Modified lignin as well as preparation method thereof and application of modified lignin in phenolic resin adhesive

A lignin and modification technology, applied in the field of materials, can solve the problem of high process requirements

Active Publication Date: 2020-07-10
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Purpose of the invention: The technical problem to be solved by the present invention is to provide a modified lignin and its preparation method in view of the need to use high-pressure equipment and high process requirements in the lignin modification process in the prior art. Hydroxylation modification of lignin through biocatalytic hydroxylation reaction without using toxic reagents and environmentally unfriendly solvents avoids the generation of unpleasant odors, and the obtained lignin increases the content of phenolic hydroxyl groups, thereby improving In order to improve the reactivity with formaldehyde, it can replace phenol to prepare lignin-based phenolic resin adhesives, which are used in various new polymer materials such as adhesives and phenolic plastics.

Method used

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  • Modified lignin as well as preparation method thereof and application of modified lignin in phenolic resin adhesive
  • Modified lignin as well as preparation method thereof and application of modified lignin in phenolic resin adhesive
  • Modified lignin as well as preparation method thereof and application of modified lignin in phenolic resin adhesive

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] In 10 mL of 50 mM pH 6.0 potassium phosphate buffer, 0.05 g of alkali lignin, 0.1 mM of FAD, 5 mM of BNAH were added, and finally 30 U / mL of phenol monooxygenase was added. Put it in a shaker at 30°C and 200rpm to react, and the reaction liquid is communicated with the outside air. After reacting for 12 hours, filter the reaction solution, wash it with water until neutral, dry it in a vacuum oven at 80°C to constant weight, obtain hydroxylated modified lignin after drying, weigh the product, and the yield is 76%, unmodified alkali lignin The phenolic hydroxyl content was 2.66%, the hydroxylated lignin phenolic hydroxyl content was 4.22%, and the phenolic hydroxyl content increased by 1.56%.

Embodiment 2

[0065]

[0066] In 20mL water, add alkali lignin 0.2g, FAD 0.2mM, C 10 h 16 N 2 O 10mM, finally add phenol monooxygenase 40U / mL. Put it in a shaker at 30°C and 150rpm to react, and the reaction liquid is connected with the outside air. After reacting for 12 hours, the reaction solution was filtered, washed until neutral, and dried in a vacuum oven at 80°C to constant weight. After drying, the hydroxylated modified lignin was obtained, and the product was weighed. The yield was 80%, and the unmodified alkali lignin The content of the phenolic hydroxyl group in the base is 2.66%, the content of the hydroxylated modified lignin is 4.44%, and the content of the phenolic hydroxyl group increases by 1.78%.

Embodiment 3

[0068]

[0069] In 30mL of 50mM pH 7.0 potassium phosphate buffer, add lignosulfonate 0.6g, FAD 0.5mM, C 11 h 18 N 2 O 50mM, finally add phenol monooxygenase 50U / mL. Put it at 40°C and react in a shaker at 200 rpm, and the reaction solution is connected to the outside air. After reacting for 15 hours, the reaction solution was filtered, washed until neutral, and dried in a vacuum oven at 80°C to constant weight. After drying, the hydroxylated modified lignin was obtained, and the product was weighed. The yield was 82%, and the unmodified lignin The phenolic hydroxyl content of sulfonate was 2.32%, the hydroxylated lignin phenolic hydroxyl content was 4.92%, and the phenolic hydroxyl content increased by 2.60%.

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Abstract

The invention discloses modified lignin as well as a preparation method and application thereof in a phenolic resin adhesive, and the preparation method of the modified lignin comprises the followingsteps: mixing lignin and a biocatalyst in a solvent, and reacting to obtain the modified lignin. The method has the advantages of mild reaction conditions, simple post-treatment, strong operability and environmental protection. Besides, phenolic hydroxyl is introduced into the modified lignin through biological catalytic hydroxylation, so that the number of active sites is increased, the activityof the modified lignin is enhanced, and the modified lignin can be used for preparing a phenolic resin adhesive and has important significance in efficient utilization of lignin and relief of petroleum resource pressure.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a modified lignin, a preparation method thereof and an application in phenolic resin adhesives. Background technique [0002] Lignin is the most abundant and important natural polymer substance after cellulose in quantity. It is estimated that about 6×10 14 Lignin is a resource with great potential. Since the molecular structure of lignin contains a certain number of active groups such as aromatic groups, alcoholic hydroxyl groups, carbonyl groups, phenolic hydroxyl groups, methoxyl groups, carboxyl groups, ether bonds and conjugated double bonds, lignin can be oxidized, reduced, hydrolyzed, Many chemical reactions, such as alcoholysis, acylation, alkylation, polycondensation or graft copolymerization, can be widely used in the synthesis of biomass-based polymer materials. Moreover, the unsubstituted active hydrogen on the lignin benzene ring structure can underg...

Claims

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Application Information

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IPC IPC(8): C08H7/00C09J161/12C08G8/20C08G8/10
CPCC08H6/00C09J161/12C08G8/20C08G8/10
Inventor 朱晨杰胡有钦应汉杰韩耀颖高成庄伟李明陈彦君欧阳平凯
Owner NANJING UNIV OF TECH
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