A method for separating and extracting highly active lignin from coniferous wood

A coniferous, high-activity technology, applied in lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve problems such as effective separation of refractory lignin, and achieve the effects of easy implementation, promotion of extraction, and mild treatment conditions

Active Publication Date: 2022-02-01
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 22h 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 powder 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 hydroxy...

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Abstract

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. Using (p-TsOH) / ClO 2 The system handles raw materials. The present invention passes p -TsOH / ClO 2 System separation and extraction of coniferous lignin with high yield and high activity, p ‑TsOH and ClO 2 The synergistic effect can effectively promote the extraction of high-activity lignin from coniferous wood, and inhibit the repolymerization of lignin monomers and the formation of low-activity C‑C linkages. The lignin product obtained by the invention is easy to process and transform; the treatment condition is mild, the selectivity of chlorine dioxide to lignin reaction is high, the degradation loss of polysaccharide is small, the method is easy to implement, and the process is simple and efficient. The fiber quality after lignin extraction is good, and the yield of synthetic cellulose is high, which 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 Patents(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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