One-step hydrothermal synthesis of carbon microspheres solid acid from fructose for catalyzing cellulose hydrolysis

A sugar-based carbon microsphere, cellulose technology, applied in the direction of physical/chemical process catalyst, application, sugar production, etc., can solve the problems of pollution, a large amount of waste gas environment, etc., and achieve a simple process, low temperature and mild reaction conditions. Effect

Inactive Publication Date: 2016-11-16
AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that a large amount of concentrated sulfuric acid is used in the preparation process of the existing active carbon sulfonated solid acid, and a large amount of waste gas and waste liquid are produced at the same time, thereby causing serious pollution to the environment

Method used

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  • One-step hydrothermal synthesis of carbon microspheres solid acid from fructose for catalyzing cellulose hydrolysis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1, preparation and characterization of the invented catalyst:

[0026] The preparation process of the carbon microsphere solid acid catalyst is summarized as follows: 10 g of fructose, 5 g of sulfo-salicylic acid and 60 ml of distilled water were successively added under magnetic stirring, and the stirring was continued for 30 min. Then the mixed solution was transferred into a 100ml stainless steel autoclave lined with polytetrafluoroethylene, sealed and heated to a constant temperature of 150°C for 4 hours, and stirred at a speed of 1000 rpm. After the reaction, the reactor was cooled to room temperature. The resulting black powder was alternately washed with distilled water and ethanol several times (ten times in total, 6 times with water and 4 times with alcohol), and dried at a constant temperature of 80°C for 12 hours to remove all the water to obtain a carbon microsphere solid acid catalyst. The catalyst is characterized by SEM, FT-IR, XRD and element...

Embodiment 2

[0027] Embodiment 2, preparation and characterization of the invented catalyst:

[0028] The preparation process of the carbon microsphere solid acid catalyst is summarized as follows: 10 g of fructose, 10 g of sulfo-salicylic acid and 60 ml of distilled water were successively added under magnetic stirring, and the stirring was continued for 30 min. Then the mixed solution was transferred into a 100ml stainless steel autoclave lined with polytetrafluoroethylene, sealed and heated to a constant temperature of 150°C for 4 hours, and stirred at a speed of 1000 rpm. After the reaction, the reactor was cooled to room temperature. The resulting black powder was alternately washed with distilled water and ethanol several times (ten times in total, 6 times with water and 4 times with alcohol), and dried at a constant temperature of 80°C for 12 hours to remove all the water to obtain a carbon microsphere solid acid catalyst. The catalyst is characterized by SEM, FT-IR, XRD and elemen...

Embodiment 3

[0029] Embodiment 3, the new catalytic process of cellulose hydrolysis:

[0030] Add 0.05g of cellulose and 1g of 1-butyl-3-methylimidazolium chloride salt ionic liquid into a 10ml reactor, dissolve the cellulose at 80°C, then add 0.01g of water and 0.05g of the catalyst synthesized in the present invention , heated to 130°C in a sealed state, reacted for 90 minutes, and then cooled rapidly with an ice-water bath; after taking out the reaction solution and diluting it, the yield of reducing sugar was measured by 3,5-dinitrosalicylic acid method (DNS) to be 62% .

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Abstract

The invention discloses carbon microsphere solid acid formed by one-step fructose hydrothermal synthesis and applied to a catalyzed hydrolysis process of cellulose, and belongs to the field of conversion and utilization of biomass resources and energy. A carbon microsphere solid acid catalyst disclosed by the invention has the molecular formula of CH0.0847O0.523S0.00840. The preparation conditions of the catalyst are mild; through one-pot reaction of fructose and sulfo salicylic acid under the hydrothermal condition of 150 DEG C, the preparation of solid microspheres and the loading of sulfo groups are realized simultaneously; the defects that a large amount of concentrated sulfuric acid is used and a large amount of sulfuric acid waste liquid is produced in a conventional process of preparing the solid acid by soaking the concentrated sulfuric acid by using activated carbon are overcome. The prepared carbon microsphere solid acid has high the catalytic activity on the hydrolysis of the cellulose. The solid acid catalyst has mild preparation conditions, no pollution, no corrosion and high activity, and can be used repeatedly for the hydrolysis of the cellulose. The carbon microsphere solid acid is prepared from the fructose and is applied to efficient hydrolysis of the cellulose; a new way is provided for the high value of the biomass resources.

Description

technical field [0001] The invention belongs to the field of transformation and utilization of biomass resources and energy, and in particular relates to the preparation of carbon microsphere solid acid catalysts by using biomass-based sugars as raw materials by a mild hydrothermal method and its application field. Background technique [0002] Lignocellulosic biomass is a potentially renewable resource that can be converted into liquid fuels and a range of important industrial platform chemicals. Hydrolysis is the key to the development and utilization of lignocellulosic biomass resources. Traditional cellulose hydrolysis methods mainly include acid hydrolysis, enzymatic hydrolysis, supercritical hydrolysis, etc. These methods have disadvantages such as serious corrosion of equipment, high cost, and harsh reaction conditions. . [0003] With the continuous development of green chemistry, solid acid catalysts have attracted people's attention due to their mild catalytic con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18C13K1/02C13K13/00
Inventor 漆新华闫碌碌廉优芬
Owner AGRO ENVIRONMENTAL PROTECTION INST OF MIN OF AGRI
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