Pollution-free low-cost technology for preparing monolayer graphene oxide

A low-cost, non-polluting technology, applied in the field of nanomaterials, can solve problems such as high cost, and achieve the effects of less time-consuming and energy-consuming, lowering preparation costs, and no danger of explosion

Active Publication Date: 2015-03-04
ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process also has a high cost

Method used

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  • Pollution-free low-cost technology for preparing monolayer graphene oxide
  • Pollution-free low-cost technology for preparing monolayer graphene oxide
  • Pollution-free low-cost technology for preparing monolayer graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Put graphite and strong acid at 0 o Stir, mix and infiltrate at C for 5 minutes, add a strong oxidant, and continue to stir for 1 hour to oxidize and peel off the graphite sheet; centrifuge, recover the supernatant as a strong acid for the next reaction, and slowly pour the muddy product into deionized water to dilute , stirred, washed with 1mol / L dilute hydrochloric acid and then repeatedly washed and centrifuged with deionized water to obtain a single-layer graphene oxide aqueous solution; In the waste water generated in step 2), feed ammonia to a pH value of 7 to obtain nitrogen, Inorganic fertilizer of potassium and iron elements; the graphene oxide aqueous solution obtained in step 2) is concentrated and subjected to freeze-drying / spray drying / supercritical drying technology to obtain graphene powder with high density and high specific surface area. The volume-to-mass ratio of the strong acid to graphite is: 40ml:1g. The mass ratio of the strong oxidizing agent to...

Embodiment 2

[0028] Combine graphite and strong acid at 40 o Stir, mix and infiltrate at C for 30 minutes, add a strong oxidant, and continue stirring for 8 hours to oxidize and peel off the graphite sheet; centrifuge, recover the supernatant as a strong acid for the next reaction, and slowly pour the muddy product into deionized water to dilute , stirred, washed with 1mol / L dilute hydrochloric acid and then repeatedly washed and centrifuged with deionized water to obtain a single-layer graphene oxide aqueous solution; In the waste water generated in step 2), feed ammonia to a pH value of 7 to obtain nitrogen, Inorganic fertilizer of potassium and iron elements; the graphene oxide aqueous solution obtained in step 2) is concentrated and subjected to freeze-drying / spray drying / supercritical drying technology to obtain graphene powder with high density and high specific surface area. The volume-to-mass ratio of the strong acid to graphite is: 100ml: 1g. The mass ratio of the strong oxidizin...

Embodiment 3

[0030] Graphite with a particle size of 0.5 μm and concentrated sulfuric acid were stirred, mixed and infiltrated at 0°C for 0.5 h, and potassium ferrate and potassium persulfate were added. Then the reaction solution was raised to room temperature for 1 h. After the reaction, the reaction solution was centrifuged to recover the strong acid. Slowly pour the bottom sediment into iced deionized water for dilution, let it stand for a period of time, wash the sediment repeatedly with 1mol / L dilute hydrochloric acid and deionized water, and centrifuge to obtain single-layer graphene oxide. The generated waste liquid is treated with ammonia gas until the pH value is 7 to obtain an inorganic fertilizer containing nitrogen, potassium and iron elements. During the reaction, the ratio of strong acid to graphite is 40ml: 1g, and the ratio of potassium ferrate to graphite is 4g: 1g. The prepared graphene oxide solution was spray-dried to prepare a khaki graphene oxide powder with a dens...

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Abstract

The invention discloses a pollution-free low-cost technology for preparing graphene oxide. The technology comprises the following steps: 1, mixing graphite with a strong acid to infiltrate graphite, adding a strong oxidant, and continuously stirring to oxidize and exfoliate graphite layers; 2, centrifuging the obtained reaction solution, recovering the strong acid to be used in a next reaction, slowly pouring the obtained muddy product into deionized water, stirring, washing by using dilute hydrochloric acid, repeatedly cleaning by using deionized water, and centrifuging to obtain monolayer graphene oxide; 3, introducing ammonia gas into wastewater until the pH value approaches 7 to obtain an inorganic fertilizer containing nitrogen, potassium, iron and phosphorus; and 4, concentrating an aqueous solution of graphene oxide, and drying to obtain graphene oxide with high density and high specific surface area. The technology has the advantages of simple, safe and controllable preparation process, less time and energy consumption, no explosion danger and no pollution. The cycle use of concentrated sulfuric acid in the raw material-to-fertilizer process makes all raw materials and elements fully used, so the preparation cost of graphene oxide is greatly reduced.

Description

technical field [0001] The invention relates to the field of nanometer materials, in particular to a process for preparing single-layer graphene oxide with no pollution and low cost. Background technique [0002] Since 2004, the excellent mechanical properties, electrical properties, thermal properties, and optical properties of graphene have been discovered one after another. Graphene has a large theoretical specific surface area, coupled with the excellent performance of the monolithic structure, carbon-based materials with graphene as the source material have been greatly developed and applied. [0003] Graphene oxide is the oxide of graphene, an important precursor of graphene, and the most important intermediate for the macroscopic assembly and modification of graphene materials. Its surface has abundant functional groups, can be dissolved in strong polar solvents, and can also be modified. In addition, it has a super large scale and specific surface area. The macr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 高超彭蠡郑耀臣魏杨扬许震刘峥孙海燕
Owner ZHEJIANG TANGUSHANGXI MATERIAL SCI & TECH
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