000rpm high-speed centrifugation to separate the graphite intercalation compound from the interca...

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Abstract

The invention relates to an intercalation agent for rapidly stripping graphite for mass production of high-quality graphene. The intercalation agent is prepared from transitional metal halogen salt, anitrogen source substance and an organic solvent; and a mass ratio of the transitional metal halogen salt to the nitrogen source substance to the organic solvent is (1 to 10): 1: (2 to 10). The transitional metal halogen salt can form eutectic crystals with the nitrogen source substance or the organic solvent, a melt point of the eutectic crystal is lower than the melt point of each component, the mixed intercalation agent is liquid at room temperature, the intercalation agent is intercalated into the graphite to form a graphite interlayer compound, so that the reaction temperature, the preparation cost and the difficulty are reduced; and meanwhile, the nitrogen source substance can also form a hydrogen bond with the organic solvent, so that a combined body of the nitrogen source substance and the organic solvent exists stably among the layers of the graphene, the interlayer accumulation of the prepared graphene can be avoided, and the stripping efficiency and the product quality canbe improved. The intercalation agent does not have chemical reaction in the ball milling process, and can be separated from the graphite interlayer compound in a centrifuging manner, and the separatedintercalation agent can be recycled, so that energy can be saved, and the environment can be protected.

Description

technical field [0001] The invention relates to the technical field of graphene preparation, in particular to an intercalation agent for rapid exfoliation graphite used for mass production of high-quality graphene. Background technique [0002] Graphene has excellent properties such as high electron mobility, ultra-high thermal conductivity, good mechanical properties, and significant room temperature Hall effect, making graphite and graphene-related materials widely used in battery electrode materials, semiconductor devices, transparent Display, seawater desalination, hydrogen storage materials, aerospace, composite materials, etc. In view of the excellent performance and potential application value of graphene materials, the research and application development of graphene at home and abroad continues to heat up. Researchers are committed to trying different methods in different fields in order to prepare high-quality, large-scale graphene materials, and through continuou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19
CPCC01B32/19C01B32/192C01G49/10C07C275/02
Inventor 杨波黄国家李茂东李悦文芳郭华超翟伟张双红王志刚李仕平伍振凌何颖怡
Owner GUANGZHOU SPECIAL PRESSURE EQUIP INSPECTION & RES INST
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