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Method for preparing graphene from agriculture and forestry waste biomass as carbon source

A technology of agricultural and forestry waste and biomass, applied in the field of graphene preparation, can solve the problems that hinder the large-scale industrial production of graphene, harsh preparation conditions, high production cost, etc., achieve large-scale industrial production, simple preparation process, and low production cost Effect

Inactive Publication Date: 2017-01-25
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Although the above two methods can use cheap biomass to prepare graphene, the preparation cycle is long, the reaction temperature is high, and the process is complicated. Both of them need to use expensive catalysts, and the production cost is high.
[0007] In short, the existing graphene preparation methods are costly, time-consuming, labor-intensive, low yield, complicated process, and harsh preparation conditions, which hinder the further large-scale industrial production of graphene.

Method used

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  • Method for preparing graphene from agriculture and forestry waste biomass as carbon source
  • Method for preparing graphene from agriculture and forestry waste biomass as carbon source
  • Method for preparing graphene from agriculture and forestry waste biomass as carbon source

Examples

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Embodiment 1

[0041] This embodiment is accomplished by the following steps:

[0042] (1) Hydrothermal carbonization of agricultural and forestry waste biomass: crush fir bark into powder, take 3g and add it to a stainless steel reactor filled with 50mL deionized water, put it into a box furnace, react at 180°C for 20h, and cool the reactor naturally Finally, the sample was taken out, washed with ionized water and ethanol successively until the filtrate was colorless, and the filtered product was dried in an oven at 100°C for 12 hours to obtain biochar.

[0043] (2) Alkali exfoliation, graphitization: Grind the obtained biochar and potassium hydroxide in an agate crucible for 30 minutes according to the ratio of potassium hydroxide / biological charcoal to 3:1 (mass ratio), and then transfer to nickel In the crucible, put it into a tube furnace, feed high-purity nitrogen as a protective gas, and the intake flow rate is 300 sccm. Raise to 400°C at a heating rate of 5°C / min, keep at this tempe...

Embodiment 2

[0048] The difference between this example and Example 1 is that the final temperature of the heating and calcination in step (2) is changed from 900°C to 1000°C.

[0049] The transmission electron microscope and the high-resolution transmission electron microscope photo of the few-layer graphene prepared in this embodiment 2 are similar to the photos of the sample in embodiment 1, respectively as figure 1 , as shown in 2. TEM results show that the number of few-layer graphene prepared in Example 2 is about 5-12 layers, the yield is 48%, and the purity is 99%.

[0050] The Raman spectrogram of the few-layer graphene prepared in this embodiment 2 is similar to that of the sample of embodiment 1, as image 3 As shown, the intensity ratio I of G peak and D peak G / I D It is 5.9, showing a strong degree of graphitization, and the existence of 2D peaks further illustrates that the prepared product is few-layer graphene.

Embodiment 3

[0052] The difference between this example and Example 1 is that the final temperature of the heating and calcination in step (2) is changed from 900°C to 800°C.

[0053] The transmission electron microscope and the high-resolution transmission electron microscope photo of the few-layer graphene prepared in this embodiment 3 are similar to the photos of the sample in embodiment 1, as figure 1 , as shown in 2. TEM results show that the few-layer graphene prepared in Example 3 has about 5 to 11 layers, the yield is 48%, and the purity is 99%.

[0054] The Raman spectrogram of the few-layer graphene prepared in this embodiment 3 is similar to that of the sample in embodiment 1, as image 3 shown. The intensity ratio I of G peak and D peak G / I D It is 5.6, showing a strong degree of graphitization, and the existence of 2D peaks further illustrates that the prepared product is few-layer graphene.

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Abstract

The invention belongs to the technical field of graphene preparation, and discloses a method for preparing graphene by using agricultural and forestry waste biomass as a carbon source. The method specifically includes the following steps: (1) Take the pulverized agricultural and forestry waste biomass, add it to a reaction kettle filled with water, undergo a hydrothermal reaction, cool to room temperature after the reaction, and then filter, wash, and dry to obtain a solid biochar; (2) mix the alkali with the biochar obtained in step (1), grind it sufficiently to make it evenly mixed, and heat and calcinate in the presence of protective gas; (3) use acid to prepare the sample after calcining in step (2) Soaking in liquid to remove by-products in the reaction, and then filtering, washing the obtained solid with water until the washing liquid is neutral, and then drying to obtain few-layer graphene. The method has the advantages of simple process, high yield, mild reaction conditions, simple required instruments and equipment, no pollution to the environment, using agricultural and forestry waste biomass as raw materials, greatly reducing production costs, and easy to realize industrial production.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a method for preparing graphene by using agricultural and forestry waste biomass as a carbon source. Background technique [0002] Graphene is made of carbon atoms with sp 2 The world's thinnest two-dimensional material composed of hybrid-connected monoatomic layers is only 0.35nm thick. Its excellent electrical properties, outstanding thermal conductivity, extraordinary specific surface area and perfect quantum tunneling effect have aroused great research interests of scientists in different fields such as physics, chemistry and materials, and became a research hotspot as soon as it came out. It is generally predicted that graphene has great application prospects in the fields of electronics, information, energy, materials and biomedicine, and is expected to set off a new technological revolution in the 21st century. [0003] The preparation method of graphene can...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01B2204/04C01B2204/30C01P2002/01C01P2002/82C01P2004/04
Inventor 刘应亮孙中新郑明涛胡航肖勇雷炳富董汉武
Owner SOUTH CHINA AGRI UNIV
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