Preparation method of high efficient sulfonated carbon solid acid catalyst

A solid acid catalyst, sulfonated carbon technology, applied in the preparation of organic compounds, catalysts for physical/chemical processes, preparation of carboxylate, etc. High and wide application prospects

Active Publication Date: 2011-10-19
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is cumbersome to operate, requires high temperature, inert atmosphere and other synthes

Method used

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  • Preparation method of high efficient sulfonated carbon solid acid catalyst
  • Preparation method of high efficient sulfonated carbon solid acid catalyst
  • Preparation method of high efficient sulfonated carbon solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh the cellulose and benzyl chloride at a mass ratio of 4:1, place them in a stainless steel pressure vessel lined with polytetrafluoroethylene, stir and mix them evenly, react in an oven at 160°C for 24 hours, take them out and cool them, and grind them , filtered and washed with deionized water and ethanol, and the obtained solid was dried in an oven at 90°C; the solid and concentrated sulfuric acid were placed in a stainless steel pressure vessel with a polytetrafluoroethylene liner at a mass ratio of 1:10, and evenly After stirring and mixing, sulfonate in an oven at 160°C for 24 hours, take it out and cool it, grind it, wash it with deionized water and ethanol at 90°C, and dry it in an oven at 90°C to obtain the required catalyst. The surface acid content measured by acid-base titration is 4.59mmol / g, and the sulfonate group content is 1.38mmol / g.

Embodiment 2

[0019] After weighing glucose and phenol according to the mass ratio of 4:2, add a small amount of N,N-dimethylformamide as a solvent, place it in a stainless steel autoclave lined with polytetrafluoroethylene, stir and mix it evenly, and heat it at 160°C React in the oven for 24 hours, take it out to cool, after grinding, filter and wash with deionized water and ethanol, and dry the obtained solid in an oven at 90°C; take this solid and concentrated sulfuric acid in a mass ratio of 1:10 and place it in a belt polymer In a stainless steel autoclave lined with tetrafluoroethylene, after uniform stirring and mixing, react in an oven at 160°C for 24 hours, take it out and cool it, after grinding, wash it with 90°C deionized water and ethanol, and then put it in an oven at 90°C for drying After drying, the desired catalyst is obtained. The surface acid content measured by acid-base titration is 4.18mmol / g, and the sulfonate group content is 1.25mmol / g.

Embodiment 3

[0021] Weigh sucrose and diphenylchloromethane in a mass ratio of 4:2, place them in a stainless steel autoclave lined with polytetrafluoroethylene, stir and mix evenly, react in an oven at 160°C for 24 hours, take them out and cool them, and grind them , filtered and washed with deionized water and ethanol, and the obtained solid was dried in an oven at 90°C; the solid and concentrated sulfuric acid were placed in a stainless steel pressure vessel with a polytetrafluoroethylene liner at a mass ratio of 1:10, and evenly After stirring and mixing, react in an oven at 160°C for 24 hours, take it out and cool it, grind it, wash it with deionized water and ethanol at 90°C, and dry it in an oven at 90°C to obtain the required catalyst. The surface acid content measured by acid-base titration is 4.25mmol / g, and the sulfonate group content is 1.43mmol / g.

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Abstract

The invention relates to a preparation method of a high efficient sulfonated carbon solid acid catalyst. According to the method, biomasses and aromatics, which are treated as reaction monomers, are used to form carbon materials with abundant surface aromatic structures through a solvent heat carbonization method, and are sulfonated by concentrated sulfuric acid to obtain the solid acid catalyst with high acid amount and high stability. The method has the outstanding characteristics that: the biomasses are used as a precursor, the aromatics are introduced, effective aromatic sulfonation is guaranteed through providing a lot of aromatic nuclei, a lot of sulfonic acid groups can be introduced, the sulfonated coal solid acid prepared with the aromatics has a higher catalytic efficiency than sulfonated coal solid acids with no aromatics added, so aromatic adding plays an important role in sulfonation; and the catalyst has the advantages of controllable acid amount, high reaction activity and good stability, can be recovered, performs excellent activity and cyclical stability in a series of organic reactions such as synthesis of biodiesel and fine chemicals, conforms to the requirements of modern society, is environment friendly, and possesses a wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a method for preparing a sulfonated carbon solid acid catalyst, in particular to a method for preparing a carbonaceous solid acid catalyst by sulfonating a carbon material whose surface is rich in aromatic ring structures. Background technique [0002] Carbonaceous solid acid catalysts have the advantages of high catalytic efficiency, good stability, easy recycling and reuse, environmental friendliness, low price and renewability. The surface of carbonaceous solid acid rich in sulfonic acid groups, due to the strong acidity of sulfonic acid groups, it can replace some reactions catalyzed by homogeneous acids such as concentrated sulfuric acid, and can also catalyze some reactions that molecular sieves with lower acidity cannot catalyze. Therefore, the carbonaceous solid acid catalyst can be used in reactions such as esterification reaction, hydrolysis of cellulose, alkylation rea...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/02C07C69/14C07C67/08C11C3/04C10L1/02
CPCY02E50/10
Inventor 任家文彭倩王艳芹卢冠忠郭杨龙郭耘刘晓晖张志刚王筠松龚学庆
Owner EAST CHINA UNIV OF SCI & TECH
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