Method for preparing 5-hydroxymethylfurfural with fructose

A technology of hydroxymethylfurfural and fructose, which is applied in the field of biomass green conversion and synthesis of compounds, can solve problems such as equipment corrosion, high viscosity of ionic liquids, and limitations in laboratory research, and achieve mild reaction conditions, low equipment corrosion and environmental friendly effect

Inactive Publication Date: 2011-08-17
海宁市袁花镇工业投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are some literature reports on the preparation of 5-hydroxymethylfurfural from six-carbon sugar: the Chinese patent application with application number CN200910228921.2 discloses a preparation of isomerase/dilute hydrochloric acid coupling catalyzed glucose to prepare 5-hydroxymethylfurfural The method, the steps of the method are as follows: firstly add sodium borate and immobilized glucose isomerase to the glucose solution to react, then filter, recover the isomerase to obtain a mixed solution of glucose and fructose, add hydrochloric acid, Sodium chloride and n-butanol carry out acid-catalyzed synthesis of 5-hydroxymethylfurfural; the disadvantage of this method: the price of isomerase is relatively expensive, and in the reaction process, the temperature is not easy to control, and the activity of the enzyme is easy to fail
A Chinese patent application with the application number CN 200810011726.X discloses a method for preparing 5-hydroxymethylfurfural. The patent uses a saturated sodium chloride-n-butanol system as a reaction solvent, phosphotungstic acid as a catalyst, and fructose Converted to 5-hydroxymethylfurfural; the disadvantage of this method: the catalyst phosphotungstic acid is not easy to recycle, and the product yield is not very high
The Chinese patent application with the application number CN200710158825.6 discloses a method for preparing 5-hydroxymethylfurfural.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of catalyst: 1 part by weight of butyl titanate (Ti(OC 4 h 9 )) was dissolved in 1.3 parts by weight of absolute ethanol, and 1 part by weight of water was added within 0.5h to hydrolyze butyl titanate to obtain stable TiO 2 gel. Then TiO 2 After drying the gel at 80°C for 3h, put it in a muffle furnace and keep it warm (fired) at 500°C for 10h, take it out, cool it down to room temperature naturally, and grind it to get TiO 2 active carrier. Then, the TiO 2 The active carrier is added to the phosphomolybdic acid aqueous solution with a concentration of 15% by mass and immersed for 36 hours, wherein TiO 2 The mass ratio to phosphomolybdic acid is 1:2, take it out and dry it at 80°C, and then place it in a muffle furnace at 150°C for activation for 3 hours to obtain the required catalyst: phosphomolybdic acid supported on titanium dioxide, namely H 3 PMo 12 o 40 / TiO 2 .

Embodiment 2

[0030] Except that phosphomolybdic acid is replaced by silicomolybdic acid, all the other operations are the same as in Example 1, and the required catalyst is obtained: the silicomolybdic acid supported by titanium dioxide, i.e. H 4 SiMo 12 o 40 / TiO 2 .

Embodiment 3

[0032] Except that phosphomolybdic acid is replaced by phosphotungstic acid, the other operations are the same as in Example 1, and the required catalyst is obtained: phosphotungstic acid supported on titanium dioxide, i.e. H 3 PW 12 o 40 / TiO 2 .

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural with fructose. The method includes the following steps: taking N, N-dimethyl acetamide as solvent, lithium chloride as additive, fructose as a reaction material, and heteropoly acid loaded by titanium dioxide as a catalyst, reacting at the temperature of 80-150DEG C to generate 5-hydroxymethylfurfural. The method has the characteristics of few by-products, high yield, environment-friendly property, moderate reaction conditions, small corrosion to equipment, recyclability of catalyst, and the like, and has industrial prospect.

Description

technical field [0001] The invention relates to the field of biomass green conversion synthetic compounds, in particular to a method for preparing 5-hydroxymethylfurfural from fructose. Background technique [0002] At present, most of the energy and organic chemical raw materials needed in the world come from petroleum, coal and natural gas. These fossil resources have made great contributions to social development and economic prosperity. However, with the gradual depletion of non-renewable fossil energy and in order to achieve the purpose of sustainable development of human beings, making full use of renewable and degradable resources and making them an important industrial raw material through chemical synthesis is the solution to resource depletion and environmental pollution. effective means. Biomass resources have large reserves, are renewable, and are low in cost. Through chemical synthesis, high value-added pharmaceutical intermediates and monomers for synthetic p...

Claims

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Application Information

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IPC IPC(8): C07D307/48
CPCY02P20/584
Inventor 吴廷华高尤剑肖文军吴瑛
Owner 海宁市袁花镇工业投资有限公司
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