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Method for preparing self-assembled all-carbon three-dimensional graphene with papermaking black liquor

A paper-making black liquor and self-assembly technology, applied in the direction of graphene, chemical instruments and methods, nano-carbon, etc., can solve the problems of reducing the quality of graphene, low production efficiency of 3D graphene, etc., and achieve the effect of overcoming agglomeration and coking

Active Publication Date: 2017-10-27
GUANGXI ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This artificial (or mechanical) 3D graphene not only has low preparation efficiency, but also inevitably adds other non-carbon components, which reduces the quality of graphene

Method used

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  • Method for preparing self-assembled all-carbon three-dimensional graphene with papermaking black liquor
  • Method for preparing self-assembled all-carbon three-dimensional graphene with papermaking black liquor
  • Method for preparing self-assembled all-carbon three-dimensional graphene with papermaking black liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The method for preparing self-assembled full-carbon three-dimensional graphene with papermaking black liquor in the present invention adopts the technical scheme including the following steps: (1) stirring and separating sediment; (2) vacuum spray drying; (3) mechanical stirring and alkali dissolution; (4) ) Acid neutralization; (5) Ultrasonic pulverization; (6) Liquid nitrogen quick-freeze drying; (7) Moderate temperature curing and setting; (8) Deionized water washing; (9) Constant temperature oven drying; (10) Moderate temperature hydrogen reduction deoxidation ; (11) High temperature carbonization treatment. Only the strict combination of these 11 steps can achieve good results, and the most critical steps of the present invention are steps (7), (8) and (9). Therefore, in order to verify the effect of the preparation scheme of the present invention, in this example In 1, step (7), step (8) and step (9) are omitted. The specific implementation process is as follows:...

Embodiment 2

[0056] Compared with Example 1, the method of preparing self-assembled full-carbon three-dimensional graphene with papermaking black liquor in Example 2 includes the following steps: (1) stirring and separating sediment; (2) vacuum spray drying; (3) mechanical (4) Acid neutralization; (5) Ultrasonic pulverization; (6) Liquid nitrogen quick freeze drying; (7) Medium temperature solidification; (8) Deionized water washing; (9) Constant temperature box drying; ( 10) Medium-temperature hydrogen reduction deoxidation; (11) High-temperature carbonization treatment. The specific implementation process is as follows:

[0057] (1) Take 10 liters of poplar papermaking black liquor and put it into a separation container. After being fully stirred by a stirrer, settle for 3 hours, and discharge the part containing sediment in the lower layer.

[0058] (2) Take the black liquor containing alkali lignin in the upper layer and carry out vacuum spray drying treatment with a vacuum dryer to o...

Embodiment 3

[0071] The method for preparing self-assembled full-carbon three-dimensional graphene with papermaking black liquor in the present invention adopts the technical scheme including the following steps: (1) stirring and separating sediment; (2) vacuum spray drying; (3) mechanical stirring and alkali dissolution; (4) ) Acid neutralization; (5) Ultrasonic pulverization; (6) Liquid nitrogen quick-freeze drying; (7) Moderate temperature curing and setting; (8) Deionized water washing; (9) Constant temperature oven drying; (10) Moderate temperature hydrogen reduction deoxidation ; (11) High temperature carbonization treatment. The specific process is as follows:

[0072] (1) Take 10 liters of eucalyptus papermaking black liquor and put it into a separation container. After being fully stirred by the agitator, settle for 4 hours, and discharge the part containing sediment in the lower layer.

[0073] (2) Take the black liquor containing alkali lignin in the upper layer and carry out v...

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Abstract

The invention discloses a method for preparing self-assembly all-carbon three-dimensional graphene from papermaking black liquid. The method includes the steps of ultrasonically smashing lignin suspension liquid, using liquid nitrogen quick freezing for drying and shape maintenance, conducting medium temperature partial carbonization shaping and solidifying and performing multi-temperature multi-atmosphere procedural deoxidation carbonization treatment. Treated lignin can be kept of a loose and porous three-dimensional structure in the high-temperature carbonization process, coking and caking which are prone to occurring are avoided, the self-assembly all-carbon three-dimensional graphene material with a supporting structure is prepared, all fragments are fused closely, multiple layers are distributed in a three-dimensional mode and support one another, structural stability is enhanced, and the superficial area of graphene is increased.

Description

technical field [0001] The invention relates to the technical field of new graphene materials, in particular to a method for preparing self-assembled full-carbon three-dimensional graphene with papermaking black liquor. Background technique [0002] Lignin is the second largest renewable resource in nature, regenerated at a quality of 50 billion tons per year, but lignin is difficult to be metabolized and degraded by microorganisms, and is often discharged as waste in the biomass industry. my country's paper industry mainly uses various wood and herbaceous plants as raw materials, such as poplar, eucalyptus, reed, wheat straw and bagasse. The paper industry discharges a large amount of foul smelling and toxic black liquor, the main component of which is alkali lignin that cannot be used by microorganisms. It is estimated that the annual discharge of lignin by my country's paper industry is as high as 40 million tons. At present, the main way to deal with the lignin in the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01B2204/32C01P2004/03
Inventor 杜奇石黎演明黄华林唐培朵谢能中黄慨陈东黄日波
Owner GUANGXI ACAD OF SCI
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