Method for separating and extracting high-activity lignin by taking coniferous wood as raw material

A coniferous, highly active technology, applied in lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve problems such as the effective separation of difficult lignin, avoid the production of toxic pollutants, good fiber quality, easy to use effect of implementation

Active Publication Date: 2020-06-16
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention addresses the traditional p- The problem that TsOH technology is difficult to achieve effective separation of lignin proposes a new method of separating and extracting highly active lignin from coniferous wood

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add coniferous spruce 40-60 mesh wood flour to p - TsOH aqueous solution and ClO 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 70 wt%, ClO 2 The dosage is 0.7 wt% (relative to the softwood raw material), the solid-liquid ratio is 1:9, the temperature is 90°C, the time is 40 min, the stirring speed is 500 rpm, and the reaction is completed by adding water twice the volume of the reaction solution 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 18 min, the supernatant is removed, the precipitate is washed and freeze-dried at a temperature of -20 °C and a vacuum of 8 Pa 22 h to get high-efficiency active lignin.

[0028] The extraction rate of the high-efficiency active lignin produced was 45.2%, the alcoholic hydroxyl content was 7.6 mmol / g, the phenolic hydroxyl...

Embodiment 2

[0032] Add 40-60 mesh wood flour of coniferous wood masson pine to p - TsOH aqueous solution and ClO 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 75 wt%, ClO 2 The dosage is 0.8 wt% (relative to the coniferous wood raw material), the solid-liquid ratio is 1:6, the temperature is 85°C, the time is 30 min, the stirring speed is 400 rpm, and the reaction is completed by adding 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 400 g for 20 min, the supernatant is removed, the precipitate is washed and freeze-dried at a temperature of -25°C and a vacuum of 10 Pa 18 h to obtain high-efficiency active lignin.

[0033] The extraction rate of the high-efficiency active lignin produced was 46.3%, the alcoholic hydroxyl content was 7.9 mmol / g, the ...

Embodiment 3

[0037] Add coniferous wood balsam fir 40-60 mesh wood flour to p - TsOH aqueous solution and ClO 2 Treated in the composed treatment system. The processing conditions are: p -TsOH aqueous solution concentration is 80 wt%, ClO 2 The dosage is 0.6 wt% (relative to the coniferous wood raw material), the solid-to-liquid ratio is 1:10, the temperature is 70°C, the time is 60 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 5 Pa for 20 h to obtain high-efficiency activity. Lignin.

[0038] The extraction rate of the high-efficiency active lignin produced was 47.5%, the alcoholic hydroxyl content was 8.1 mmol / g, the phenolic hydroxyl...

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Abstract

The invention belongs to the technical field of biomass refining and recycling, and relates to a method for separating and extracting high-activity lignin by taking coniferous wood as a raw material.A (p-TsOH)/ClO2 system is adopted to treat the raw material. According to the method, high-yield and high-activity coniferous lignin is separated and extracted through the p-TsOH/ClO2 system, extraction of the coniferous high-activity lignin can be effectively promoted through the synergistic effect of p-TsOH and ClO2, and repolymerization of lignin monomers and generation of low-activity C-C connecting bonds are inhibited. The obtained lignin product is easy to process and convert; the method has the advantages of mild treatment conditions, high selectivity of chlorine dioxide to lignin reaction, small degradation loss of glycan, simple process and high efficiency, and is easy to implement. After lignin is extracted, the fiber quality is good, the yield of holocellulose is high, and the lignin 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 separating and extracting highly active lignin from coniferous wood. Background technique [0002] Coniferous wood fibers are longer, generally between 2.56-4.08 mm in length and 40.9-54.9 μm in width, and their aspect ratio is mostly below 70; while hardwood fibers are short, generally about 1 mm in length, and their length-width The ratio is below 60; coniferous wood has a tight structure and less miscellaneous cells, and most of the miscellaneous cells in the chemical pulp are lost during washing, so the quality of the pulp is good. The lignin content of coniferous wood is high, between 25-35%, and the content of polypentose is low, mostly between 9-12%. [0003] The components of plant fiber raw materials mainly include cellulose, hemicellulose and lignin. Lignin is a three-dimensional polymer compound composed of phenylpropane s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00C07G1/00
CPCC08H6/00C07G1/00
Inventor 庞志强黎鹏飞吴丽冉刘玉龙
Owner QILU UNIV OF TECH
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