Organic solid catalyst and preparation method thereof

A technology of organic solids and catalysts, applied in organic chemistry, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of limited synthesis and use of acidic catalysts, low stability of HMF, and preparation process Complicated and other issues, to achieve the effect of short time, simple preparation process and easy recycling

Inactive Publication Date: 2015-03-11
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the shortcomings of acid catalysts that have occurred are mainly manifested in: (1) the preparation process is complicated and time-consuming, which limits the large-scale synthesis and use of acid catalysts in this field
(2) The stability of HMF in the reaction system is not high, and it is easy to continue to convert into by-products

Method used

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  • Organic solid catalyst and preparation method thereof
  • Organic solid catalyst and preparation method thereof
  • Organic solid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Preparation of organic solid catalyst

[0030] Add 1g of divinylbenzene to 128g of cyclohexane solvent, stir for 20-30min to make it evenly mixed, drop 0.12g of boron trifluoride ethyl ether (BFEE) into the mixed system, and react at 10°C for 30s , adding 2g of methanol to terminate the reaction; the obtained product was washed with methanol or ethanol and water for 3 to 5 times, and dried under vacuum at 50 to 55°C for 20 to 24 hours to obtain a nanotubular polymer with hydrophobic properties;

[0031] Take 0.25g of the material obtained above, grind it into powder, add it to 50mL of 98% concentrated sulfuric acid solution, stir at 10°C for 2h, and dry it in vacuum at 70-80°C to obtain a nanotube-shaped hydrophobic acidic catalyst.

[0032] Depend on figure 1 a, b It can be seen that the organic solid catalyst before sulfonation is in the shape of a tube, the tube diameter is distributed in 80-100nm, and the two ends of the nanotube are open; figure 1 c It can be...

Embodiment 2

[0044] (1) Preparation of organic solid catalyst

[0045] Add 4g of styrene to 250g of hexane solvent, stir for 20-30min to make it evenly mixed, take 0.48g of BFEE into the mixed system, and react at 25°C for 120s, then add 10g of ethanol to terminate the reaction; Washing with methanol or ethanol and water for 3 to 5 times, drying under vacuum at 50 to 55°C for 20 to 24 hours to obtain a polymer with nanotubular hydrophobic properties;

[0046] Take 0.25g of the material obtained above and grind it into powder, add it to 50mL of 98% concentrated sulfuric acid solution, stir at 30°C for 6h, and vacuum dry at 70-80°C to obtain a nanotubular hydrophobic acidic catalyst.

[0047] (2) Analysis and test of catalytic performance

[0048]Catalytic performance analysis test method is the same as embodiment 1.

[0049] The results show that the yield of HMF is 38.2%, and the reaction time is 0.5h. The catalyst has higher catalytic performance, shorter catalytic time and less catalys...

Embodiment 3

[0054] (1) Preparation of Nanotubular Hydrophobic Acid Catalysts

[0055] Add 8g of vinylbenzyl chloride into 385g of dichloromethane solvent, stir for 20-30min to make it evenly mixed, take 0.96g of BFEE into the mixed system, and react at 40°C for 300s, then add 20g of ethanol to terminate the reaction; The product is washed with methanol or ethanol and water for 3 to 5 times, and dried under vacuum at 50 to 55°C for 20 to 24 hours to obtain a polymer with nanotubular hydrophobic properties;

[0056] Take 0.25g of the material obtained above, grind it into powder, add it to 50mL of 98% chlorosulfonic acid solution, stir at 50°C for 10h, and dry it in vacuum at 70-80°C to obtain a nanotubular hydrophobic acidic catalyst.

[0057] (2) Analysis and test of catalytic performance

[0058] Catalytic performance analysis test method is the same as embodiment 1.

[0059] The results show that the yield of HMF is 37%, and the reaction time is 0.5h. The catalyst has higher catalytic...

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Abstract

Belonging to the field of environment functional materials, the invention provides an organic solid catalyst, and solves the technical problems that in the reaction of preparing 5-hydroxymethylfurfural (HMF) from cellulose, the catalyst dosage is great but the HMF yield is not increased, and HMF further converts into a by-product in the reaction. A nanotube hydrophobic catalyst is prepared by a cationic polymerization method, and acid modification is carried out on the catalyst so as to be used as the catalyst for converting cellulose into HMF.

Description

technical field [0001] The invention belongs to the field of environmental functional materials, in particular to an organic solid catalyst and a preparation method thereof. Background technique [0002] 5-Hydroxymethylfurfural (HMF) is produced by dehydration of glucose or fructose. The molecule contains a furan ring, an aldehyde group and a hydroxymethyl group. Its chemical properties are relatively active, and it can be prepared by oxidation, hydrogenation and condensation reactions. Derivatives are important fine chemical raw materials. In the past few decades, the production of HMF from glucose or fructose has become an important research field to solve the energy crisis. As the most abundant, renewable and carbon-neutral macromolecular polysaccharide polymer in nature, cellulose is the most researched biomass material to replace edible glucose and fructose to produce HMF. The conversion of cellulose to HMF involves three main reactions: (1) conversion of cellobiose t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/10C07D307/46C08F112/36C08F112/08C08F112/14C08F4/14C08F8/36
Inventor 张云雷潘建明高和平殷毅
Owner JIANGSU UNIV
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