A method for preparing graphene by combining ultrasonic stripping and jet stripping

A technology of ultrasonic exfoliation and graphene, applied in the direction of graphene, nano-carbon, etc., can solve the problems of low conversion rate of raw materials, high equipment requirements, low equipment requirements, etc., and achieve the effect of high concentration, simple equipment requirements, and few production steps.

Active Publication Date: 2018-11-09
SHANGHAI LEVSON ENTERPRISE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the quality of graphene prepared by mechanical exfoliation method is the highest, but its yield is very low and can only be used for scientific research; the high cost of ultra-high vacuum graphene epitaxial growth method and the structure of small wafers limit its application; chemical vapor deposition and The graphene prepared by the epitaxial growth method has few defects, but it has high requirements on equipment and low conversion rate of raw materials, which greatly limits its application; although the preparation of graphene by redox method can produce graphene with fewer layers on a large scale, the strong oxidant The damage to the graphene lattice makes it impossible to recover the hexagonal honeycomb crystal structure, resulting in the loss of some of its properties; a large amount of graphene can be synthesized by electrolysis, but the surface of the synthesized graphene has a large number of positive ions or negative ions or Organic matter; ultrasonic exfoliation method uses graphite or expanded graphite as raw material, low equipment requirements, low energy consumption, and the prepared graphene has few defects and high concentration, which is considered to be the most promising preparation method; graphite synthesized by thermal solvent method The purity of alkenes is relatively high, but the reaction time is relatively long, and the yield is only 1-5%.

Method used

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  • A method for preparing graphene by combining ultrasonic stripping and jet stripping
  • A method for preparing graphene by combining ultrasonic stripping and jet stripping
  • A method for preparing graphene by combining ultrasonic stripping and jet stripping

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Prepare 0.5g / L sodium dodecylbenzenesulfonate aqueous solution and stir at high speed for 30 minutes;

[0037] 2, the purity is 99.90wt%, and the graphite whose median particle diameter (D50) is 10 μm is added in the sodium dodecylbenzenesulfonate aqueous solution of step 1, and graphite concentration is 25g / L, stirs at high speed for 30 minutes;

[0038] 3. Press figure 1 Schematic diagram of ultrasonic peeling device for ultrasonic peeling, where the ultrasonic power is 300W and the ultrasonic time is 12 hours;

[0039] 4. Press figure 2 Schematic diagram of the jet stripping device for jet stripping, where the flow rate is 300L / h, the feed pump pressure is 2bar, the outlet temperature is 56°C, the nozzle pressure is 300bar, and the number of cycles is 8;

[0040] 5. Vacuum drying to obtain graphene, wherein the drying temperature is 80° C., and the drying time is 6 hours.

Embodiment 2

[0042] 1. Prepare 1.0g / L cetyltrimethylammonium bromide aqueous solution and stir at high speed for 30 minutes;

[0043] 2. Add the graphite with a purity of 99.90wt% and a median particle size (D50) of 60 μm to the cetyltrimethylammonium bromide aqueous solution in step 1, the graphite concentration is 50 g / L, and stir at high speed for 30 minutes;

[0044] 3. Press figure 1 Schematic diagram of ultrasonic peeling device for ultrasonic peeling, where the ultrasonic power is 500W and the ultrasonic time is 10 hours;

[0045] 4. Press figure 2 Schematic diagram of the jet stripping device for jet stripping, where the flow rate is 350L / h, the feed pump pressure is 3bar, the outlet temperature is 58°C, the nozzle pressure is 500bar, and the number of cycles is 7;

[0046] 5. Vacuum drying to obtain graphene, wherein the drying temperature is 80° C., and the drying time is 6 hours.

Embodiment 3

[0048] 1. Prepare 2.0g / L sodium lauryl sulfate aqueous solution and stir at high speed for 30 minutes;

[0049] 2. The graphite with a purity of 99.95wt% and a median diameter (D50) of 50 μm is added to the sodium lauryl sulfate aqueous solution of step 1, and the graphite concentration is 50 g / L, and stirred at high speed for 30 minutes;

[0050] 3. Press figure 1 Schematic diagram of ultrasonic peeling device for ultrasonic peeling, where the ultrasonic power is 750W and the ultrasonic time is 8 hours;

[0051] 4. Press figure 2 Schematic diagram of the jet stripping device for jet stripping, where the flow rate is 350L / h, the feed pump pressure is 3bar, the outlet temperature is 57°C, the nozzle pressure is 700bar, and the number of cycles is 5;

[0052] 5. Vacuum drying to obtain graphene, wherein the drying temperature is 80° C., and the drying time is 5 hours.

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Abstract

The invention discloses a method for preparing graphene by combining ultrasonic peeling and jet flow peeling. The method comprises the steps that firstly, graphite is dispersed in an aqueous surfactant solution; secondly, the mixed liquid obtained in the first step is subjected to ultrasonic peeling, and multilayer graphene dispersion liquid is obtained; thirdly, the multilayer graphene dispersion liquid obtained in the second step is subjected to jet flow peeling, and monolayer graphene dispersion liquid is obtained; fourthly, the monolayer graphene dispersion liquid obtained in the third step is dried, and the graphene is obtained. According to the preparation method, the ultrasound and jet flow combined peeling mode is adopted for the first time, the obtained graphene in the dispersion liquid has few structural defects and layers and high concentration, the excellent performance of graphene is retained very well, and the graphene can be widely applied to the fields of automotive parts, sensors, conductive materials, heat conduction materials and the like. The method is economical and environmentally friendly, the raw material utilization rate is increased, and the industrialization cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of preparation of graphene functional materials, and in particular relates to a method for preparing graphene by combining ultrasonic stripping and jet stripping. technical background [0002] Since Andre K. Geim (Andre K. Geim) of the University of Manchester in the United Kingdom prepared graphene materials in 2004, due to its unique structure and photoelectric properties, it has received widespread attention. Graphene is a two-dimensional carbon nanomaterial composed of a layer of carbon atoms. It is the thinnest known two-dimensional material, with a thickness of only 0.34nm. Single-layer graphite is considered an ideal material due to its large specific surface area, excellent electrical and thermal conductivity, and low thermal expansion coefficient. It can be widely used in polymer materials, supercapacitors, fibers, electrode materials, electronics and other fields. [0003] At present, the prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
CPCC01P2002/72C01P2004/04
Inventor 沈理欢张燕萍赵志国
Owner SHANGHAI LEVSON ENTERPRISE GRP
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