Method for preparing graphene by utilizing black-liquor rough lignin

A technology of lignin and graphene, applied in graphene, nano-carbon and other directions, can solve the problems of easy agglomeration, long sintering time, and uneven size of carbon source, and achieve the effect of reducing dosage, small size and reducing production cost.

Active Publication Date: 2017-10-10
CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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Problems solved by technology

[0033] The purpose of the present invention is to provide a method for preparing graphene by using black liquor crude lignin, so as to solve the problem of uneven size of the carbon source mentioned in the prior art, waste liquid treatment and sintering process generated in the pre-treatment of raw materials. Technical problems of long sintering time and easy agglomeration

Method used

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  • Method for preparing graphene by utilizing black-liquor rough lignin

Examples

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Example Embodiment

[0060] Example 1:

[0061] 1) The crude lignin extracted from the papermaking black liquor by acid deposition or electrolysis is used as raw material, crushed to below 80 mesh, and washed repeatedly with deionized water until the washing liquid is neutral.

[0062] 2) Centrifugal separation on a centrifuge at a speed of 4000 revolutions / min for 30 minutes, filter and separate the neutral crude lignin.

[0063] 3) The separated crude lignin is placed in a vacuum drying oven at 70° C. and dried to a moisture content of about 8%, and then ground into a powder with a particle size of less than 40 mesh.

[0064] 4) Weigh 8g of the above lignin powder, add 0.4g KOH and 40g deionized water to completely dissolve the lignin. After stirring for 0.5h in a magnetic stirrer, it was filtered, and the filtrate was placed in an evaporating dish and dried to absolute dryness at a temperature of 50°C to obtain a load K + 5g of alkali lignin is taken as the raw material for the preparation of graphene.

Example Embodiment

[0070] Example 2:

[0071] 1) The crude lignin extracted from the papermaking black liquor by acid deposition or electrolysis is used as raw material, crushed to below 80 mesh, and washed repeatedly with deionized water until the washing liquid is neutral.

[0072] 2) Centrifugal separation on a centrifuge at a speed of 4000 revolutions / min for 30 minutes, filter and separate the neutral crude lignin.

[0073] 3) The separated crude lignin is placed in a vacuum drying oven at 70° C. and dried to a moisture content of about 5%, and then ground into a powder with a particle size of less than 40 mesh.

[0074] 4) Weigh 8g of dried lignin powder, add 0.5g NaOH and 40g deionized water to completely dissolve the lignin. Stir in a magnetic stirrer for 1 hour and then filter. Place the filtrate in an evaporating dish and dry it to absolute dryness at 60°C to obtain a loaded Na + 5g of alkali lignin is taken as the raw material for the preparation of graphene.

[0075] 5) Configure the composite

Example Embodiment

[0080] Example 3:

[0081] 1) The crude lignin extracted from the papermaking black liquor by acid deposition or electrolysis is used as raw material, crushed to below 80 mesh, and washed repeatedly with deionized water until the washing liquid is neutral.

[0082] 2) Centrifugal separation on a centrifuge at a speed of 4000 revolutions / min for 30 minutes, filter and separate the neutral crude lignin.

[0083] 3) The separated crude lignin is placed in a vacuum drying oven at 70° C. and dried to a moisture content of about 5%, and then ground into a powder with a particle size of less than 40 mesh.

[0084] 4) Weigh 8g of dried lignin powder, add 0.75g KOH and 50g deionized water to completely dissolve the lignin. Stir in a magnetic stirrer for 1 hour and then filter. Place the filtrate in an evaporating dish and dry it to absolute dryness at 65°C to obtain a load K + 5g of alkali lignin is taken as the raw material for the preparation of graphene.

[0085] 5) The composite expansion ca

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Abstract

The invention provides a method for preparing graphene by utilizing black-liquor rough lignin. The method comprises the following steps: taking the paper-making black-liquor rough lignin extracted according to an acid deposition or electrolytic process as a raw material; drying and then preparing alkali lignin by mixing lignin and KOH or NaOH at the mass ratio of 20:(1-5); preparing a compound expanding catalyst by mixing calcium salt, borate, nickel salt and a swelling agent at the mass ratio of (3-6):(6-3):(1-2):(1-3); and adding the compound expanding catalyst into the alkali lignin, placing into a vacuum sintering furnace, keeping the temperature under atmosphere protection and sintering for 0.5-4h and then cooling to room temperature, thereby obtaining a sample. In the process of preparing the graphene, the compound expanding catalyst is used, and the compound catalyst is sintered at high temperature and can reduce the graphitizing temperature and reduce the requirement for production equipment; only little nickel salt is used, so that the content of magnetic oxide is reduced, and the later purification and separation are benefited; and the swelling agent can prevent caking and is beneficial to the forming of a thinner carbon layer, so that the generation of a graphene slice is benefited.

Description

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Claims

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Application Information

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Owner CENTRAL SOUTH UNIVERSITY OF FORESTRY AND TECHNOLOGY
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