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Environment-friendly catalysis method for preparing 5-hydroxymethyl furfural in water phase

A technology for the preparation of hydroxymethylfurfural and aqueous phase, which is applied in the fields of materials chemistry, physical chemistry, and organic chemistry. It can solve the problems of large catalyst usage, difficult product separation, and long reaction time, and achieve good cycle performance and convenient repetition. The effect of using

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

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Problems solved by technology

But there are also problems, such as long reaction time, large amount of catalyst used, low initial fructose concentration, unfriendly reaction system to the environment, organic solvent used in the reaction corrodes equipment, difficult separation of products, difficult circulation of catalyst, etc. ( A. A. Rosatella, S. P. Simeonov, R. F. M. Frade and C. A. M. Afonso, Green Chem., 2011, 13, 754.)

Method used

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  • Environment-friendly catalysis method for preparing 5-hydroxymethyl furfural in water phase
  • Environment-friendly catalysis method for preparing 5-hydroxymethyl furfural in water phase
  • Environment-friendly catalysis method for preparing 5-hydroxymethyl furfural in water phase

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Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 0.2g fructose in 9.8g water to prepare a 2% fructose solution. Add 0.05 g of layered niobic acid catalyst into the above fructose solution to obtain a substrate-catalyst mass ratio of 4, and mix evenly. The above reaction system was placed in a microwave heating reactor and heated at 140°C. After reacting for 108 minutes, the sample was taken out and analyzed by liquid chromatography, and the conversion rate of fructose was 78.0%, the selectivity of 5-hydroxymethylfurfural was 50.0%, and the yield of 5-hydroxymethylfurfural was 39.0%.

Embodiment 2

[0024] Dissolve 1g of fructose in 9g of water to prepare a 10% fructose solution. Add 0.05 g of layered niobic acid catalyst into the above fructose solution to obtain a substrate-catalyst mass ratio of 20, and mix evenly. The above reaction system was placed in a microwave heating reactor and heated at 140°C. After reacting for 72 minutes, the sample was taken out and analyzed by liquid chromatography, the conversion rate of fructose was 86.3%, the selectivity of 5-hydroxymethylfurfural was 54.1%, and the yield of 5-hydroxymethylfurfural was 46.7%.

Embodiment 3

[0026] Dissolve 3g of fructose in 7g of water to prepare a 30% fructose solution. Add 0.05 g of layered niobic acid catalyst into the above fructose solution to obtain a substrate-catalyst mass ratio of 60, and mix evenly. The above reaction system was placed in a microwave heating reactor and heated at 140°C. After reacting for 24 minutes, the sample was taken out and analyzed by liquid chromatography, the conversion rate of fructose was 93.7%, the selectivity of 5-hydroxymethylfurfural was 43.7%, and the yield of 5-hydroxymethylfurfural was 41.0%.

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Abstract

The invention belongs to the intersection field of organic chemistry, material chemistry and physical chemistry, and particularly relates to an environment-friendly catalysis method for preparing 5-hydroxymethyl furfural in water phase, wherein the specific steps are as follows: (1) dissolving an initial raw material into water to prepare a solution with the mass percentage of 0.01-90; (2) adding a catalyst into the solution obtained in step (1), mixing uniformly, wherein the mass ratio of the initial raw material to the catalyst is 5000:1-0.01:1; and (3) placing the solution obtained in step (2) into a microwave-heating reactor, heating to 80-240 DEG C, and reacting for 1 second to 360 minutes. The method provided by the invention is capable of efficiently, conveniently, quickly and environmentally obtaining 5-hydroxymethyl furfural. Additionally, the catalysis system has a good recycling property; and the catalyst is easy to separate from 5-hydroxymethyl furfural and can be reused conveniently.

Description

technical field [0001] The invention belongs to the fields intersecting organic chemistry, material chemistry and physical chemistry, and relates to a green catalytic method for preparing biomass-derived platform compounds in water phase, in particular to a green catalytic method for preparing 5-hydroxymethylfurfural in water phase. Background technique [0002] In recent years, due to the rapid depletion and dwindling reserves of fossil fuels, renewable resources have attracted increasing attention. Biomass and biomass-derived compounds are considered to be a promising class of compounds to replace petroleum, and thus a great deal of work has focused on them. Among them, 5-Hydroxymethylfurfural is a biomass-derived platform compound, which has been reported in the literature (X. Tong, Y. Ma and Y. Li, Appl. Catal. A-Gen. , 2010, 385, 1.) referred to as "sleeping giant". 5-Hydroxymethylfurfural has rich functional groups, and can undergo many chemical reactions such as oxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
CPCY02P20/584
Inventor 唐颐武庆斌颜雅妮卢金华杨志剑张亚红
Owner FUDAN UNIV