Preparation method of catalyst for preparing 5-hydroxymethylfurfural from cellulose

A technology of hydroxymethyl furfural and catalyst, applied in the field of nano catalyst preparation, can solve the problems of cumbersome reaction steps, complex species selection, environmental burden and the like, and achieves the effect of high yield

Active Publication Date: 2018-12-28
QINGDAO UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the reaction steps are cumbersome, distillation and other processes are required, the selection of anions and cations for ionic liquid catalysts is more complicated, and organic reagents also bring a certain burden to the environment.
[0008] In summary, the traditional system for preparing 5-hydroxymethylfurfural mainly requires organic reagents to dissolve the raw materials, and the catalysts mostly use ionic liquid systems, containing various metal solid acid catalysts, etc., and strong acids and compounds are required in the preparation process. and other organic reagents, which are a burden on the environment. Although the conversion rate of raw materials is high, the selectivity of 5-hydroxymethylfurfural has certain limitations, and the product needs additional treatment for separation and purification.

Method used

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  • Preparation method of catalyst for preparing 5-hydroxymethylfurfural from cellulose

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Experimental program
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Effect test

Embodiment 1

[0020] Choose glucose as the raw material, water as the solvent, and nickel acetate tetrahydrate as the nickel source, and control the ratio of the two to 5:1. After mixing evenly, pour it into a polytetrafluoroethylene-lined reaction kettle, put it into a muffle furnace, and heat it to 190°C, constant temperature reaction for 6 hours, after the reaction kettle was cooled to room temperature, it was filtered and washed to obtain a dark brown nickel-doped carbon composite. The obtained dried product was put into a tubular calciner, and the temperature was raised to 900° C. under a nitrogen atmosphere, and the temperature was kept constant for 3 hours to obtain a nickel-doped carbon catalyst.

[0021] 200mg of the obtained catalyst, 1g of cellulose, and 100ml of water are used as the reaction solvent. After mixing evenly, put it into a high-temperature and high-pressure reactor, and feed hydrogen gas to ensure that the hydrogen pressure is maintained at 4MPa during the reaction. ...

Embodiment 2

[0023] Select larch powder as raw material, water as solvent, nickel hydroxide as nickel source, control the ratio of raw material and nickel source to 2:1, mix well and pour it into a polytetrafluoroethylene-lined reaction kettle, and put it into a muffle furnace , heated to 230°C, and reacted at a constant temperature for 5 hours. After the reactor was cooled to room temperature, it was filtered and washed to obtain a dark brown nickel-doped carbon composite. Put the obtained dry product into a tubular calciner, raise the temperature to 800° C. under a nitrogen atmosphere, and keep the temperature constant for 2 hours to obtain a nickel-doped carbon catalyst.

[0024] 500mg of the obtained catalyst, 1g of cellulose, and 100ml of water are used as the reaction solvent. After mixing evenly, put it into a high-temperature and high-pressure reactor, and feed hydrogen to ensure that the hydrogen pressure is maintained at 6MPa during the reaction. Heat up to 200°C and react for 15 ...

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Abstract

A preparation method of a catalyst for preparing 5-hydroxymethylfurfural from cellulose is characterized in that a nickel doped biomass-based carbon compound is prepared from biomass sources such as glucose, the cellulose and bark as well as a nickel-containing compound as raw materials under hydrothermal conditions and is then carbonized at high temperature in an inert gas atmosphere, and a nickel doped carbon-based catalyst is obtained and has L-type and B-type double-acid active sites and developed pore structure. When the catalyst is applied to a catalytic degradation reaction of the cellulose in a hydrothermal environment with the hydrogen atmosphere, the product 5-hydroxymethylfurfural has higher yield, and recyclability of the catalyst is good. The operation process is mainly characterized in that the carbon-based catalyst prepared from the biomass sources is used for catalytic degradation of biomass, a high value-added platform chemical compound is obtained, the biomass sourceswhich are environmentally friendly, cheap and easily available are fully used, the catalysis reaction process is simple to operate, and yield is high.

Description

Technical field: [0001] The invention relates to the field of nano catalyst preparation, in particular to a method for preparing a catalyst for preparing 5-hydroxymethylfurfural from cellulose Background technique: [0002] 5-Hydroxymethylfurfural is a platform compound for the preparation of levulinic acid by degrading cellulose, an important intermediate for the synthesis of fine chemicals and furan polymers, and an effective active component for pharmaceuticals. 5-Hydroxymethylfurfural is considered to be the main intermediate in the fields of biomass chemical industry, petrochemical industry and organic chemistry. Therefore, it is of practical significance and value to seek an effective green path to prepare 5-Hydroxymethylfurfural from cellulose. [0003] When the reaction temperature using water as the medium is higher than 200 °C, the reactants undergo thermal degradation and hydrolysis at the same time, which is called "hydrothermal degradation". Studies have pointe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J37/08B01J37/10C07D307/46
CPCB01J23/755B01J37/084B01J37/10C07D307/46Y02P20/584
Inventor 吴琼于世涛刘仕伟李文静张高月高明明
Owner QINGDAO UNIV OF SCI & TECH
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