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Method for preparing 5-hydroxymethylfurfural by hydrothermally decomposing wood fibers

A technology for hydroxymethyl furfural and lignocellulose, applied in the field of preparing 5-hydroxymethyl furfural, can solve the problems of low reactivity of cellulose, difficult recovery of acid-containing wastewater, etc., achieves inhibition of hydration reaction, important application value, and solution Effects of environmental problems

Active Publication Date: 2014-08-27
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of these methods is that the inorganic acid used has a certain corrosiveness to the equipment, and the acid-containing wastewater is not easy to recycle, and the temperature range of the catalytic hydrolysis of solid acids such as ion exchange resins can only achieve a good catalytic effect at about 130 ° C, and because Cellulose has a high degree of crystallinity, and the reactivity of cellulose in common solvents is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Grind the dried cotton stalks to 40-120 mesh (40.8% cellulose, 15.7% hemicellulose, 10.23% lignin, 0.17% ash content in the dry basis), soak with an appropriate amount of water, and put it into an ultrasonic instrument for ultrasonic treatment 40kHz, 10 minutes, add the water of 1: 1:MIBK mixed solvent, the weight of solvent addition is 50 times of cotton stalk powder (comprising the amount of water added by ultrasonic treatment), with 5% (by weight of cotton stalk powder) HZSM molecular sieve catalyst Put them together in an autoclave, set the reaction temperature to 210°C, and adopt a heating rate of 10K / min. When the temperature rises to the preset temperature, heat-preserve and hydrolyze for 90 minutes. After the reaction, take out the autoclave for cooling, and then filter the residue to obtain Cotton stalk hydrolyzate. The aqueous phase of the hydrolyzed solution was extracted with MIBK, then combined with the organic phase of the hydrolyzed solution, and the crud...

Embodiment 2

[0030] Add 5% (W%) (by weight of cotton stalk powder) MCM-41 catalyst to the material of Example 1 that adds 4: 1 MIBK and water mixed solvent, put it in the autoclave, and the temperature rises to 210 ° C, and the temperature is kept The hydrolysis reaction was carried out for 90 minutes. After the reaction, the kettle body was taken out for cooling, and then the residue was filtered to obtain the cotton stalk hydrolyzate. After the aqueous phase of the hydrolyzate was extracted with MIBK, it was combined with the organic phase of the hydrolyzate, and the solvent was evaporated to obtain 5- Crude HMF. The yield of cellulose converted to 5-HMF in cotton stalk was determined by HPLC to be 43.7%.

Embodiment 3

[0032] Replace the cotton stalk in Example 1 with rice straw (containing 42.3% cellulose, 25.1% hemicellulose, and 4.87% lignin in the dry basis), and then add 4:1 DMSO: water mixture after ultrasonic treatment for 5 minutes Solvent, add 5% MCM-41 catalyst (W%) (by weight of cotton stalk powder), put it into an autoclave and heat up to a set reaction temperature of 210°C, heat preservation and hydrolysis reaction for 90min, take out the kettle body after the reaction is over, and cool it down. Then filter the residue to obtain the straw hydrolyzate. The aqueous phase of the hydrolyzate was extracted with MIBK, then combined with the organic phase of the hydrolyzate, and the solvent was evaporated to obtain crude 5-HMF. The yield of cellulose in rice straw converted to 5-HMF was determined by HPLC to be 53.9%.

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural by hydrothermally decomposing wood fibers, which comprises the following steps: drying and pulverizing wood fibers to 40-120 meshes, soaking with water, treating with an ultrasonic apparatus for 5-20 minutes, mixing with a catalyst and a solvent, and stirring to carry out hydrolysis reaction at 170-250 DEG C for 30-150 minutes; after the reaction finishes, cooling and filtering; extracting the water phase with an organic solvent, merging the extraction liquid and the organic phase, and removing the solvent to obtain the 5-hydroxymethylfurfural. The invention has the advantages of cheap and accessible raw material and abundant sources, can solve the problem of raw material sources of 5-hydroxymethylfurfural, relieves the environmental pollution from stacked waste wood fibers, and enhances the wood fiber hydrolysis efficiency by using ultrasonic processing.

Description

Technical field: [0001] The invention relates to a method for preparing 5-hydroxymethylfurfural from wood fibers, in particular to a method for preparing 5-hydroxymethylfurfural through hydrothermal decomposition of wood fibers after ultrasonic treatment. Background technique: [0002] 5-Hydroxymethylfurfural (5-HMF) molecule contains an aldehyde group and a hydroxymethyl group, which can be used to synthesize many useful compounds through hydrogenation, oxidative dehydrogenation, esterification, halogenation, polymerization, hydrolysis and other chemical reactions. Compounds and new polymer materials are an important platform compound. 2,5-dimethylfuran, a biomass liquid fuel similar to ethanol synthesized from 5-HMF, has an energy density 40% higher than ethanol and a boiling point 20°C higher. It is a more ideal substitute than ethanol New energy substances from fossil fuels. [0003] The raw material that the traditional method for preparing 5-HMF adopts is fructose, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
Inventor 周涛桂颖蒋崇文苏爱鲜廖孝艳
Owner CENT SOUTH UNIV
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