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A method for preparing 5-hydroxymethylfurfural by dehydration of fructose

A technology of fructose and hydrophobic groups, which is applied in the field of catalytic application of nanomaterials, can solve the problems of reducing selectivity and hindering the continued reaction of substrate molecules, and achieve the effect of increasing conversion rate, increasing yield, and facilitating adsorption

Active Publication Date: 2016-04-06
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The surface of traditional acidic catalysts is hydrophilic, and the water produced by dehydration of fructose will be adsorbed on the surface of the catalyst, which will easily lead to the degradation of the generated HMF or polymerization into huminous matter, hindering the continued reaction of substrate molecules and reducing selectivity

Method used

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  • A method for preparing 5-hydroxymethylfurfural by dehydration of fructose
  • A method for preparing 5-hydroxymethylfurfural by dehydration of fructose
  • A method for preparing 5-hydroxymethylfurfural by dehydration of fructose

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1 Material A (SpPh-SiO 2 (15,15)) preparation

[0023] Take 20g Np-12, 25g cyclohexane, 5g water, 2g ammonia water (25-28%) and 3g n-octanol and mix to obtain solution A; 0.2g 3-mercaptopropyltrimethoxysilane (precursor of acidic group), Mix 1g tetraethyl orthosilicate and 0.2g phenyltriethoxysilane (hydrophobic silane) to obtain solution B; add solution B to solution A under vigorous stirring, and age for 8 hours; then, add 10mL ethanol and stir vigorously for 30min , centrifuged to obtain a white powder; add 60mL ethanol to the solid, heat and stir for 15min, and centrifuge; repeat this step several times until the surfactant is removed; add 20mL ethanol and 1g mass concentration of 30% hydrogen peroxide to the solid, stir 2h. Centrifuge to obtain a white solid, add 10 mL of 1M sulfuric acid solution, stir for 3 hours, and centrifuge to obtain a white solid powder. Add 30mL of distilled water to it, stir for 30min, centrifuge, repeat this step several ti...

Embodiment 2

[0025] The preparation of embodiment 2 material B-E

[0026] The preparation method of material B-E is the same as that of material A, the difference lies in the type and content of the selected organosilane, the specific type of organosilane used is shown in Table 1, and the obtained materials are listed in Table 1.

[0027] Table 1 Types of organosilanes used in the preparation of materials B-E

[0028]

Embodiment 3

[0030] The synthesized 0.025gSpEt-SiO 2 The catalyst of (10,15) was added to 5mL DMSO, 0.5g fructose was added, heated to 80°C in an oil bath, and reacted in air for 5h. After the reaction, the content of fructose was analyzed by HPLC, and the conversion rate was 92%. The yield of HMF was quantified by GC, and the yield was 80%.

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Abstract

The invention discloses a novel method for preparing 5-hydroxymethyl furfural (HMF) through dehydration of fructose. According to the method, a silicon dioxide-base hydrophobic nano solid acid material which is taken as a catalyst is applied to a process of preparing the HMF through dehydration of fructose. The material, due to surface hydrophobicity and acid site, is favorable for promoting efficient implementation of reaction, thus achieving high fructose conversion rate and HMF selectivity.

Description

technical field [0001] The invention belongs to the catalytic application of nanometer materials, and specifically applies a silicon dioxide-based hydrophobic nanometer solid acid material to fructose dehydration reaction to obtain HMF with high efficiency and high selectivity. Background technique [0002] With the decrease of fossil resources, the development of substitutes for fossil resources is a subject of common concern to mankind. Compared with new energy sources such as wind energy and solar energy, biomass resources are particularly important because they can be converted into fine chemicals and then replace the existing petrochemical routes. HMF, namely 5-hydroxymethylfurfural, is an important platform compound in the catalytic conversion of biomass to chemicals, which can be further converted into 2,5-furandicarbaldehyde, 2,5-furandicarboxylic acid, 2 ,5-Dimethylfuran and maleic anhydride and other downstream products. These downstream products can be utilized ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46B01J31/02
CPCB01J31/0225B01J31/0231B01J2231/70C07D307/46
Inventor 徐杰石松陈晨王敏贾秀全郑玺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI