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A kind of polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method and application

A technology of solid acid catalysts and polymers, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low acid density and small specific surface area, etc. Achieve the effects of low corrosion loss, high specific surface area and cost reduction

Active Publication Date: 2018-03-23
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a solid acid catalyst with high acid density and large specific surface area in order to overcome the shortcomings of low acid density and small specific surface area. Polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method, as well as the application of catalyzing the esterification reaction of long-chain fatty acid and short-chain alcohol and catalyzing the "one-pot method" of high acid value oil and short-chain alcohol to prepare biodiesel

Method used

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  • A kind of polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method and application
  • A kind of polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method and application
  • A kind of polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Example 1 Synthesis of polysulfonic acid functionalized mesoporous polymer solid acid

[0046] Proceed as follows:

[0047] (1) Add 2 g of divinylbenzene and 0.05 g of azobisisobutyronitrile to a mixed solution of 2 mL of water in 20 mL of tetrahydrofuran, stir at room temperature for at least 3 h, and then transfer to a polytetrafluoroethylene substrate Heat treatment at 100°C for 24 h in a pressure reaction vessel, after the temperature dropped to room temperature, open the cover, and evaporate the solvent at room temperature to obtain polydivinylbenzene (PDVB) with mesoporous structure;

[0048] (2) Grind 2 g of mesoporous polydivinylbenzene into 200-mesh powder, add 30 mL of chloromethyl methyl ether to the powder, add 7 g of anhydrous aluminum chloride under ice bath, transfer to room temperature, Stir for 24 h. After the reaction, add water to the system, filter the product, wash with water and acetone, and dry in vacuum at 80 °C to obtain mesoporous polydivinylb...

Embodiment 2

[0051] Example 2 Application of polysulfonic acid functionalized mesoporous polymer solid acid catalyzed esterification reaction of oleic acid and methanol in preparation of biodiesel.

[0052] In autoclave, add 6.8 g methyl alcohol and 2 g oleic acid (the mol ratio of alcohol and fatty acid is 30:1), then add 0.08 g polysulfonic acid functionalization mesoporous polymer solid acid catalyst (catalyst amount is 4% of fatty acid quality %), at a temperature of 100 °C, stirred for 4 h, after the reaction, filtered, the filtrate was rotary evaporated to remove unreacted methanol, and Na 2 SO 4 Dry to obtain crude biodiesel. The conversion rate of oleic acid was calculated by acid-base titration, and the conversion rate of oleic acid was calculated to be 98.0%.

Embodiment 3

[0053] Example 3 Application of polysulfonic acid-functionalized mesoporous polymer solid acid catalyzed jatropha oil and methanol in the "one-pot" preparation of biodiesel.

[0054] Add 3.5 g methyl alcohol and 2 g Jatropha oil (the mol ratio of alcohol and Jatropha oil is 50:1) in autoclave, add 0.1 g polysulfonic acid functionalized mesoporous polymer solid acid catalyst again (catalyst amount 6% of the fatty acid mass), at a temperature of 160 °C, stirred and reacted for 8 h, after the reaction was completed, petroleum ether was added, filtered, the filtrate was separated, the supernatant was taken, and petroleum ether and unreacted methanol were removed by rotary evaporation. use Na 2 SO 4 Dry to obtain crude biodiesel. The content of biodiesel was calculated by gas chromatography, and the content of biodiesel was calculated to be 78.4%.

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Abstract

The invention discloses a multi-sulfonic acid funtionalized mesoporous polymeric solid acid catalyst and a preparation method thereof and an application of the catalyst in high-efficiency catalysis of an esterification reaction between free fatty acid and short-chain alcohols (ethanol and methanol) and catalysis of one-pot preparation of biodiesel from high acid-value grease and methanol. The preparation method of the catalyst comprises the following steps: mesoporous polydivinylbenzene is used as a carrier, and the carrier firstly reacts with chloromethyl methyl ether to introduce the carrier into chloromethylene; then, a product reacts with ethene diamine to make the carrier to be linked in the form of a covalent bond with ethene diamine; and finally, chlorosulfonic acid is used to carry out sulfonation so as to obtain the multi-sulfonic acid funtionalized mesoporous polymeric solid acid catalyst. The mesoporous polymeric solid acid catalyst obtained by the preparation method has a lot of mesoporous pore structures, large specific surface area and pore volume and high acid density. The catalyst is applied in catalysis of an esterification reaction between free fatty acid and short-chain alcohols (ethanol and methanol) and catalysis of one-pot preparation of biodiesel from high acid-value grease and methanol, and has a high catalytic activity. Thus, the catalyst has good industrial application value.

Description

technical field [0001] The invention relates to a polysulfonic acid functionalized mesoporous polymer solid acid catalyst and its preparation method, and its catalyzing the esterification reaction of long-chain fatty acids and short-chain alcohols and the "one-pot method" of catalyzing high acid value oil and methanol to prepare biological Diesel applications. The invention relates to the fields of material chemistry, green synthesis technology of esterification reaction and transesterification reaction in organic synthesis, environmental protection and renewable energy preparation technology. Background technique [0002] With the development of the world economy, global oil resources are decreasing day by day, and the combustion of fossil fuels has caused environmental problems. Under this background, renewable and clean energy has attracted great attention from all countries in the world. Biodiesel is a clean, environmentally friendly and renewable energy that replaces p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06C11C3/04C11C3/10C10L1/02C08F112/36C08F8/36C08F8/24C08F8/32
CPCY02E50/10
Inventor 杨松潘虎薛伟胡德禹张衡周磊常飞周全刘晓芳
Owner GUIZHOU UNIV
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