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A kind of method for efficient extraction and separation of active lignin

A kind of activity and lignin technology, applied in the direction of lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems such as difficult to achieve effective separation of lignin, and achieve the effect of easy implementation, good fiber quality and reduced conversion loss

Active Publication Date: 2022-04-05
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention addresses the traditional p- The problem that TsOH technology is difficult to achieve effective separation of lignin proposes a new method for efficient extraction and separation of active lignin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add poplar 40-60 mesh wood flour to p -TsOH aqueous solution and H 2 o 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 80 wt%, H 2 o 2 The dosage is 1.0 wt% (relative to the hardwood raw material), the solid-to-liquid ratio is 1:9, the temperature is 75°C, the time is 80 min, the stirring speed is 500 rpm, and after the reaction, add 5 times the volume of the reaction liquid to wash and filter the product. The pore size of the filter paper used is 30-50 μm, so that the extracted lignin is coagulated and precipitated, the filtrate is centrifuged at 1000 g for 20 min, the supernatant is removed, the precipitate is washed and freeze-dried at a temperature of -20°C and a vacuum of 10 Pa 28 h to obtain high-efficiency active lignin.

[0027] The extraction rate of high-efficiency active lignin is 61.3%, the alcoholic hydroxyl content is 9.2 mmol / g, the phenolic hydroxyl content is 6.7 mmol / g, the carb...

Embodiment 2

[0032] Add eucalyptus 40-60 mesh wood powder to p -TsOH aqueous solution and H 2 o 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 70 wt%, H 2 o 2 The dosage is 1.5 wt% (relative to the hardwood raw material), the solid-to-liquid ratio is 1:7, the temperature is 70°C, the time is 60 min, the stirring speed is 550 rpm, and after the reaction, add 8 times the volume of the reaction liquid to wash and filter the product. The pore size of the filter paper used is 30-50 μm, so that the extracted lignin is coagulated and precipitated. The filtrate is centrifuged at 600 g for 25 min, the supernatant is removed, the precipitate is washed and freeze-dried at a temperature of -18 °C and a vacuum of 9 Pa for 26 h Get high-efficiency active lignin.

[0033] The extraction rate of the high-efficiency active lignin produced is 62.4%, the alcoholic hydroxyl content is 9.5 mmol / g, the phenolic hydroxyl content is 6.5 m...

Embodiment 3

[0037] Add Acacia 40-60 mesh wood flour to p -TsOH aqueous solution and H 2 o 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 75 wt%, H 2 o 2 The dosage is 2.5 wt% (relative to the hardwood raw material), the solid-to-liquid ratio is 1:5, the temperature is 74°C, the time is 40 min, the stirring speed is 600 rpm, and the reaction is completed by adding 6 times the volume of the reaction liquid to wash and filter the product. The pore size of the filter paper used is 30-50 μm, so that the extracted lignin is coagulated and precipitated. The filtrate is centrifuged at 500 g for 15 min, and the precipitate is washed and freeze-dried at a temperature of -15 °C and a vacuum of 7 Pa for 20 h to obtain high-efficiency activity. Lignin.

[0038] The extraction rate of the high-efficiency active lignin produced was 61.1%, the alcoholic hydroxyl content was 8.9 mmol / g, the phenolic hydroxyl content was 6.5 mmol / g...

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Abstract

The invention belongs to the technical field of biomass refining and resource utilization, and relates to a method for efficiently extracting and separating active lignin. Using p-toluenesulfonic acid / H 2 o 2 The system handles raw materials. p-TsOH and H 2 o 2 The synergistic effect can effectively extract high-activity lignin from hardwood, inhibit the repolymerization of lignin monomers and the formation of low-activity C-C linkages. The lignin separation product is easy to process and transform; the treatment conditions are mild, only a small amount of cellulose and hemicellulose components with a low degree of polymerization undergo hydrolysis reaction, and the delignification selectivity is high. The invention is easy to implement, has the advantages of simple process and high efficiency, the solvent and chemicals used are green reagents, the solvent can be reused through evaporation and recrystallization, and the generation of toxic pollutants can be avoided. The fiber quality after lignin extraction is good, the yield of synthetic cellulose is high, the conversion loss of polysaccharides is reduced, and it can be used as an excellent biomass energy material.

Description

technical field [0001] The invention belongs to the technical field of biomass refining and resource utilization, and relates to a method for efficiently extracting and separating active lignin. Background technique [0002] Broad-leaved wood generally refers to dicotyledonous trees, including poplar, eucalyptus, locust tree, etc., and its main components include cellulose (40-55%), hemicellulose (24-40%) and lignin (18- 25%) of these three components. From a structural point of view, cellulose is a chain-like polysaccharide obtained by connecting glucose units through β-1-4-glycosidic bonds. Due to the existence of cellulose crystallization region, high degree of polymerization and chain structure, the cellulose structure in plant fiber raw materials is more stable. The cellulose structure of plant fiber raw materials has higher thermal stability than the hemicellulose structure. A large number of acetyl groups connected to hemicellulose, better removal efficiency and re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08H8/00C08H7/00C07G1/00
CPCC08H8/00C07G1/00
Inventor 庞志强黎鹏飞刘玉龙
Owner QILU UNIV OF TECH
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