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Method for preparing 5-hydroxymethylfurfural by taking galactose as base material

A hydroxymethylfurfural and galactosyl technology, which is applied in the field of preparing the platform compound 5-hydroxymethylfurfural (5-HMF), can solve the problems of harsh operating conditions, difficulty in actual production, and high cost, and achieves equipment and The effect of low environmental requirements and simple and easy preparation methods

Inactive Publication Date: 2015-11-25
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, how to efficiently produce 5-HMF is one of the research hotspots. At present, most studies use fructose and glucose as substrates, and maximize the yield of 5-HMF by selecting appropriate catalysts or solvents, but it is only suitable for Sugars with fructose and glucose as the basic structural units often have high costs, high energy consumption, and harsh operating conditions, so it is difficult to apply them in actual production

Method used

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  • Method for preparing 5-hydroxymethylfurfural by taking galactose as base material
  • Method for preparing 5-hydroxymethylfurfural by taking galactose as base material
  • Method for preparing 5-hydroxymethylfurfural by taking galactose as base material

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Experimental program
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Effect test

Embodiment 1

[0037] Weigh 100, 200, 300, 400, 500, 600, 800 grams of galactose respectively, add water to 1 liter to obtain galactose solutions of different concentrations; weigh 120 grams of calcium hydroxide solids, slowly stir and add half In the lactose solution, the isomerization reaction was carried out at 20°C for 20 hours, and yellow gelatinous products were obtained after the reaction. Put each yellow colloidal product in a water bath at 20°C, slowly stir and add phosphoric acid to adjust the pH to 1.5, centrifuge to remove the precipitate, and obtain a supernatant.

[0038] The contents of galactose and tagatose in each supernatant were determined by HPLC, and the results showed that galactose in each supernatant was completely consumed, and the concentrations of tagatose were 40 g / L, 86 g / L, and 140 g / L, respectively. liter, 250 g / l, 380 g / l, 460 g / l, 520 g / l. That is, the yield of tagatose obtained by isomerization of galactose at various concentrations is as follows figure 1...

Embodiment 2

[0042]Weigh 500 grams of galactose and add water to 1 liter. Weigh 222 grams of calcium hydroxide solids and 111 grams of calcium chloride solids, add them to the galactose solution, and stir fully while adding, so that calcium hydroxide and calcium chloride solids are fully dispersed in the solution. Then, the isomerization reaction was allowed to stand in a water bath at 30° C. for 8 hours, and a yellow colloidal substance was obtained after the reaction. Place the yellow gelatinous substance in an ice-water bath at 0°C, slowly add 50% sulfuric acid aqueous solution, stir and dissipate heat while adding, adjust the pH to 1.0, and centrifuge to remove the precipitate to obtain a supernatant.

[0043] Divide the supernatant into 5 parts, each 200 ml, add ferric chloride, zinc chloride, SO 4 - / Fe 3 o 4 -Al 2 0 4 , 2 grams of phosphoric acid, —— (the “——” means no catalytic acid was added, for comparison with the aforementioned situation of adding catalytic acid), and the...

Embodiment 3

[0046] Add 60 kg of galactose to a 250L temperature-controlled reaction tank, add 100 liters of water to dissolve, slowly add 3.7 kg of calcium hydroxide solids, 0.2 kg of sodium sulfate, stir and disperse evenly with a stirrer, control the temperature at 20°C, and continuously stir for isomerization reaction for 10 hours, isomeric products were obtained. Control the temperature at 20°C, slowly pump 50% phosphoric acid aqueous solution into the isomer product at a rate of 1 liter / hour with a feed pump until the pH value is 2.0, stop adding acid, and continue stirring to dissipate heat during feeding. Then let it stand for 12 hours to fully precipitate, remove the precipitate and add 1.0 kg of SO to the supernatant 4 - / Fe 3 o 4 -Al 2 0 4 , react in a high-pressure reactor at 120° C. for 1 hour to obtain a post-reaction solution.

[0047] After HPLC detection, the galactose in the solution was exhausted after the reaction, that is, the conversion rate of galactose was 100...

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Abstract

The invention relates to a method for preparing 5-hydroxymethylfurfural with high efficiency, the method takes galactose or a galactose-based carbohydrate as base materials, according to special performance of the galactose aldose, a compound 5-HMF is produced by a two-step method, the method is characterized in that galactose is isomated to tagatose under alkaline environment; and 5-HMF can be degraded by talgatose under high temperature by employing acid catalysis. The test confirms that the conversion rate of 5-HMF in the method is high, the method is easy and simple to operate, energy consumption is little, cost is low, and the method has good application prospect.

Description

Technical field [0001] The invention belongs to the technical field of biomass energy, and specifically relates to a method for preparing the platform compound 5-hydroxymethylfurfural (5-HMF) using galactose as a base material. Background technique [0002] With the increasingly serious problems of global warming and environmental pollution caused by the extensive use of fossil energy, the development and utilization of sustainable biomass resources has attracted more and more attention. Biomass resources are organic carbon resources that exist in large quantities in nature. Through appropriate conversion methods, biomass resources can provide fuels, high-quality chemicals, new materials, etc. [0003] Biomass is mainly composed of sugars, lignin, fatty acids, lipids and proteins, with sugars accounting for the largest proportion. Sugars use hexose and pentose as basic units, including cellulose, hemicellulose, starch, etc. Among them, the compound 5-hydroxymethylfurfural (...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 吕学兰杨池张亚杰李丽丽马中森
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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