Levoglucosenone preparation method

A technology of L-glucosone and charcoal sulfonic acid, which is applied in the preparation of sugar derivatives, chemical instruments and methods, dehydrated sugar, etc., to achieve the effects of convenient recovery, avoiding impregnation and drying of raw materials, and avoiding environmental pollution

Active Publication Date: 2015-04-15
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, different catalysts have different problems in the process of use, so the development of new and efficient catalysts is still an important problem to be solved in the process of preparing LGO by selective pyrolysis of biomass.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Using 200 g of dry poplar wood (average particle size 0.1 mm) as raw material, the temperature was raised from room temperature to 350 ℃ at a rate of 20 ℃ / min under a vacuum of 50 Pa and kept for 1 h for pyrolysis to obtain Poplar charcoal: Mix the above poplar charcoal and concentrated sulfuric acid (98%) at a mass ratio of 1:10, then sulfonate at a constant temperature of 150 °C for 12 h under a nitrogen atmosphere, and wash with deionized water until no sulfuric acid is removed after cooling Root ions were obtained after drying to obtain 40 g of charcoal sulfonic acid.

[0023] Take 10 g of the above charcoal sulfonic acid and grind it to an average particle size of 0.2 mm. Poplar wood is used as a raw material (average particle size is 0.1 mm), and the two are mechanically mixed. The mass ratio of poplar wood and charcoal sulfonic acid is 1:2 , and then the mixture was pyrolyzed at 330 °C for 25 s under a nitrogen atmosphere, and the yield of liquid product was 47%....

Embodiment 2

[0025] Measure 30 g of FeCl respectively 2 4H 2 O and 6 g FeCl 3 ·6H 2 O, add water to prepare a 200 mL mixed solution and add it to a three-necked flask, place it in a constant temperature water bath at 65 °C, and slowly add NaOH solution with a concentration of 0.1 mol / L dropwise while stirring until the pH value of the solution reaches 12, continue Stir and age at constant temperature for 30 min; then remove the three-neck flask from the constant temperature water bath and cool to room temperature, use a magnetic field to separate the magnetic matrix and the supernatant, then wash the magnetic matrix repeatedly with water until it is neutral, and dry it at 110 °C for 12 h. The black solid magnetic matrix Fe can be obtained 3 o 4 .

[0026] Take 2 g of magnetic matrix Fe 3 o 4 Carry out mechanical mixing with 10 g charcoal sulfonic acid (prepared according to embodiment 1), add the water of 2.5 g again and stir, obtain the cylindrical magnetic charcoal sulfonic acid c...

Embodiment 3

[0029] Get 10 g of charcoal sulfonic acid prepared in Example 1, grind to an average particle size of 0.2 mm, use commercial microcrystalline cellulose as raw material (average particle size is 0.05 mm), the two are mechanically mixed, cellulose and carbon The mass ratio of sulfonic acid is 1:1, and then the mixed material is pyrolyzed at 340 °C under nitrogen atmosphere for 20 s, and the yield of liquid product is 52%. The yield of L-glucosone was 21.9%.

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Abstract

The invention belongs to the field of biomass energy use and particularly relates to a levoglucosenone preparation method. The levoglucosenone preparation method includes: mechanically mixing char sulfonic acid or magnetic char sulfonic acid serving as a catalyst with biomass raw materials, performing fast pyrolysis at the temperature of 280-450 DEG C under the anaerobic condition, and condensing pyrolysis gas so that a liquid product rich in levoglucosenone can be obtained. In the liquid product prepared by the method, both yield and purity of the levoglucosenone are high; and the catalyst is stable in performance, can be directly separated and recovered from solid residues mechanically or by the aid of a magnetic field and is reusable.

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. Background technique [0002] Levoglucosone (LGO, 1,6-anhydro-3,4-dideoxy-β-d-pyranosen-2-one) is a biomass pyrolysis process in which cellulose is depolymerized and dehydrated An anhydrosugar derivative is formed, which has high reactivity and can be widely used in various synthetic reactions, so it has extremely high added value in chemical industry or medicine. However, the yield of LGO produced by conventional pyrolysis of biomass is very low, and its content in the pyrolysis liquid product is also extremely low, making it economically and technically impossible to separate LGO from conventional pyrolysis liquid products. Row. [0003] In order to improve the selectivity of biomass pyrolysis to LGO, a suitable catalyst can be introduced in the pyrolysis process, so as to control the pyrolysis reaction pathway direc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H3/10C07H1/00B01J31/02B01J31/28
CPCY02P20/584
Inventor 陆强张智博董长青杨勇平
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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