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Nano spherical carbon-based solid acid taking lignin as raw material as well as preparation method and application thereof

A carbon-based solid acid and nanosphere technology, applied in the field of nano-carbon materials, can solve the problems of low surface area, hindering the activity of carbon-based solid acid, and low porosity, and achieve high carbon content, easy separation, and low equipment corrosion Effect

Pending Publication Date: 2019-11-22
DALIAN POLYTECHNIC UNIVERSITY
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] Traditional carbon-based solid acids have disadvantages such as low porosity and low surface area, which may hinder the activity of carbon-based solid acids, so carbon-based solid acids need to be developed to improve catalytic performance

Method used

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  • Nano spherical carbon-based solid acid taking lignin as raw material as well as preparation method and application thereof
  • Nano spherical carbon-based solid acid taking lignin as raw material as well as preparation method and application thereof
  • Nano spherical carbon-based solid acid taking lignin as raw material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 0.1g of industrial lignin and place it in a 250ml beaker, add 20ml of acetone to obtain a 5mg / ml lignin in acetone solution. 80ml of deionized water was slowly added dropwise therein and stirred continuously at normal temperature and pressure to obtain a lignin nanomicelle solution. Then freeze-dry the lignin micellar solution to obtain lignin nanosphere powder. Disperse 0.1g of lignin nanosphere powder in 3ml of deionized water, put it into a polytetrafluoroethylene tank, put it in an oil bath for hydrothermal carbonization at 260°C for 10h, and suction filter the carbonized product. After washing with deionized water and drying, lignin carbon nanospheres are obtained. Mix 0.1g lignin nanocarbon spheres and 2ml concentrated sulfuric acid in a polytetrafluoroethylene tank, carry out sulfonation at 150°C for 6h, filter the black liquid after sulfonation, and wash the black liquid repeatedly with boiled deionized water product until the filtrate is neutral. That ...

Embodiment 2

[0032] Weigh 1 g of alkali lignin into a 25 ml flask, and then add 5 ml of acetic anhydride to obtain a lignin acetic anhydride solution. Put the flask into a water bath and heat it at a temperature of 90°C for 2 hours. After the reaction is completed, the solution is suction-filtered, washed with deionized water, and dried to obtain acetylated lignin. 0.1 g of acetylated lignin was weighed and placed in a 250 ml beaker, and 20 ml of tetrahydrofuran was added to obtain a 5 mg / ml lignin tetrahydrofuran solution. 80ml of deionized water was slowly added dropwise therein and stirred continuously at normal temperature and pressure to obtain a lignin nanomicelle solution. Then freeze-dry the lignin micellar solution to obtain lignin nanosphere powder. Disperse 0.1g of lignin nanosphere powder in 3ml of deionized water and put it into a polytetrafluoroethylene tank, put it in an oil bath for hydrothermal carbonization at 240°C for 10h, and suction filter the carbonized product to ...

Embodiment 3

[0034] Add 1g of alkali lignin into a 25ml round bottom flask, then add 5ml of acetyl chloride and 10ml of glacial acetic acid, heat the flask in a water bath at 40°C for 2h, after the reaction is over, filter the solution with suction, wash with deionized water, and dry , to obtain acetylated lignin. 0.1 g of acetylated lignin was weighed and placed in a 250 ml beaker, and 20 ml of dimethylamide was added to obtain a 5 mg / ml lignin dimethylamide solution. 80ml of deionized water was slowly added dropwise therein and stirred continuously at normal temperature and pressure to obtain a lignin nanomicelle solution. Then freeze-dry the lignin micellar solution to obtain lignin nanosphere powder. Disperse 0.1g of lignin nanosphere powder in 3ml of deionized water and put it into a polytetrafluoroethylene tank, put it in an oil bath for hydrothermal carbonization at 240°C for 10h, and suction filter the carbonized product to remove After washing with ion water and drying, lignin c...

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Abstract

The invention belongs to the field of nanometer material catalysis, and particularly discloses a method for preparing nanometer spherical carbon-based solid acid by taking lignin as a raw material. The method comprises the following steps: dissolving the modified or unmodified lignin in an organic solvent, and adding water, so that the lignin is self-assembled to obtain lignin nano colloidal spheres; drying the lignin nano colloidal spheres, then dispersing the dried lignin nano colloidal spheres into a certain volume of water, filling a polytetrafluoroethylene tank with the mixture, carryingout hydrothermal carbonization, and carrying out suction filtration, washing and drying on the carbonized product; and putting the dried lignin nano carbon spheres and a certain volume of concentratedsulfuric acid into a polytetrafluoroethylene tank for sulfonation, and carrying out suction filtration, washing and drying on the sulfonated product to obtain the lignin nano spherical carbon-based solid acid. The carbon-based solid acid can replace sulfuric acid for application in an acid catalytic reaction, and has the advantages of being green, regenerable and low in corrosion to equipment andthe like.

Description

technical field [0001] The invention belongs to the field of nano-carbon materials, and in particular relates to a nano-spherical carbon-based solid acid using lignin as a raw material, a preparation method and application thereof. Background technique [0002] At present, most industrial production still uses inorganic acids such as sulfuric acid as catalysts, which are low in cost and fast in reaction, but there are also problems such as corrosion of reaction equipment, many by-products, difficulty in separating the product from the catalyst, and difficulty in recycling the catalyst. Aiming at the limitations of homogeneous catalysts, solid acids have attracted more and more attention. Carbon-based solid acid is a new type of high-efficiency solid protonic acid synthesized by introducing sulfonic acid groups on the surface of carbon materials after incomplete carbonization. The solid acid can replace the liquid acid and is widely used in hydrolysis, esterification, conden...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J35/08B01J37/08C07C67/08C07C69/24C07H1/00C07H3/02
CPCB01J27/02B01J37/084C07C67/08C07H1/00C07H3/02B01J35/23B01J35/51C07C69/24
Inventor 韩颖马子豪王兴孙广卫李尧郭延柱王海松
Owner DALIAN POLYTECHNIC UNIVERSITY
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