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Preparation method of biochar-based solid acid and application of biochar-based solid acid to cellulose hydrolysis reaction

A hydrolysis reaction and solid acid technology, applied in the field of biomass resource utilization, can solve the problems of high and difficult batch production of equipment, secondary pollution of sulfuric acid, etc., and achieve the effects of low requirements for reaction equipment, low price and wide sources

Inactive Publication Date: 2016-11-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problem of secondary pollution caused by the use of a large amount of sulfuric acid in the existing carbon-based solid acid preparation process, or the high requirements for equipment and difficulty in mass production, the present invention proposes to use cheap biomass as the carrier raw material and synthesize carbon microparticles by "ion heat". spheres, with organic sulfonic acid as acid site donor, through nucleophilic substitution reaction, bio-carbon-based solid catalyst was synthesized under normal pressure, and then used in the hydrolysis reaction of cellulose to prepare reducing sugar

Method used

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  • Preparation method of biochar-based solid acid and application of biochar-based solid acid to cellulose hydrolysis reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First weigh 1g of cellulose and 10g of 1-butyl-3-methylimidazolium chloride ([BMIM]Cl), mix them thoroughly in a three-necked glass flask, and then fix the flask at 120°C in an oil bath with magnetic stirring middle. Stir for 60 minutes, after the cellulose is completely dissolved, raise the temperature to 200°C, add 5g of 4-chlorobenzenesulfonic acid dropwise to carry out the synchronous "carbonization-nucleophilic substitution" reaction for 5 hours, after the reaction, the obtained black solid powder is mixed with water and acetone respectively Alternately washed 5 times each until the pH>6, freeze-dried and then heat-dried to obtain a bio-carbon-based solid catalyst with a yield of 49.3%. The SEM spectrum of the catalyst is attached figure 1 As shown, the BET test results prove that its specific surface area is 350m 2 / g, FT-IR shows that the catalyst has -OH, -COOH and -SO 3 H, the elemental analysis catalyst sulfonic acid group content is 4.6mmol / g.

[0018] In...

Embodiment 2

[0020] First, weigh 1 g of glucose and 10 g of [BMIM]Cl, mix them thoroughly in a three-neck glass flask, and then fix the flask in an oil bath with magnetic stirring at 100°C. Stir for 30 minutes, after the glucose is completely dissolved, raise the temperature to 150°C, add 4.17g of 3-fluoromethanesulfonic acid dropwise to carry out the synchronous "carbonization-nucleophilic substitution" reaction for 5 hours, after the reaction, the obtained black solid powder is mixed with water and acetone respectively Alternately washing each 5 times until pH > 6, freeze-drying and then heat-drying to obtain a biocarbon-based solid acid with a yield of 66.9%. The catalyst BET test results prove that its specific surface area is 420m 2 / g, FT-IR shows that the catalyst has -OH, -COOH and -SO 3 H, elemental analysis catalyst sulfonic acid group content is 4.85mmol / g.

[0021] In a 10ml reactor, add 5.0g [BMIM]Cl, 0.25g cellulose and 0.2g deionized water respectively, stir at 100°C for 3...

Embodiment 3

[0023] First weigh 1g of bamboo powder and 10g of [BMIM]Cl, mix them thoroughly in a three-necked glass flask, and then fix the flask in an oil bath at 120°C with magnetic stirring. Stir for 60 minutes, after the bamboo powder is completely dissolved, raise the temperature to 180°C, add 5.35g of sulfamic acid dropwise to carry out the synchronous "carbonization-nucleophilic substitution" reaction for 5 hours, after the reaction, wash the obtained black solid powder alternately with water and acetone 5 times each until the pH>6, freeze-dried and then heat-dried to obtain a biocarbon-based solid acid with a yield of 53.3%. The catalyst BET test results prove that its specific surface area is 120m 2 / g, FT-IR shows that the catalyst has -OH, -COOH, -NH 3 and-SO 3 H, the elemental analysis catalyst sulfonic acid group content is 1.37mmol / g.

[0024] In a 10ml reactor, add 5.0g [BMIM]Cl, 0.25g cellulose and 0.2g deionized water respectively, stir at 100°C for 30min, the cellulos...

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Abstract

A preparation method of biochar-based solid acid and an application of the biochar-based solid acid to a cellulose hydrolysis reaction belong to the technical field of biomass resource utilization. The preparation method of biochar-based solid acid comprises the following steps: in the normal pressure and temperature and in an air atmosphere, adding organic strong acid in a biomass ionic liquid solution drop by drop, performing a synchronous carbonization and nucleophilic substitution reaction, performing alternative washing with water and acetone, and performing drying to obtain the biochar-based solid acid. The raw biomass is cheap in price and available in resources; the ionic liquid solution is taken as a solvent; and sub-micron carbon sphere carriers high in specific surface area, abundant in surface functional groups and high in acid site capacity are obtained through ionothermal carbonization. Synthesis of the biochar-based solid acid catalyst is conducted in normal pressure and in an air atmosphere and is low in requirements to reaction equipment and simple and easy in operation, and the catalyst in high in yield. The biochar-based solid acid is used for cellulose hydrolysis, is mild in reaction condition and high in yield of reduction sugar and glucose, and can be reused.

Description

technical field [0001] The invention belongs to the technical field of biomass resource utilization, and relates to a preparation method of biological carbon-based solid acid and its application in cellulose hydrolysis reaction. Background technique [0002] The in-depth development and utilization of fossil resources has created a highly developed material civilization. However, the excessive consumption of fossil energy has also caused resource depletion and environmental degradation, posing severe challenges to the survival and development of human society. As a renewable resource, biomass can not only be converted into energy forms, but also shows great potential in the chemical industry. Among them, lignocellulosic raw materials are low in price and large in supply, but they have not been fully developed and utilized. [0003] There is an increasingly urgent demand for the development of efficient technologies for converting lignocellulose into liquid fuels and bulk c...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J35/08C13K1/02C13K5/00C13K7/00C13K11/00
CPCC13K1/02C13K5/00C13K7/00C13K11/00B01J31/0225B01J31/0238B01J35/51B01J35/615
Inventor 郭峰郭晓倩金盈管红伟
Owner DALIAN UNIV OF TECH
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