Preparation method of xylogen-based magnetic solid acid catalyst

A magnetic solid acid, lignin-based technology, applied in the direction of organic chemistry, can solve the problems of difficult separation and recycling of carbon-based solid acids, the inability to achieve large-scale production, complicated preparation procedures, etc., and achieve good catalytic effect and low production cost. The effect of low cost and simple preparation process

Inactive Publication Date: 2015-05-20
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation procedures of these solid acids are very complicated, and most of the raw materials are relatively expensive, which is far from meeting the requirements of large-scale production.
In addition, the widely studied carbon-based solid acid catalysts

Method used

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  • Preparation method of xylogen-based magnetic solid acid catalyst
  • Preparation method of xylogen-based magnetic solid acid catalyst
  • Preparation method of xylogen-based magnetic solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Weigh 20 g of residual lignin from enzymatic hydrolysis of corncobs, wash 12 times with deionized water and absolute ethanol, and dry in vacuum at 105 °C for 8 h; grind the residual lignin from enzymatic hydrolysis after washing and drying to a size of 200 mesh , and it was added to a concentration of 20 mmol·L according to the solid-liquid ratio of 1:50 -1 Stir in the ferric chloride solution for 10 h, then heat to evaporate the excess water in the solution, and the remaining solid mixture is vacuum-dried at 105 °C for 8 h; impregnate the dried enzymatic residue lignin with ferric chloride and continue grinding To a size of 200 mesh, carbonize it at 600 °C under nitrogen atmosphere for 1 h; add the carbonized lignin-based magnetic carbon carrier to sulfallic acid at a solid-to-solid ratio of 1:10, and stir at 200 °C under nitrogen atmosphere Heated for 5 h; the sulfonated lignin-based magnetic carbon carrier was washed with deionized water at 100 °C until ...

Embodiment 2

[0023] Example 2: Weigh 10 g of residual lignin from enzymatic hydrolysis of corn stalks, wash with deionized water and absolute ethanol for 6 times, and dry in vacuum at 65 °C for 24 h; grind the lignin from enzymatic hydrolysis residue after washing and drying to 100 mesh size , and it was added to a concentration of 10 mmol·L according to the solid-liquid ratio of 1:100 ?1 Stir in the ferric chloride solution for 5 h, then heat to evaporate the excess water in the solution, and dry the remaining solid mixture in vacuum at 65 °C for 24 h; impregnate the dried enzymatic residue lignin with ferric chloride and continue grinding to a size of 100 mesh, carbonize it at 400 °C for 5 h under a nitrogen atmosphere; add the carbonized lignin-based magnetic carbon carrier to thioglycolic acid at a solid-to-liquid ratio of 1:20, and stir at room temperature for 24 h under a nitrogen atmosphere. After filtration, it was added to 30% hydrogen peroxide at a solid-to-liquid ratio of 1:20...

Embodiment 3

[0024] Example 3: Weigh 15 g of enzymolysis residue lignin, wash with deionized water and absolute ethanol 8 times respectively, and vacuum-dry at 80 °C for 12 h; grind the enzymolysis residue lignin after washing and drying to 400 mesh size, and It was added according to the solid-liquid ratio of 1:80 to a concentration of 25 mmol L ?1 Stir in the ferric chloride solution for 8 h, then heat to evaporate the excess water in the solution, and the remaining solid mixture is vacuum-dried at 80 °C for 12 h; impregnate the dried enzymatic residue lignin with ferric chloride and continue grinding To 400 mesh size, carbonize it at 500 °C for 3 h under nitrogen atmosphere; add the carbonized lignin-based magnetic carbon carrier to mercaptopropionic acid at a solid-to-liquid ratio of 1:15, and stir at room temperature for 12 h under nitrogen atmosphere , after filtration, it was added to concentrated nitric acid at a solid-to-liquid ratio of 1:15, and stirred at room temperature for ...

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Abstract

The invention discloses a preparation method of a xylogen-based magnetic solid acid catalyst. According to the method, xylogen which is enzymolysis residue is used as raw material and is sequentially subjected to pretreatment, dipping, carbonization and sulfonation to obtain xylogen-based magnetic solid acid catalyst. The preparation method of the xylogen-based magnetic solid acid catalyst has the advantages that the raw material price is low, the preparation cost is low, the prepared catalyst has the advantages of large specific surface area, high acid load, good thermal stability, has relatively high catalytic activity in cellulose hydrolyzation reaction, fructose cellulose hydrolyzation and 5-hydroxymethylfurfural etherification reaction and can be reused after being simply magnetically seperated.

Description

technical field [0001] The invention belongs to the field of solid catalyst preparation, and relates to a preparation method of a solid acid catalyst, in particular to a preparation method of a lignin-based magnetic solid acid catalyst. Background technique [0002] At present, in the process of biomass conversion and utilization, the hydrolysis reaction of cellulose, the dehydration reaction of fructose and the etherification reaction of hydroxymethylfurfural have become the hot research fields of many scientists, and it needs to be pointed out that the acid catalyst It plays a vital role in the above three types of chemical reactions, and is the core and key to restrict their smooth progress. [0003] Traditional acid catalysts are mostly some liquid inorganic acids such as HCl, H 2 SO 4 、HNO 3 and H 3 PO 4 These inorganic acids not only have low catalytic activity, but also have disadvantages such as corrosion of equipment, difficulty in recycling, and environmental ...

Claims

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Application Information

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IPC IPC(8): B01J27/02C07D307/46
Inventor 胡磊吴真周守勇徐继明
Owner HUAIYIN TEACHERS COLLEGE
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