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A method for preparing graphene by composite shear stress exfoliation using vibrating screw extruder

A technology of screw extruder and shear stress, which is applied in the field of preparation of graphene by compound shear stress exfoliation of vibrating screw extruder, which can solve the problem of difficult to overcome van der Waals force of graphite layer, difficulty in controlling the number of graphene layers, and long reaction time and other issues, to achieve the effect of preserving lattice integrity, efficient preparation, and stripping time period

Active Publication Date: 2017-07-25
ZHEJIANG ZHONGYANG SCREW MFG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above technical means accelerate the peeling to a certain extent, but the yield is low, the shear force is weak, and it is difficult to overcome the van der Waals force between graphite layers, so the reaction time is long and the efficiency is low, especially the number of graphene layers obtained is difficult to control

Method used

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  • A method for preparing graphene by composite shear stress exfoliation using vibrating screw extruder
  • A method for preparing graphene by composite shear stress exfoliation using vibrating screw extruder
  • A method for preparing graphene by composite shear stress exfoliation using vibrating screw extruder

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Effect test

Embodiment 1

[0036] (1) Combine graphite with excess intercalant C 12 The long-chain organic quaternary ammonium salt is added into water, homogeneously dispersed for 10 minutes, then repeatedly washed with deionized water and filtered to obtain a graphite filter cake;

[0037] (2) Disperse and mix the dried graphite filter cake in step (1) with sodium stearate and sulfamic acid at 80-120°C for 30 minutes. The mass ratio of graphite filter cake, sodium stearate and sulfamic acid 100:1:0.5;

[0038] (3) Send the mixture obtained in step (2) into a co-rotating twin-screw electromagnetic dynamic extruder. The temperature of the vibrating extruder is set at 300-400°C, the speed is 800rpm, the vibration frequency is 80Hz, and the amplitude is 0.1mm. Among them, the screw of the extruder is composed of the staggered angles between the meshing blocks of 30°, 45°, 60°, 90°, reverse 30°, reverse 45°, reverse 60°, through the high-speed rotating shear force field and vibration pull Extensive force...

Embodiment 2

[0041] (1) Combine graphite with excess intercalant C 16 The long-chain organic quaternary ammonium salt was added to water, homogeneously dispersed for 25 minutes, then repeatedly washed with deionized water and filtered to obtain a graphite filter cake;

[0042] (2) Disperse and mix the dried graphite filter cake in step (1) with calcium stearate and sodium polyaspartate at 80-120°C for 45 minutes. The mass ratio of sodium aspartate is 100:1.5:1;

[0043] (3) Send the mixture obtained in step (2) into a co-rotating four-screw ultrasonic vibration extruder. The temperature of the vibration extruder is set at 300-400°C, the speed is 1200rpm, the ultrasonic frequency is 20kHz, and the power is continuously adjustable at 2KW. Through the high-speed rotating shear force field and the ultrasonic vibration tension field, the graphite is sheared and exfoliated to obtain graphene.

Embodiment 3

[0045] (1) Combine graphite with excess intercalant C 18 The long-chain organic diamine is added into water, homogeneously dispersed for 10 minutes, then repeatedly washed with deionized water and filtered to obtain a graphite filter cake;

[0046] (2) Disperse and mix the dried graphite filter cake in step (1) with zinc stearate and diethylthiourea at 80-120°C for 35 minutes. The mass ratio of urea is 100:1:0.5;

[0047] (3) Send the mixture obtained in step (2) into a co-rotating three-screw longitudinal mechanical vibrating extruder. The temperature of the vibrating extruder is set at 300-400°C, the speed is 600rpm, the frequency is set at 50Hz, and the amplitude is 3mm. Graphene is obtained by shearing and exfoliating graphite through a high-speed rotating shear force field and a vibrating tension force field.

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Abstract

The invention provides a method for preparing graphene through composite shear stress stripping of a vibrating screw extruder, and belongs to the field of graphene materials. According to the method, an electromagnetic, ultrasonic and longitudinal mechanical vibration tensile force field is introduced into the extruder rotating at high speed, the vibration tensile force field periodically changes along with the time to enable the graphite interface to be tensioned, graphite becomes loosened under the action of a stripping agent, the graphite generates powerful shearing stripping through contact interfaces of meshing blocks of the extruder in a tensioned state, thinner graphene with the narrower thickness distribution range is obtained, and then rapid and efficient high-quality graphene preparation under the high-shearing action is achieved. The method has the advantages that the production cost of the high-quality graphene is significantly lowered, the preparation process is green and environmentally friendly, no exhaust gas or waste liquid or waste residue is generated, and scale production of the graphene is promoted.

Description

technical field [0001] The invention relates to the field of graphene materials, in particular to a method for preparing graphene by compound shear stress exfoliation of a vibrating screw extruder. Background technique [0002] Graphene is a single-layer carbon atom surface material exfoliated from graphite material, which is a two-dimensional structure of carbon. The thickness of this graphite crystal film is only 0.335 nanometers, and 200,000 sheets of standard graphene are stacked together, which is only as thick as a hair. Since the discovery of graphene, due to its excellent performance, it has been applied in many fields such as energy, electronic materials, biomedicine, and environmental protection, and its application fields are being gradually expanded. [0003] At present, the preparation techniques of graphene include mechanical exfoliation method, substrate epitaxy method, chemical vapor deposition method, redox method, chemical cleavage method and so on. The d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
Inventor 陈庆曾军堂叶任海陈兵
Owner ZHEJIANG ZHONGYANG SCREW MFG
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