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
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[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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