Method for preparing 5-hydroxymethylfurfural by degrading cellulose in formic acid/acetic acid system

A technology for hydroxymethylfurfural and cellulose degradation, applied in the field of chemical engineering, can solve the problems of high cost, inconvenient industrialization, and high cost, and achieve the effect of improving selectivity

Active Publication Date: 2021-11-19
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the research on the preparation of 5-HMF mostly uses glucose or fructose as raw materials through dehydration reaction. Due to the high cost of glucose and fructose, this method is not convenient for industrialization
In addition, most studies use ionic liquids as cellulose solvents, which are expensive, and the yield of 5-HMF prepared from cellulose is generally 40%-70%, and the yield is not high.

Method used

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  • Method for preparing 5-hydroxymethylfurfural by degrading cellulose in formic acid/acetic acid system
  • Method for preparing 5-hydroxymethylfurfural by degrading cellulose in formic acid/acetic acid system
  • Method for preparing 5-hydroxymethylfurfural by degrading cellulose in formic acid/acetic acid system

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Embodiment 1

[0038] A method for preparing 5-hydroxymethylfurfural by degrading cellulose in a formic acid / acetic acid system, comprising the steps:

[0039] Step 1, pretreatment of cellulose

[0040] Weigh 1g of cellulose and put it into a 100ml beaker, then add 30ml of distilled water to the beaker and mix evenly, then use an ultrasonic cell pulverizer to sonicate at a power of 600W, set the ultrasonic working mode to 12s (ultrasonic 8s, intermittent 4s), ultrasonic Stop after 8 minutes to obtain ultrasonically pretreated cellulose, and freeze-dry the ultrasonically pretreated cellulose at -40°C for 24 hours before use;

[0041] Step 2, SO 42- / TiO 2 Preparation of solid acid catalyst

[0042] Step 2.1, weigh 1g of nano-titanium dioxide powder and pour it into a beaker, then add 30ml of sulfuric acid with a concentration of 3mol / L to the beaker, stir for 5min and let it stand for 20h, after standing, use a sand filter to filter out the sulfuric acid solution to obtain sulfuric acid tr...

Embodiment 2

[0047] A method for preparing 5-hydroxymethylfurfural by degrading cellulose in a formic acid / acetic acid system, comprising the steps:

[0048] Step 1, pretreatment of cellulose

[0049] Weigh 2g of cellulose and put it into a 100ml beaker, then add 50ml of distilled water to the beaker and mix evenly, then use an ultrasonic cell pulverizer to sonicate at a power of 800W, set the ultrasonic working mode to 12s (ultrasonic 8s, intermittent 4s), ultrasonic Stop after 10 minutes to obtain ultrasonically pretreated cellulose, freeze-dry the ultrasonically pretreated cellulose at -45°C for 24 hours before use;

[0050] Step 2, SO 4 2- / TiO 2 Preparation of solid acid catalyst

[0051] Step 2.1, weigh 2g of nano-titanium dioxide powder and pour it into a beaker, then add 50ml of sulfuric acid with a concentration of 3mol / L to the beaker, stir for 8min and then let it stand for 20h. Nano-titanium dioxide; dry the sulfuric acid-treated nano-titanium dioxide in a vacuum oven at 1...

Embodiment 3

[0056] A method for preparing 5-hydroxymethylfurfural by degrading cellulose in a formic acid / acetic acid system, comprising the steps:

[0057] Step 1, pretreatment of cellulose

[0058] Weigh 3g of cellulose and put it into a 100ml beaker, then add 60ml of distilled water to the beaker and mix evenly, then use an ultrasonic cell pulverizer to sonicate at a power of 900W, set the ultrasonic working mode to 12s (ultrasonic 8s, intermittent 4s), ultrasonic Stop after 12 minutes to obtain ultrasonically pretreated cellulose, freeze-dry the ultrasonically pretreated cellulose at -50°C for 36 hours before use;

[0059] Step 2, SO 4 2- / TiO 2 Preparation of solid acid catalyst

[0060] Step 2.1, weigh 3g of nano-titanium dioxide powder and pour it into a beaker, then add 60ml of sulfuric acid with a concentration of 3mol / L to the beaker, stir for 8min and then let it stand for 24h. After standing, use a sand filter to remove the sulfuric acid solution to obtain sulfuric acid tr...

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural by degrading cellulose in a formic acid / acetic acid system, comprising the following steps: ultrasonic pretreatment of cellulose; preparation of a solid acid catalyst; preparation of 5-hydroxymethylfurfural in a formic acid / acetic acid system Methylfurfural. The present invention first uses ultrasonic pretreatment to destroy the structure of cellulose, effectively improving the selectivity of cellulose acid hydrolysis, and then in formic acid / acetic acid mixed solvent, using SO 4 2‑ / TiO 2 The solid acid is used as a catalyst to catalyze the degradation of cellulose to prepare 5-hydroxymethylfurfural. The mixed solution of formic acid / acetic acid can swell the cellulose and destroy the hydrogen bonds between the cellulose molecules. The yield of the prepared 5-hydroxymethylfurfural reaches 80%. above. The invention uses cheap cellulose as a raw material to prepare 5-hydroxymethylfurfural with high added value, has simple process, easy control of conditions, low cost, high yield and good economic and environmental benefits.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and in particular relates to a method for preparing 5-hydroxymethylfurfural by degrading cellulose in a formic acid / acetic acid system. Background technique [0002] Cellulose is rich in resources and comes from a wide range of sources. It is a macromolecular compound with a crystalline structure linked by D-glucose through β-1,4 glycosidic bonds, and is insoluble in water, dilute acid and dilute alkali at room temperature. The long chains of cellulose macromolecules can combine to form cellulose bundles through van der Waals forces or hydrogen bonds. The dense fiber bundle crystal structure of cellulose and the numerous hydrogen bonds within and between molecular chains make the chemical properties of cellulose The property is very stable, it is not easily soluble in general organic solvents, water, dilute acid, dilute alkali, etc., and it will not be hydrolyzed at room temperature...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46B01J27/053
CPCB01J27/053C07D307/46
Inventor 孙晓锋何妍
Owner NORTHWESTERN POLYTECHNICAL UNIV
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