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Sulfonic acid functionalized amylose solid acid catalyst as well as preparation method and application thereof

A solid acid catalyst and sulfonic acid functionalization technology, which is applied in the preparation of organic compounds, physical/chemical process catalysts, catalytic reactions, etc., can solve the problems of polluting furfural industry, unstable catalysts, and low yield of furfural. Good practicability and economy, low cost and high catalytic activity

Pending Publication Date: 2018-12-07
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

China's furfural production accounts for more than 60% of the international market. However, the rapid development of my country's furfural industry has not brought about technological innovation. Practical problems such as low furfural yield and high energy consumption have seriously hindered the development of furfural industry. The environmental requirements are particularly high, which has caused great trouble to the polluting furfural industry
Amylose carbon-based solid acid catalysts in the prior art have the technical problem of catalyst instability

Method used

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  • Sulfonic acid functionalized amylose solid acid catalyst as well as preparation method and application thereof
  • Sulfonic acid functionalized amylose solid acid catalyst as well as preparation method and application thereof
  • Sulfonic acid functionalized amylose solid acid catalyst as well as preparation method and application thereof

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Experimental program
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preparation example Construction

[0035] The concrete steps of this synthetic method are:

[0036] 1) Add 20-200 mL of deionized water to 2-8 g of high straight-chain corn starch, heat at 100-130 ° C for 40-50 min to obtain a gel, and place it in a refrigerator at 5 ° C for 24 h. After filtration, the solid is washed with ethanol to obtain rigid porous expanded cornstarch;

[0037] 2) 3-6g of expanded cornstarch, 20-40mL of dry toluene, under the protection of nitrogen, slowly add 4-6g of 3-mercaptopropyl triethoxy silicon dropwise, and react under reflux conditions for 24h, after the reaction , cooled to room temperature, filtered, and subjected to Soxhlet extraction with dichloromethane to obtain thiolated puffed cornstarch;

[0038] 3) 1-5 g of thiolated expanded cornstarch, mixed with 10-50 mL of 30% H 2 o 2 , 1 to 2 drops of concentrated sulfuric acid, react at room temperature for 12 hours, filter after the reaction, and wash with deionized water until neutral to obtain a solid acid catalyst for sulfo...

Embodiment 1

[0042] Preparation of amylose-loaded catalyst:

[0043] Preparation of rigid and porous expanded cornstarch: 5g of high-amylose cornstarch was added to 100mL of deionized water, heated at 120°C for 45min to obtain a gel, and placed in a refrigerator at 5°C for 24h. After filtration, the solid was washed with ethanol to obtain a rigid porous expanded cornstarch.

[0044] Preparation of thiolated expanded cornstarch: 1.00g of expanded cornstarch, 20mL of dry toluene, under the protection of nitrogen, slowly add 5.00g of 3-mercaptopropyl triethoxy silicon, and react under reflux for 24h, After the reaction is finished, cool to room temperature, filter, and perform Soxhlet extraction with dichloromethane to obtain mercaptolated puffed cornstarch;

[0045] Preparation of sulfonic acid functionalized amylose: 5g of mercaptolated expanded cornstarch, mix with 50mL of 30% hydrogen peroxide, add two drops of concentrated sulfuric acid, 15mL of methanol, react at room temperature for 1...

Embodiment 2

[0050] Application of Sulfonic Acid Functionalized Amylose Solid Acid Catalyst:

[0051] Xylose 0.4g, sulfonic acid functionalized amylose solid acid catalyst 0.1g, microwave reaction at 140°C for 30min in 10mL of γ-valerolactone and water mixed solution (volume ratio 1:1), after the reaction, filter The catalyst was removed, and furfural was obtained by distillation under reduced pressure with a yield of 78%.

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Abstract

The invention discloses a sulfonic acid functionalized amylose solid acid catalyst as well as a preparation method and application thereof. The preparation method comprises the steps of puffing linearchain corn starch so as to increase the number of hydroxide radicals on the surface, reacting with 3-mercaptopropyl triethoxysilane so as to obtain sulfhydrylated corn starch, and oxidizing sulfydryl, so as to obtain the sulfonic acid functionalized amylose solid acid catalyst. According to the synthesized solid catalyst, the disadvantages of homogeneous catalysts are overcome, and the synthesized solid catalyst has the advantages of easiness in preparation, environment friendliness, high catalytic activity, capability in repeated use and low cost and is a good solid catalyst for etherification reaction, esterification reaction and ester exchange reaction.

Description

technical field [0001] The invention belongs to the technical field of preparation of solid catalysts, and in particular relates to a preparation method of a sulfonic acid functionalized amylose solid acid catalyst and its product and application. Background technique [0002] Furfural is a key chemical derivative product obtainable from biomass and an important raw material for many chemical products. It can be used to extract high-grade lubricating oil and diesel oil, is a good organic solvent, and can also be used as a raw material to produce fuel and some important chemical products. China's furfural production accounts for more than 60% of the international market. However, the rapid development of my country's furfural industry has not brought about technological innovation. Practical problems such as low furfural yield and high energy consumption have seriously hindered the development of furfural industry. The environmental requirements are particularly high, which h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07D307/46C07D307/48C07C227/10C07C229/30
CPCB01J31/06B01J2231/40C07C227/10C07D307/46C07D307/48C07C229/30
Inventor 洪梅闵洁崔焕贵赵雨欣
Owner NANJING FORESTRY UNIV