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Method for extracting biomass lignin by utilizing quaternary ammonium base

A technology of quaternary ammonium base and lignin, which is applied in the direction of lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems that the extraction rate is only about 10%, the structure undergoes chemical changes, and the purity of lignin is not high. Achieve the effect of low cost, mild extraction conditions and short cycle

Inactive Publication Date: 2017-12-15
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Disadvantages: The traditional pulping method produces a large amount of wastewater during the pulping process. The wastewater contains a large amount of organic matter, especially lignin, which not only causes environmental pollution but also causes a lot of waste of resources
Disadvantage: This method also dissolves the cellulose component
Insufficient: acid lignin is affected by acid during the separation process, and its structure will undergo chemical changes
Liu Yunyan from Wuhan Institute of Technology used NaOH as lye to extract lignin from chestnut shells. The amount of lye was large, the solid-to-liquid ratio was 1:40 under optimal conditions, and the lignin extraction rate was only about 10%. The result was Crude lignin, the purity of lignin is not high

Method used

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  • Method for extracting biomass lignin by utilizing quaternary ammonium base
  • Method for extracting biomass lignin by utilizing quaternary ammonium base

Examples

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Effect test

Embodiment 1

[0035] A method utilizing tetramethylammonium hydroxide to extract wheat lignin:

[0036] The dried wheat straw was extracted in a Soxhlet extractor with a benzene:ethanol solution with a volume ratio of 2:1 for 6 hours, and the residue was dried to obtain the degreased sample used in this experiment. Take 1.000g of defatted and dewaxed straw, use the Klason method to measure the lignin content in wheat straw, measure three times in parallel, and take the average value.

[0037] Accurately weigh 10g of dried wheat straw, add 200ml of tetramethylammonium hydroxide with a mass concentration of 24%, treat it in a constant temperature water bath at a temperature of 50°C for 14h, filter it with gauze while it is hot, adjust the pH of the filtrate to 5.5 with acetic acid, and depressurize Concentrate, treat with three volumes of 95% ethanol and vacuum filter. The filtrate was distilled off under reduced pressure to remove ethanol, then the pH was adjusted to 2.0 with 6 mol / L HC...

Embodiment 2

[0040] A method utilizing tetraethylammonium hydroxide to extract corn stalk lignin:

[0041] Wash and dry the corn stalks, and pulverize them with a pulverizer for later use. Take 1.000g of defatted and dewaxed straw, and use the Klason method to determine the lignin content in wheat straw. The content of lignin in wheat straw was measured three times in parallel, and the average value was 12.78%.

[0042]Accurately weigh 10g of dried corn stalks, add 200ml of 20% tetraethylammonium hydroxide, treat in a constant temperature water bath at a temperature of 50°C for 10h, filter with gauze while it is hot, adjust the pH of the filtrate to 5.5 with acetic acid, and concentrate under reduced pressure , treated with three volumes of 95% ethanol and vacuum filtered. The filtrate was distilled under reduced pressure to remove ethanol, and then adjusted to pH 2.0 with 6 mol / L HCl solution, centrifuged, and freeze-dried. The obtained product was corn straw lignin, and the calculated l...

Embodiment 3

[0045] A method of extracting wheat lignin with tetrabutyl ammonium hydroxide:

[0046] Wash and dry the wheat stalks, and pulverize them with a pulverizer for later use. Take 1.000g of defatted and dewaxed straw, and use the Klason method to determine the lignin content in wheat straw. The content of lignin in wheat straw is measured three times in parallel, and the average value is 18.75%.

[0047] Accurately weigh 10g of dried wheat straw, add an appropriate amount of tetraethylammonium hydroxide with a concentration of 20%, treat it in a constant temperature water bath at a temperature of 50°C for 15 hours, filter it with gauze while it is hot, adjust the pH of the filtrate to 5.5 with acetic acid, and reduce pressure Concentrate, treat with three volumes of 95% ethanol and vacuum filter. The filtrate was distilled under reduced pressure to remove ethanol, then adjusted to pH 2.0 with 6 mol / L HCl solution, centrifuged, and freeze-dried. The product obtained was wheat lign...

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Abstract

The invention discloses a method for extracting biomass lignin by utilizing a quaternary ammonium base. The method comprises the following steps: adding an aqueous solution of the quaternary ammonium base into a biomass raw material, heating and extracting in a water bath, and filtering; regulating the pH value of the filtrate to be 5.0-6.0, performing reduced pressure concentration, treating with ethanol in a volume of three times that of the material, and filtering; and performing reduced pressure distillation on the filtrate to remove ethanol, regulating the pH value to be 2.0-3.0, performing centrifugal separation, performing freeze drying, thereby obtaining the product biomass lignin. The method for extracting biomass lignin by utilizing the quaternary ammonium base disclosed by the invention is low in cost in the extraction process, mild in conditions, short in period and high in lignin extraction rate. The lignin component measured and extracted by various structural characterization methods has high purity, the functional structure of the lignin is kept integral in the separation and regeneration process, and the extracted lignin has high chemical activity.

Description

technical field [0001] The invention relates to a method for extracting high molecular compounds, in particular to a method for extracting biomass lignin by using quaternary ammonium base. Background technique [0002] Biomass is mainly composed of cellulose, hemicellulose and lignin. From the perspective of structure and chemical composition, lignin has the most complex structure. It is a three-dimensional complex structure formed by disorderly polymerization of phenylpropane monomers substituted by hydroxyl or methoxy groups. It is an abundant raw material for aromatic compounds in chemical and chemical production. resource. [0003] The depletion of fossil energy, the abundant reserves of lignin, and the rapid development of lignin science determine the sustainable development of lignin's economic benefits. The cost of lignin is low, and lignin and its derivatives have multiple functions, and can be used as dispersants, adsorbents / desorbents, oil recovery aids, and asph...

Claims

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Application Information

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IPC IPC(8): C08H7/00
CPCC07G1/00C08H6/00
Inventor 贾红华程芳朱瀛奎韦萍周俊
Owner NANJING UNIV OF TECH
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