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A method for separating lignin from nut shells by using high boiling alcohol

A high-boiling alcohol and lignin technology, applied in the field of separating nut shell lignin, can solve the problems of low ash content of high-boiling alcohol lignin, low lignin yield, rising cost, etc. effect used

Inactive Publication Date: 2011-12-14
CHANGCHUN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention solves the problem of low lignin yield due to the compact structure of nutshell biomass, and the separated and prepared high-boiling alcohol lignin has low ash content and high activity, and the number average and weight average molecular weight of lignin are both about 5000. The polydispersity index of the lignin is about 1, and the detection of infrared and NMR proves that the separated lignin belongs to the guaiacyl-syringyl type lignin (GS type lignin)
The invention solves the environmental pollution and cost increase caused by the volatilization of low-boiling point solvents, and the solvent used is a high-boiling point solvent, which effectively solves the problems of solvent volatilization and recycling, and eliminates waste water, waste gas, and waste residue during the extraction process production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Example 1: 20 g of pine nut shell powder crushed to a particle size of 40 mesh is placed in a high-pressure reactor with a temperature-controlled stirring paddle, and 1,4-butanediol and water are added as solvents. 1,4-butanediol The volume ratio of water and water is 60:40; the mass g of pine nut shell powder and the volume mL of high-boiling alcohol aqueous solution are 1:4; the reaction temperature is 180 ° C, the reaction time is 1 hour, lignin is dissolved in high-boiling alcohol solvent; filter to remove cellulose, and the obtained cellulose can be used separately; then inject the filtrate into water, and the volume ratio of the filtrate to water is 1:1; lignin forms a precipitate; Rinse and dry to obtain lignin, and the extraction rate of lignin is 56.9%; the filtrate containing high boiling alcohol is distilled under reduced pressure to remove water, and the high boiling alcohol solvent can be recycled.

Embodiment 2

[0009] Example 2 20g of walnut shell powder crushed to a particle size of 80 meshes is placed in a high-pressure reactor with a temperature-controlled stirring paddle, and Mg(NO 3 ) 2 ·6H 2 O is used as a catalyst, adding 1,4-butanediol and water as a solvent, and the volume ratio of 1,4-butanediol and water is 70:30; the mass ratio of walnut shell powder and catalyst is 100:3; the mass of walnut shell powder The ratio of g to volume mL of high-boiling alcohol aqueous solution is 1:6; the reaction temperature is 220°C, the reaction time is 2 hours, lignin is dissolved in high-boiling alcohol solvent; the cellulose obtained by filtering can be used separately Then inject the filtrate into water, the volume ratio of filtrate to water is 1:2; lignin forms a precipitate; filter, the obtained lignin product is washed with warm water at 60°C, and dried to obtain lignin, and the extraction rate of lignin is 71.3 %; The filtrate containing high-boiling alcohol is distilled under red...

Embodiment 3

[0010] Example 3 Put 20 g of pine nut shell powder crushed to a particle size of 120 mesh, place it in a high-pressure reactor with a temperature-controlled stirring paddle, add MgCl 2 ·6H 2 O is used as a catalyst, adding ethylene glycol and water as a solvent, and the volume ratio of ethylene glycol and water is 90: 10; the mass ratio of pine nut shell powder and catalyst is 100: 7; the mass g of pine nut shell powder and the volume of high boiling alcohol aqueous solution The mL ratio is 1:14; the reaction temperature is 240°C, the reaction time is 3 hours, lignin is dissolved in a high-boiling alcohol solvent; the cellulose is removed by filtration, and the obtained cellulose can be used separately; then the filtrate is injected into water, The volume ratio of filtrate to water is 1:5; lignin forms a precipitate; after filtration, the obtained lignin product is washed with warm water at 30°C and dried to obtain lignin, and the extraction rate of lignin is 74.6%; the filtra...

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Abstract

The invention discloses a method for separating lignin from nut shells by using high-boiling alcohol. The high-boiling alcohol solution is used as a solvent to effectively separate lignin from nut shell biomass with dense structure under the action of a catalyst. The invention makes full use of waste biomass resources. The obtained lignin has low ash content, the hydroxyl value is 197.2mgKOH / g, the number average and weight average molecular weight are around 5000, and the polydispersity index of lignin is around 1, so it can be seen that the obtained lignin has high purity, good activity, The range of molecular weight distribution is narrow, and it is high-quality lignin. The invention solves the environmental pollution and cost increase caused by the volatilization of low-boiling solvents, and the solvents used are high-boiling solvents and water, effectively solving the problems of solvent volatilization and recycling. The invention solves the problem of low lignin yield due to the compact structure of the nut shell biomass, and can make the lignin extraction rate in the nut shell within the range of 56.9-74.6%.

Description

technical field [0001] The invention relates to a method for separating lignin from nut shells by using high boiling alcohol. Background technique [0002] With the increasing scarcity of fossil energy, the use of renewable biomass resources to obtain various chemicals has become one of the focuses of sustainable human development today. The research in this area is currently mainly focused on the conversion of hemicellulose and cellulose, but less research on lignin. Lignin is a polyphenolic three-dimensional network polymer composed of three basic structural monomers-guaiacyl, syringyl and p-hydroxyphenyl-structured phenylpropane units linked by ether bonds and carbon-carbon bonds. Aromatic compounds. As the only aromatic natural polymer that can be obtained from renewable resources in nature, lignin can be directly used to prepare gasoline, diesel, methanol and aromatic compounds, and is a potential effective substitute for petroleum resources. At present, the method o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
Inventor 李亚丰贾俊曲玉超
Owner CHANGCHUN UNIV OF TECH
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