Method for preparing biomass graphene employing cellulose as raw material

A biomass graphene and cellulose technology, applied in graphene, chemical instruments and methods, material excitation analysis, etc., can solve the problems of complex graphene preparation process, complex equipment required for the reaction, poor production safety, etc. The effect of industrialized production, high production safety, and increased output

Active Publication Date: 2015-06-24
HEILONGJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] One of the objectives of the present invention is to solve the existing problems of complex graphene preparation process, poor production safety, high production cost, complex equipment required for reaction, harsh reaction conditions, low yield, etc.

Method used

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  • Method for preparing biomass graphene employing cellulose as raw material
  • Method for preparing biomass graphene employing cellulose as raw material
  • Method for preparing biomass graphene employing cellulose as raw material

Examples

Experimental program
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Embodiment 1

[0028] Embodiment 1: the method that present embodiment prepares biomass graphene with cellulose as raw material is to be finished by following steps:

[0029] Step 1: prepare catalyst solution: 18gFeCl 2 Add it into 100ml of distilled water and stir for 25 minutes to obtain a uniform catalyst solution, wherein the ratio of solute to solvent in the catalyst solution is 18:100;

[0030] Step 2: Preparing the precursor: adding cellulose to the catalyst solution obtained in Step 1, stirring for 2 hours, then reacting at 140°C for 10 hours, deoxidizing and drying to obtain a precursor, wherein the cellulose and solvent The mass ratio is 26:100;

[0031] Step 3: heat treatment: pre-carbonization: put the precursor obtained in step 2 into an environment of nitrogen, argon or hydrogen, heat it to 280°C at a heating rate of 10°C / min, and put the precursor obtained in step 2 into Pre-carbonization of the body for 3 hours; secondary carbonization: heat the pre-carbonized product for 6...

Embodiment 2

[0035] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the cellulose described in step 1 is the cellulose extracted from soybean straw biomass.

[0036] The transmission electron micrograph of the graphene that present embodiment 2 prepares is close to the transmission electron micrograph of embodiment 12, as figure 2 shown. The Raman spectrogram of the Graphene prepared in this embodiment 2 is similar to the Raman spectrogram of the Graphene prepared in Example 12, as image 3 shown.

[0037]The size of the graphene obtained in this embodiment is uniform, with a single-layer or multi-layer two-dimensional layered structure, the size is 0.5-2 μm, and the conductivity is above 25000-45000 S / cm; the yield of graphene in this embodiment is 99.9% or more.

Embodiment 3

[0038] Embodiment 3: the difference between this embodiment and embodiment 2 is: the catalyst described in step one is FeCl 2 with FeCl 3 A mix of both.

[0039] The transmission electron micrograph of the graphene that present embodiment 3 prepares is close to the transmission electron micrograph of embodiment 12, as figure 2 shown. The Raman spectrogram of the Graphene prepared in this embodiment 3 is similar to the Raman spectrogram of the Graphene prepared in Example 12, as image 3 shown.

[0040] The size of the graphene obtained in this embodiment is uniform, with a single-layer or multi-layer two-dimensional layered structure, the size is 0.5-2 μm, and the conductivity is above 25000-45000 S / cm; the yield of graphene in this embodiment is 99.9% or more.

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Abstract

The invention provides a preparation method of graphene, and particularly relates to a method for preparing biomass graphene employing cellulose as a raw material. The specific preparation method comprises the following steps: 1, preparing a catalyst solution; 2, carrying out ionic coordination and high-temperature deoxidization on cellulose and a catalyst, so as to obtain a precursor; 3, carrying out thermal treatment; 4, carrying out acid treatment, and drying to obtain the graphene, wherein the prepared graphene is uniform in morphology, has a single-layer or multi-layer two-dimensional layered structure; the dimension is 0.5-2 microns; and the electrical conductivity is 25,000-45,000S/m. The preparation method is simple in preparation technology, low in cost, high in yield, high in production safety, and controllable in product dimension and physical property; industrialized production can be realized; the graphene prepared by the method can be applied to electrode materials of super capacitors and lithium ion batteries, and can also be added to resin and rubber as an additive; and the physical property of the material can be improved.

Description

technical field [0001] The invention relates to a method for preparing graphene, in particular to a method for preparing biomass graphene by using cellulose as a raw material. Background technique [0002] Biomass is a natural cellulosic raw material considered to be the most valuable and abundant renewable resource on earth. In China, the annual production rate of natural cellulose biomass exceeds 700 million tons, of which corncobs and straw account for more than 30%. Biomass is rich in nutritional value and useful chemical components. Although it is widely used in industry, agriculture and animal husbandry, more than 50% of biomass has not been utilized. At present, my country lacks comprehensive measures for the effective utilization of biomass (corncobs and straw, etc.), which often causes serious air pollution, which also leads to frequent occurrence of smog and high concentration of fine particles with a diameter smaller than PM2.5 in the air. important factor. Alth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCB01J27/128B01J27/26C01B32/184B01J27/043C08B15/08G01N21/65
Inventor 付宏刚王蕾唐一林张金柱郑应福蒋保江
Owner HEILONGJIANG UNIV
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