Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite

A technology of graphite flakes and graphite intercalation, which is applied in the fields of high-efficiency intercalation and exfoliation of micron graphite flakes, low-order graphite intercalation compounds and micron thin-walled porous expanded graphite. Inhomogeneity, low expansion volume and other problems, to achieve the effect of shortening the process time, avoiding secondary pollution, and easy equipment

Active Publication Date: 2015-08-12
北京鼎臣石墨科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to overcome the problems of traditional oxidation intercalation method, such as long oxidation intercalation reaction time, difficult control, uneven intercalation, large order, low expansion volume, etc., the present invention provides a high-efficiency intercalation and exfoliation method for micron graphite flakes

Method used

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  • Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite
  • Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite
  • Efficient intercalation stripping method of micrometer graphite flakes and low-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite

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Embodiment 1

[0028] Example 1 : The efficient intercalation stripping method of the micron graphite flake provided by the invention adopts a one-step composite oxidation intercalation system, and basic materials are natural flake graphite (NFG), HClO 4 、HNO 3 、CH 3 COOH and KMnO 4 , and the material mass (g) volume (ml) ratio is:

[0029] NFG:HNO 3 :KMnO 4 :HClO 4 :CH 3 COOH=2g:1.6mL:0.68g:6.3mL:1.5mL.

[0030] where KMnO 4 as oxidizing agent, HClO 4 and HNO 3 is a composite oxide intercalator, CH 3 COOH is a synergistic auxiliary intercalation agent, the reaction time is 15min, ultrasonic waves and mechanical stirring are applied alternately at the same time, the reaction temperature is 35°C, and the puffing treatment temperature is 900°C.

[0031] Concrete preparation steps:

[0032] Build the reaction apparatus. Adjust and set the heating temperature of the water bath to 35°C, build a fixed three-necked flask on an iron stand, put a stirring rod in the three-necked flask,...

Embodiment 2

[0038] Example 2 : High-efficiency intercalation stripping method is adopted, and the basic materials are natural flake graphite (NFG), HClO 4 、HNO 3 、CH 3 COOH and KMnO 4 , and the material mass (g) volume (ml) ratio is:

[0039] NFG:HNO 3 :KMnO 4 :HClO 4 :CH 3 COOH=2g:1.6mL:0.68g:3.6mL:1mL, the specific preparation steps are as follows:

[0040] HNO 3 , KMnO 4 and HClO 4 Mix and prepare the main reaction solution, then add the main reaction solution to natural flake graphite, and add CH dropwise 3 COOH, the reaction time is 10min, and the reaction temperature is 45°C. During the reaction process, mechanical stirring and ultrasonic assisted stirring are continuously performed, wherein the mechanical stirring speed is 90r / min, the ultrasonic cavitation power is 150W, and the frequency is 30KHz, and the ultrasonic assisted application time is not more than 1 / 4 of the reaction time. After the reaction is finished, wash with water, decolorize, and suction filter, th...

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Abstract

The invention discloses an efficient intercalation stripping method of micrometer graphite flakes and lower-order graphite intercalation compounds and micrometer thin-wall porous expanded graphite. By the aid of a one-step combined-oxidation intercalation system, KMnO4 is oxidant, polar molecule HClO4 and planar polar micromolecule HNO3 are combined-oxidation intercalation agent, and polar micromolecule CH3COOH is used as auxiliary intercalation agent. The intercalation of the low-order graphite intercalation compounds includes three to five orders. The thermal impact capacity of the micrometer thin-wall porous expanded graphite is 508-588 mL / g, hole cavity wall thickness is down to micrometer level, hole diameter of the inside and the surface of the expanded graphite ranges widely, between 1 micrometer to 20 micrometers, and holes are mostly large and medium holes. The efficient intercalation stripping method is simple in technical process, and devices are easy to operate; reaction time is shortened and resultantly the integral technical process time is shortened as compared with that cost by the conventional preparation method, and preparation efficiency of the expanded graphite is greatly improved.

Description

technical field [0001] The invention relates to flame retardant and heat insulation, shielding damping, heat conduction and conduction, sealing and lubricating micron graphite flake carbon material which is widely used in the fields of construction, metallurgy, military, machinery, chemical industry, aerospace, electronic information and so on. Nature Flake Graphite) intercalation exfoliation preparation method and low-order graphite intercalation compounds (GIC, Graphite Intercalation Compounds) and micron thin-walled porous expanded graphite (EG, Expanded Graphite). Background technique [0002] The method of chemical oxidation intercalation is the most widely used and mature method for preparing graphite intercalation carbon materials in industry. The method is generally: soak natural flake graphite (NFG, Nature Flake Graphite) in a mixed solution of oxidant and intercalation agent, The graphite sheet is oxidized by the oxidation of the oxidant, the edge of the graphite s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 王三胜
Owner 北京鼎臣石墨科技有限公司
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