Process for Separation of Mild Acid Catalyzed Lignin Depolymerization Products and Its Extraction Products

A depolymerization product, lignin technology, applied in the field of natural organic polymer chemical industry, can solve the problems of separation and screening of depolymerization products, complex reaction products, etc., and achieve the effect of low cost, low process temperature and convenient operation

Active Publication Date: 2019-05-07
HUANGSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, for industrial-grade lignin, it usually contains more sugars, inorganic substances and insoluble impurities. After acid-catalyzed oxidation, the reaction products are more complex, and it is particularly difficult to separate and screen its depolymerization products.

Method used

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  • Process for Separation of Mild Acid Catalyzed Lignin Depolymerization Products and Its Extraction Products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Using phenol as a solvent, add pre-sulfonated alkali lignin, the quality of phenol is 75g, the quality of alkali lignin is 30g, add concentrated hydrochloric acid under normal pressure conditions, heat at 94 ° C under stirring conditions, the concentration of concentrated hydrochloric acid The dosage is 4wt% of the total amount of phenol and alkali lignin. After being heated to a predetermined temperature, the heat preservation liquefaction reaction is carried out for 30 minutes to obtain the alkali lignin depolymerization product;

[0028] (2) The above-mentioned lignin depolymerization products were extracted by solvent continuous extraction, that is, the above-mentioned lignin depolymerization products were continuously extracted with diethyl ether at 50°C for 6 days, the solvent was separated, and then continuously extracted with methanol at 70°C for 1 day, Finally, the extracted product is obtained.

[0029] By adjusting the depolymerization process and separatio...

Embodiment 2

[0034] (1) Take phenol as solvent, add lignosulfonate, the quality of phenol is 5g, the quality of lignosulfonate is 20g, add concentrated phosphoric acid under normal pressure condition, heat 100 ℃ under stirring condition, the concentrated phosphoric acid The dosage is 5wt% of the total amount of phenol and lignosulfonate. After being heated to a predetermined temperature, the heat preservation liquefaction reaction is carried out for 15 minutes to obtain the depolymerization product of lignosulfonate;

[0035] (2) Use the simultaneous distillation extraction method to extract the above-mentioned lignin depolymerization products, that is, use a simultaneous distillation extraction device, one side of which is the acid-catalyzed depolymerization product, add water according to the volume ratio of 1:2, heat at 120 ° C, and the other side is acetone, Continuously extract at 70°C for 1 day, separate the solvent, continue to extract with acetic acid at 85°C for 6 days, and finally...

Embodiment 3

[0039] (1) Using phenol as a solvent, add pre-sulfonated high-boiling alcohol lignin, the mass of phenol is 50g, the quality of high-boiling alcohol lignin is 40g, add concentrated sulfuric acid under normal pressure conditions, and heat at 96°C under stirring conditions , the amount of concentrated sulfuric acid is 6wt% of the total amount of phenol and high-boiling alcohol lignin, after being heated to a predetermined temperature, heat-preserved and liquefied for 45 minutes to obtain a high-boiling alcohol lignin depolymerization product;

[0040] (2) The above-mentioned lignin depolymerization products were extracted by solvent continuous extraction, that is, the above-mentioned lignin depolymerization products were continuously extracted with tetrahydrofuran at 50°C for 3 days, the solvent was separated, and then continuously extracted with acetonitrile at 90°C for 3 days, Finally, the extracted product is obtained.

[0041] By adjusting the depolymerization process and se...

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Abstract

The invention discloses a process for separating a product of mild acid-catalyzed depolymerization of lignin. The process comprises the following steps: (1) with phenol as a solvent, adding main and auxiliary acidic catalysts under the conditions of stirring and normal pressure heating or normal pressure, wherein the usage amount of the acidic catalysts is 1 to 6 wt% of the total amount of phenol and lignin, adding lignin in batch, wherein a mass ratio of lignin to phenol is 4: 1-20, carrying out a catalytic reaction at a constant temperature of 90 to 150 DEG C for a period of time and selectively acquiring the product of mild acid-catalyzed depolymerization of lignin; and (2) extracting the depolymerization product of lignin by using a continuous solvent extraction method or simultaneous distillation and extraction method so as to obtain extraction products. Moreover, the invention also discloses the extraction products prepared by using the process. The process is low in separating temperature, so no damage is posed to the structure of the extraction products; the process is convenient to operate, low in cost, green, environment-friendly; an extraction agent can be continuously used; and compounds which can be extracted by the extraction agent can be thoroughly extracted by using a small amount of the extraction agent.

Description

technical field [0001] The invention belongs to the field of natural organic polymer chemical industry; it relates to a process for separating lignin depolymerization products and its products; more specifically, it relates to a process for separating mild acid-catalyzed lignin depolymerization products and its extraction products. Background technique [0002] Lignin is an amorphous, three-dimensional natural polymer, which accounts for about 10-35% of the total cell wall content, about 30% of the earth's organic carbon content, and about 40% of bio-based energy. The macromolecular structure of lignin is complex and has not been fully clarified so far. It is generally believed that lignin is composed of syringyl (3,5-dimethoxy-4-hydroxyphenylpropane), guaiacyl (3-methoxy -4-hydroxyphenylpropane) and p-hydroxyphenyl-(4-hydroxyphenylpropane) unit structures are complex organic polymers formed by C-O-C or C-C bonds, most of which are β-O-4 linkages. The molecular structure of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/04
CPCC07B63/00C07G1/00
Inventor 方红霞李长江钱晨崔朋杨永梅刘同欢
Owner HUANGSHAN UNIV
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