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Method for preparing levoglucosenone through biomass catalytic pyrolysis

A technology of L-glucosone and catalytic pyrolysis, which is applied in the field of biomass energy utilization, can solve the problems of poor thermal stability, environmental pollution, high ionic liquid price and the like, and achieves the effect of low cost

Active Publication Date: 2017-07-07
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, among the above-mentioned catalysts, catalysts such as liquid acids need to be loaded onto cellulose or biomass raw materials through cumbersome pretreatment processes; and ionic liquids are not only expensive but also have poor thermal stability.
More importantly, the above-mentioned acid catalysts all have very strong acidity. During the pyrolysis process, due to the existence of water vapor, the acid sites are prone to be lost and enter into the pyrolysis liquid product to promote the formation of levoglucosone in the form of catalyst. Secondary reactions in the pyrolysis liquid, making it difficult for levoglucosone to exist stably
In addition, after the catalytic pyrolysis reaction, the catalyst and coke are mixed together, the catalyst is difficult to recycle, and it also affects the use of coke
And the massive use of these strongly acidic catalysts also easily causes problems such as environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 100g of dry poplar wood (0.1-0.3mm in particle size) as raw material, immerse in 70% concentration of phosphoric acid solution for 1h, and dry at 110°C for 18h to remove free water. The loading of phosphoric acid is 45.8%, and then Under an inert atmosphere, the temperature was raised from room temperature to 500°C at a rate of 10°C / min and activated at a constant temperature for 2 hours. After cooling, it was washed with deionized water at 60°C until neutral, and after drying, 27 g of activated carbon activated by biomass-based phosphoric acid was obtained.

[0022] Get 10g of the above-mentioned biomass-based phosphoric acid-activated activated carbon and grind it to an average particle size of about 0.2mm, use poplar as a raw material (particle size is 0.1-0.3mm), the two are mechanically mixed, and the mass ratio of poplar to catalyst is 5 : 1, then the mixed material is pyrolyzed for 15s at 330°C, the heating rate is greater than 500°C / s, and nitrogen atmospher...

Embodiment 2

[0024] Adopt biomass-based phosphoric acid activated carbon catalyst 5g prepared in Example 1, grind to about 0.2mm in average particle diameter, take pine as raw material (particle diameter is 0.1-0.3mm), the two are mechanically mixed, pine and catalyst The mass ratio is 4:1, then the mixed material is pyrolyzed at 300°C, the heating rate is greater than 500°C / s, and nitrogen atmosphere for 20s, and the yield of the liquid product is 41.6%, and the levoglucosone is analyzed by gas chromatography. Content, calculated that the productive rate of L-glucosone is 9.9%.

Embodiment 3

[0026] Adopt 7 g of biomass-based phosphoric acid activated carbon catalysts prepared in Example 1, grind to an average particle diameter of about 0.2 mm, use corn stalks as raw material (particle diameter is 0.1-0.3 mm), the two are mechanically mixed, corn stalks The mass ratio to the catalyst is 3:1, and then the mixed material is pyrolyzed at 310°C, the heating rate is greater than 500°C / s, and an argon atmosphere for 20s, and the yield of the liquid product is 41.9%, which is analyzed by gas chromatography. According to the content of glucosone, it is calculated that the yield of glucosone is 8.2%.

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Abstract

The invention belongs to the field of utilization of biomass energy, and in particular relates to a method for preparing levoglucosenone through biomass catalytic pyrolysis. The method comprises the following steps: by taking biomass base phosphoric acid activated carbon as a catalyst, performing mechanical mixing on the catalyst with biomasses, performing flash pyrolysis at 250-470 DEG C under an inert anaerobic condition, and condensing a pyrolysis gas, thereby obtaining a liquid product rich in levoglucosenone. In pyrolysis products of the biomasses subjected to catalytic pyrolysis of the biomass base phosphoric acid activated carbon, the yield and the purity of levoglucosenone are both relatively high; in addition, a mixture of solid coke generated through pyrolysis and the catalyst can be used as a carbon source which is continuously adopted to prepare activated carbon; due to adoption of the biomass base phosphoric acid activated carbon which is low in price and can be recycled, the production cost and the pollution can be effectively reduced, and the method is an economic and effective method for preparing the levoglucosenone.

Description

technical field [0001] The invention belongs to the field of utilization of biomass energy, and in particular relates to a method for preparing L-glucosone by catalytic pyrolysis of biomass. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-D-pyranosen-2-one) is produced by dehydration of cellulose and part of hemicellulose during biomass pyrolysis. An important anhydrosugar derivative formed; it has high reactivity, is an important raw material for organic synthesis, and has high application value. [0003] It has been more than 40 years since L-glucosone was first discovered in 1973. However, due to its low yield and difficult purification in the conventional pyrolysis process of biomass, the market price is high, which limits its application in organic synthesis. Previous studies have proved that in the pyrolysis process of cellulose or biomass, the introduction of a suitable acid catalyst can significantly promote the formation of glucosone. Th...

Claims

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Application Information

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IPC IPC(8): C07H3/10C07H1/00
CPCC07H1/00C07H3/10C07D493/08
Inventor 陆强叶小宁王昕郭浩强彭立董长青杨勇平
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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