Biomass carbon-based solid acid catalyst and preparation method and application thereof

A carbon-based solid acid and biomass technology, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of general cycle effect, low yield of glucose conversion to HMF, etc., and achieve catalytic conversion efficiency High, high catalytic activity, the effect of increasing the loading capacity

Active Publication Date: 2018-12-07
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The existing biomass carbon-based solid acid catalysts have a general cyclic effect, and the initial effect is often only good in the process of catalyzing the preparation of HMF, and generally only contain Brenest acid, and the conversion rate of glucose to HMF is too low

Method used

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  • Biomass carbon-based solid acid catalyst and preparation method and application thereof
  • Biomass carbon-based solid acid catalyst and preparation method and application thereof
  • Biomass carbon-based solid acid catalyst and preparation method and application thereof

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preparation example Construction

[0024] The invention provides a method for preparing a biomass carbon-based solid acid catalyst, comprising:

[0025] A) immersing the biomass of nitrogen-containing compounds in an acid solution, and filtering to obtain a solid product;

[0026] B) carbonizing the solid product to obtain a porous carbon carrier;

[0027] C) reacting the porous carbon carrier with p-aminobenzenesulfonic acid and isoamyl nitrite to obtain a catalyst through sulfonation.

[0028] In the present invention, firstly, the biomass containing nitrogen compounds is soaked in an acid solution.

[0029] The nitrogen-containing compound biomass of the present invention includes but not limited to tobacco stems or bean straws; the embodiment of the present invention uses tobacco stems.

[0030] In the present invention, it is preferred to firstly dry and grind the biomass containing nitrogen compounds at 100-105°C. The present invention does not limit the specific manner of grinding, as long as those sk...

Embodiment 1-4

[0071] Embodiment 1-4. the preparation of catalyst A-D

[0072] Take 10 g of ground tobacco stem powder as a raw biomass material rich in nitrogen-containing compounds, soak it in 45% pyrophosphoric acid solution for 12 hours, the mass ratio of pyrophosphoric acid and tobacco stem is 1.3:1, and then filter the filtrate; Under the protection of an inert gas, carbonize the obtained solid at 350, 400, 450, and 500°C for 1 hour to obtain a black solid. 1~4. In the sulfonation process, a certain amount of porous carbon is first impregnated in water and stirred, then sequentially added p-aminobenzenesulfonic acid and isoamyl nitrite (mass: 2:1) and refluxed at 80°C for 12 hours. After the end, the solid-liquid separation and Washed and dried under vacuum at 80°C for 12 hours to obtain the corresponding catalysts numbered sequentially A-D.

Embodiment 5-8

[0074] Add 0.1g of fructose, 4.7ml of γ-valerolactone, 0.3ml of water, and 0.05g of catalyst into a 15ml pressure-resistant tube, and react for 30min at a speed of 500r / min at a temperature of 130°C. After completion, filter the reaction solution and use HPLC detection of sugar and HMF products. The specific results are shown in Table 1.

[0075] Table 1. The conversion rate of fructose under different catalysis, the yield and selectivity of HMF

[0076] catalyst

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Abstract

The invention provides a preparation method and an application of a biomass carbon-based solid acid catalyst. The preparation method comprises the following steps: A) impregnating biomass of a nitrogen-containing compound in an acid solution, and filtering to obtain a solid product; B) carbonizing the solid product to obtain a porous carbon carrier; and C) reacting the porous carbon carrier with p-aminobenzenesulfonic acid and isoamyl nitrite, and sulfonating to obtain a catalyst. In the preparation method provided by the invention, the biomass of the nitrogen-containing compound is impregnated and carbonized to obtain the porous carbon carrier; and after carbonization, diversified surface chemical compositions have better sulfonic acid group loading property compared with a highly carbonized surface, so that the Bronsted acid loading amount is increased, and the conversion efficiency of various types of sugar is improved. The adjustable and controllable carbon-based carrier porous structure formed in the preparation method provided by the invention enables sulfonic acid groups to be firmly loaded inside pore passages, and the pore passages are mesopores and macropores after loading, thereby being beneficial to contact of a substrate with acid sites, and maintaining better recycling property. The biomass carbon-based solid acid catalyst prepared by the invention has high catalytic activity, good stability and high catalytic conversion efficiency.

Description

technical field [0001] The invention relates to the technical field of biomass chemical utilization, in particular to a biomass carbon-based solid acid catalyst and its preparation method and application. Background technique [0002] As the problems of environmental pollution and energy shortage caused by the use of traditional fossil energy are becoming more and more serious, the production of chemicals and liquid fuels from renewable biomass raw materials has attracted great attention. 5-Hydroxymethylfurfural (HMF) is an important biomass-based platform compound, which can be converted into levulinic acid, 2,5-dimethylfuran, 2,5-furandicarboxylic acid, 2 , 5-furandimethanol, 1,6-hexanediol and maleic anhydride can be used in various chemicals such as medicine, fuel, plastic products and fine chemicals. [0003] 5-Hydroxymethylfurfural is mainly obtained through catalytic dehydration of carbohydrate acids. Carbohydrates can be six-carbon monosaccharides, polysaccharides o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02C07D307/46C07D307/48
CPCB01J27/02C07D307/46C07D307/48Y02P20/584
Inventor 李文志黄锋张听伟安胜欣
Owner UNIV OF SCI & TECH OF CHINA
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