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Method for preparing graphene with solid phase assisted microwaves

A graphene and microwave technology, applied in the field of materials science, can solve the problems of polluting the environment, high energy consumption, complex reduction process, etc., and achieve the effects of high reduction degree, simplified process, and simple preparation process.

Inactive Publication Date: 2017-12-01
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the above-mentioned technical problems in the prior art, the invention provides a kind of method that adopts solid-phase assisted microwave to prepare graphene, described this method that adopts solid-phase assisted microwave to prepare graphene will solve the oxidation problem in the prior art Graphene reduction process is complex, pollutes the environment, and consumes a lot of technical problems

Method used

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  • Method for preparing graphene with solid phase assisted microwaves

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Utilize improved Hummers method to prepare the mixed solution of graphite oxide and water, concrete steps are as follows:

[0024] Measure 96mL of concentrated sulfuric acid and place it in a dry container, add 2g of sodium nitrate to it, stir to dissolve the sodium nitrate, then add 2g of flake graphite, after the flake graphite is evenly dispersed, slowly add 12g of potassium permanganate, react for 1.45h, During the whole process, an ice bath was used to keep the system at 0-3°C, then the temperature was raised to 35°C for 2 hours, then 80 mL of deionized water was slowly added to the reaction system, the temperature was raised to 95°C for 30 minutes, and then 200 mL of deionized water was slowly added to the reaction system. deionized water, followed by 10 mL H 2 o 2 , continue to react for 10min, the resulting reaction solution is centrifuged, and the gained precipitate is washed with 1000mL mass percentage concentration of 5% HCl aqueous solution to remove metal ...

Embodiment 2

[0026] A method for preparing graphene by solid-phase assisted microwave reduction of graphene oxide, specifically comprising the steps of:

[0027] (1) Sonicate the mixture of graphite oxide and water to 1L, 80W, 40KHz for 45min, centrifuge the suspension obtained after sonication at 2000rpm for 60min, take the supernatant and dry it in a vacuum oven at 80°C for 24h before grinding. Obtain graphene oxide powder;

[0028] The mixed solution of described graphite oxide and water is prepared by an improved Hummers method;

[0029] (2) Fill 150g of silicon carbide powder 5 into the annular gap between the first quartz glass 1 and the second quartz glass 3, and put 200mg of graphene oxide 2 prepared in step (1) into the first quartz Glass 1 (eg figure 1 shown), then put it into an industrial microwave oven to evacuate to make the absolute pressure in the furnace lower than 0.1MPa, pass argon gas to normal pressure and then evacuate, repeat this process three times. Before turni...

Embodiment 3

[0032]A method for preparing graphene by solid-phase assisted microwave reduction of graphene oxide, specifically comprising the steps of:

[0033] (1) Sonicate the mixture of graphite oxide and water for 45min at 0.5L, 80W, 40KHz, centrifuge the suspension obtained after sonication at 2500rpm for 30min, take the supernatant and dry it in a blast drying oven at 60°C for 24h Collect to obtain graphene oxide fragments;

[0034] The mixed solution of described graphite oxide and water is prepared by an improved Hummers method;

[0035] (2) Fill 80g of graphite powder 5 into the annular gap between the first quartz glass 1 and the second quartz glass 3, and put 100mg of graphene oxide 2 prepared in step (1) into the first quartz glass Cup 1 (as in figure 1 shown), then put it into an industrial microwave oven to evacuate to make the absolute pressure in the furnace lower than 0.1MPa, pass argon gas to normal pressure and then evacuate, repeat this process three times. Before tu...

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Abstract

The invention discloses a method for preparing graphene with solid phase assisted microwaves. The method comprises the following steps: a graphite oxide and water mixed solution is subjected to ultrasonic treatment for 10 min-1 h, then a suspension obtained after ultrasonic treatment is centrifuged under the condition of 2000-3000 rpm for 20-60 min, a supernatant liquid obtained after centrifugation is graphene oxide colloid, the graphene oxide colloid is dried, and graphene oxide is obtained; graphene oxide and an assisted wave absorbing material are placed into a reaction chamber of an industrial microwave oven and react under the power of 300-2000 W for 15-90 s with inert gas shielding, then the microwaves are stopped, and graphene is obtained after cooling to the room temperature. Any chemical reagent harmful to the human body and the environment is not required to be added in the reaction process, and safety and environmental protection are realized; the preparation process is simple, the reaction time is short, and high efficiency and energy saving are realized.

Description

technical field [0001] The invention belongs to the field of materials science and relates to a graphene, in particular to a method for preparing graphene by using solid-phase assisted microwaves. Background technique [0002] Graphene is a sp 2 A new type of carbon nanomaterial with a two-dimensional periodic honeycomb lattice structure composed of hybrid carbon six-membered rings. In the lattice structure of ideal graphene, each C atom is connected to three adjacent C atoms through a strong δ bond. Each C atom in the six-membered ring has an unbonded valence electron, which forms a conjugated delocalized large π bond in the direction perpendicular to the plane, and the special lattice of graphene The structure endows it with many unique properties. Its special structure and excellent properties have attracted extensive attention from the material science and physics circles. Research in recent years has shown that graphene has the characteristics of ultra-high specific ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192
CPCY02P20/10
Inventor 金双玲唐珊刘美晨曹陆伟金鸣林陆王钊胡震张睿刘艳
Owner SHANGHAI INST OF TECH
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