Method for preparing 5-hydroxymethylfurfural (5-HMF) by catalyzing cellulose transformation in green solvent system

A technology of hydroxymethylfurfural and green solvents, which is applied in the development of new catalytic reaction systems, can solve problems such as low stability, difficulty in separation and extraction of 5-HMF, difficulty in separation and regeneration of catalysts, and achieve simple preparation process, easy operation and high efficiency conversion effect

Inactive Publication Date: 2016-11-30
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this type of reaction system usually uses expensive ILs or strong polar aprotic solvents, resulting in the difficulty of separation and regeneration of the catalyst

Method used

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  • Method for preparing 5-hydroxymethylfurfural (5-HMF) by catalyzing cellulose transformation in green solvent system
  • Method for preparing 5-hydroxymethylfurfural (5-HMF) by catalyzing cellulose transformation in green solvent system
  • Method for preparing 5-hydroxymethylfurfural (5-HMF) by catalyzing cellulose transformation in green solvent system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Preparation of biological enzyme catalyst

[0047] 0.1g of FeCl 3 ·6H 2 O and 1.0g of NaAc were added to 30mL of ethylene glycol, and ultrasonically formed a uniformly mixed solution; then 0.2g of dried silicon-based mesoporous molecular sieve SBA-15 was dispersed in the above solution, and mixed with Add 0.4g PEG dropwise to the system, and put the mixed solution into the autoclave. After reacting at 100°C for 6h, the resulting solid is washed with water and ethanol, collected by centrifugation, and vacuum-dried at 40°C to obtain a magnetic Fe-loaded 3 o 4 SBA-15(Fe 3 o 4 @SBA-15).

[0048] Take 10mg of Fe obtained in the previous step 3 o 4 @SBA-15 was dispersed in 1mL of citric acid buffer solution with pH = 2.0. After mixing evenly, 0.4mg of cellulase was added to the mixed system under stirring. After the reaction system was reacted at 0°C for 12h, the obtained product was passed Collected by centrifugation and vacuum dried at 20°C to obtain the biologi...

Embodiment 2

[0068] (1) Preparation of biological enzyme catalyst

[0069] 4.0g of FeCl 3 ·6H 2 Add O and 20g of NaAc into 120mL of ethylene glycol, and ultrasonically form a uniformly mixed solution; then take 5.0g of dried silicon-based mesoporous molecular sieve SBA-15 and disperse it in the above solution. 10g of PEG was added dropwise in the solution, and the mixed solution was added to the autoclave, and reacted at 200°C for 24h. The resulting solid was washed with water and ethanol, collected by centrifugation, and vacuum-dried at 80°C to obtain a magnetic Fe-loaded 3 o 4 SBA-15(Fe 3 o 4 @SBA-15).

[0070] Get 50mg of Fe obtained in the previous step 3 o 4 @SBA-15 was dispersed in 5 mL of buffer solution of citric acid with pH=3.6. After mixing evenly, 2.5 mg of cellulase was added to the mixed system under stirring, and the reaction system was reacted at 5°C for 48 hours. Collected by centrifugation and vacuum-dried at 35°C to obtain the biological enzyme catalyst cellulase...

Embodiment 3

[0080] (1) Preparation of biological enzyme catalyst

[0081] 6.5g of FeCl 3 ·6H 2 Add O and 40g of NaAc into 200mL of ethylene glycol, and ultrasonically form a uniformly mixed solution; then take 10g of dried silicon-based mesoporous molecular sieve SBA-15 and disperse it in the above solution. Add 20g PEG drop by drop, and put the mixed solution into the autoclave. After reacting at 300°C for 48h, the obtained solid is washed with water and ethanol, collected by centrifugation, and vacuum-dried at 120°C to obtain a magnetic Fe-loaded 3 o 4 SBA-15(Fe 3 o 4 @SBA-15).

[0082] Get 100mg of Fe obtained in the previous step 3 o 4 @SBA-15 was dispersed in 10mL, pH=4.8 citric acid buffer solution. After mixing evenly, 5.0mg of cellulase was added to the mixed system under stirring conditions. After the reaction system was reacted at 10°C for 96h, the obtained product was passed Collected by centrifugation and vacuum dried at 50°C to obtain the biological enzyme catalyst ce...

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Abstract

The invention belongs to the field of biomass catalysis, and provides a method for preparing 5-hydroxymethylfurfural (5-HMF) by catalyzing cellulose transformation in a green solvent system. Based on a silicon-based mesoporous molecular sieve SBA-15, a magnetic carrier Fe3O4@SBA-15 is prepared, and the magnetic carrier Fe3O4@SBA-15 is used for preparing a biological enzyme catalyst cellulase-Fe3O4@SBA-15 through loading of cellulase; and through loading of ZrO2/SO4<2-> type solid super acid, a 2SZ@SBA-15 chemical catalyst is successfully prepared. The two catalysts are coupled, the biological enzyme catalyst efficiently catalyzes and degrades the cellulose in an aqueous solution so that glucose is obtained, and in an isopropyl alcohol/water mixed solution, the chemical catalyst catalyzes and degrades the glucose obtained after a reaction so that the 5-HMF is prepared. The series connection of two steps of catalytic reactions can realize the high-efficient transformation from the cellulose to the 5-HMF in the green solvent system.

Description

technical field [0001] The invention relates to the field of development of new catalytic reaction systems, in particular to a method for preparing 5-hydroxymethylfurfural (5-HMF) by catalytic conversion of cellulose in a green solvent system. At the same time, the method can be extended to catalyze a series of Substance transformation to prepare 5-HMF. Background technique [0002] 5-Hydroxymethylfurfural (5-hydroxymethylfurfural, 5-HMF) is a biomass-based platform compound containing active aldehyde groups, hydroxyl groups and furan rings in its structural formula. Many downstream products can be derived through further reactions. It is Key intermediates connecting biomass chemistry and petrochemistry. Currently, the biomass-based carbohydrates used to prepare 5-HMF mainly include fructose, glucose and cellulose. Among them, although the yield of 5-HMF prepared from fructose and glucose is high, the price of raw materials is expensive. At the same time, a large amount of...

Claims

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Application Information

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IPC IPC(8): B01J29/03B01J31/00B01J35/10C07D307/46C12P17/04C12N11/14
CPCB01J29/0333B01J29/035B01J31/003B01J35/0006B01J35/1019C07D307/46C12N11/14C12P17/04
Inventor 张云雷陈瑶李春香闫永胜金佩
Owner JIANGSU UNIV
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