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Preparation method of sulfur-carbon-based solid acid catalyst

A solid acid catalyst, sulfur carbon-based technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve high cost, environmental pollution, sulfur-containing carrier Difficult to obtain and other problems, to achieve the effect of increased catalytic activity and safe transportation process

Pending Publication Date: 2020-09-15
TAIYUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to the above literature, people have some problems with the sulfonation method of carbon-based solid acids. To study this process, in order to solve the dangers in the use and transportation of sulfonating agents in the past, the pollution to the environment caused by the sulfonation process, and the sulfonating agent Unstable, some literature shows that sulfur-containing groups can be synthesized by other methods such as sulfonic acid groups, but the sulfur-containing carrier used is difficult to obtain and the cost is high. Under such circumstances, a new method can be developed Preparation of sulfur carbon solid acid, which has excellent catalytic performance and reduces environmental pollution

Method used

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  • Preparation method of sulfur-carbon-based solid acid catalyst

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preparation example Construction

[0028] The preparation method of sulfur-carbon-based solid acid of the present invention, it mixes carbon source and sulfur source and heats, and oxidizes the obtained sulfur-containing carbon carrier with one or more of hydrogen peroxide, peracetic acid, etc., or Alkaline hydrolysis is carried out with sodium hydroxide, potassium hydroxide, etc., and the preparation methods of the sulfur-carbon-based solid acid catalyst of the present invention and these substances are described in detail below.

[0029] The raw materials of the sulfur-carbon-based solid acid of the present invention are the carbon source and the sulfur source. There is no special limitation on the carbon source. In the carbon-based solid acid of the present invention, the carbon source is any carbon-containing substance, such as sugars, lignin, naphthalene , anthracene, pitch, and carbon sources can be used alone or in combination of two or more.

[0030] In the following embodiments of the thiocarbon-based so...

Embodiment 1

[0033] After mixing the cellulose and sulfur evenly in a ratio of 10:1, weigh a certain mass of the mixture and carbonize it at 440°C under nitrogen to obtain a black solid, which is the sulfur-containing carbon carrier; oxidize the obtained sulfur-containing carbon carrier at 4mol / L Alkaline hydrolysis with sodium at 150°C for 6 hours, cooling, washing, filtering, and drying to obtain sulfocarbon-based solid acid; the sulfur content was detected to be 3.0% by analysis, and sulfonic acid was removed from the structure of thiocarbon-based solid acid. In addition to the base, the sulfur carbon-based solid acid generally contains S=O, C-S-C and O=S=O. In a reactor with a condensing reflux device, the sulfur carbon-based solid acid and methanol are in the ratio of 1g: 5ml. React in the heating device of the high-speed magnetic stirring device, react at a temperature of 70°C for 2 hours, and calculate the conversion rate of oleic acid to be 41.2%; then take a quantitative amount of ...

Embodiment 2

[0035] After mixing cellulose and sodium thiosulfate uniformly according to a certain ratio of 2:1, weigh a certain mass of the mixture and carbonize it at 700°C under nitrogen to obtain a black solid that is the sulfur-containing carbon carrier; / L sodium hydroxide was alkaline hydrolyzed at 100°C for 8 hours, cooled, washed, filtered, and dried to obtain a sulfocarbon-based solid acid; the sulfur content was 15.4% as determined by a sulfur analyzer, and the thiocarbon-based solid acid was obtained by XRS analysis. In the structure of solid acid, except for the sulfonic acid group, the structure of sulfur carbon-based solid acid is O=S=O, C-S-C, S-S. In a reactor with a condensation reflux device, mix sulfur carbon-based solid acid and methanol by 1g: The proportion of 5ml was reacted in a heating device with a constant speed magnetic stirring device, and the reaction was carried out at a temperature of 70°C for 2 hours, and the conversion rate of oleic acid was calculated to ...

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Abstract

The invention discloses a preparation method of a sulfur-carbon-based solid acid catalyst. According to the method, a carbon source and a sulfur source are used as raw materials to react to obtain a dark solid product, the dark solid with different sulfur-containing groups is placed in an oxidizing solution or an alkaline solution, the sulfur-carbon-based solid acid catalyst is prepared after reaction, and the solid catalyst has sulfonic acid groups and other sulfur-containing groups.

Description

technical field [0001] The invention relates to a preparation method of a solid acid catalyst, in particular to a preparation method of a sulfur-carbon-based solid acid catalyst. Background technique [0002] At present, carbon-based solid acids are highly valued by people, and the research on carbon-based solid acids is getting more and more in-depth. They can be prepared by relatively simple preparation methods and cheap materials, and have the advantages of low price, little corrosion to the reaction vessel, Low environmental pollution, easy separation, reusable and other advantages. [0003] In order to obtain carbon-based solid acids with stable structure and excellent catalytic performance, most of these raw materials are partially carbonized by two-step method (carbonization-sulfonation), and then processed by sulfuric acid, oleum, chlorosulfonic acid, diazonium salt, etc. Preparation of carbon-based solid acid catalysts by sulfonation; but generally speaking, there ...

Claims

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Application Information

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IPC IPC(8): B01J27/02B01J27/22B01J31/02B01J35/10
CPCB01J27/02B01J27/22B01J31/0218B01J31/022B01J31/0225B01J31/0222B01J31/0229B01J35/613
Inventor 申曙光景帅旗马雪平周子健李静王翠潘华杰郭晨源郭红生范济民
Owner TAIYUAN UNIV OF TECH
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