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A kind of preparation method of enzymolysis lignin-based epoxy resin

A technology for enzymatically decomposing lignin and epoxy resin, applied in lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of complex extraction process, affected structure, low chemical activity, etc., and achieve high purity , mild experimental conditions and simple operation

Active Publication Date: 2019-02-19
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The prior art adopts the method for preparing epoxy resin from lignin to mainly have the following problems: (1) most of the raw materials used are through complicated extraction process, the cost is high, and the environment is polluted; (3) Before synthesizing epoxy resin, chemically modify lignin to improve its activity, and a large amount of organic reagents are used in the modification method

Method used

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  • A kind of preparation method of enzymolysis lignin-based epoxy resin
  • A kind of preparation method of enzymolysis lignin-based epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Weigh 10g of enzymatic lignin into a three-neck flask, add 100g of 20wt% lithium bromide molten salt hydrate, stir and heat up to 110°C, react for 4h, cool in an ice bath to terminate the reaction, filter with suction, wash with water, and dry in vacuum to obtain depolymerization enzymolysis lignin products. Dissolve 5g of depolymerized enzymatic lignin in 12g of epichlorohydrin, add 0.04g of tetramethylammonium bromide, stir and heat up to 60°C, add 5g of 20wt% NaOH solution dropwise, react for 2 hours, and adjust the pH of the reaction product to neutrality, distill under reduced pressure to remove excess epichlorohydrin and water, wash the distilled product to neutrality, and vacuum-dry to obtain a depolymerized enzymatic lignin-based epoxy resin product.

Embodiment 2

[0021] Weigh 10g of enzymolytic lignin into a three-neck flask, add 150g of 40wt% lithium bromide molten salt hydrate, stir and heat up to 140°C, react for 3h, cool in an ice bath to terminate the reaction, filter with suction, wash with water, and dry in vacuum to obtain depolymerization enzymolysis lignin products. Dissolve 5g of depolymerized enzymatic lignin in 25g of epichlorohydrin, add 0.06g of tetramethylammonium bromide, stir and heat up to 100°C, add 17g of 5wt% NaOH solution dropwise, react for 4 hours, and adjust the pH of the reaction product to neutrality, distill under reduced pressure to remove excess epichlorohydrin and water, wash the distilled product to neutrality, and vacuum-dry to obtain a depolymerized enzymatic lignin-based epoxy resin product.

Embodiment 3

[0023] Weigh 10g of enzymolytic lignin into a three-necked flask, add 150g of 40wt% lithium bromide molten salt hydrate, stir and heat up to 90°C, react for 5h, cool in an ice bath to terminate the reaction, filter with suction, wash with water, and dry in vacuum to obtain depolymerization enzymolysis lignin products. Dissolve 5g of depolymerized enzymatic lignin in 19g of epichlorohydrin, add 0.05g of tetramethylammonium bromide, stir and heat up to 70°C, add 4g of 10wt% NaOH solution dropwise, react for 3 hours, and adjust the pH of the reaction product to neutrality, distill under reduced pressure to remove excess epichlorohydrin and water, wash the distilled product to neutrality, and vacuum-dry to obtain a depolymerized enzymatic lignin-based epoxy resin product.

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Abstract

The invention relates to a method for preparing epoxy resin from zymolytic lignin. The method comprises the following steps: performing depolymerization treatment on the zymolytic lignin through a fused salt aquo-complex; increasing the content of phenolic hydroxyl group; controlling the temperature within 90-140 DEG C; performing thermal reaction for 1-5h; purifying a depolymerized product by the methods of suction filtration, washing with water, and the like; dissolving the depolymerized product in epoxy chloropropane; adding a phase transfer catalyst; increasing the temperature to 60-100 DEG C; adding an alkaline solution; reacting for 2-4h; adjusting pH of the product to be neutral; performing reduced pressure distillation; washing with water; and drying, thereby obtaining brown depolymerized zymolytic lignin-based epoxy resin solid powder. The raw materials adopted by the preparation method provided by the invention are high in purity; the chemical activity of the lignin is well maintained; the modifying process is environment-friendly and nontoxic; the modified effect is good; the process is simple; the application prospect is extensive; and the operability is high.

Description

technical field [0001] The invention relates to the technical field of comprehensive utilization of biomass resources and epoxy resin manufacturing, in particular to a method of preparing bio-based epoxy resin by using enzymolysis lignin obtained from enzymolysis residue in bio-ethanol production as raw material and depolymerizing molten salt hydrate. A new approach to resins. Background technique [0002] Lignin is the only renewable natural polymer that can provide aromatic compounds in nature, and its content is abundant, second only to cellulose. It is estimated that about 150 billion tons of lignin are produced worldwide every year through the growth of plants. Although my country's forest resources are not very rich, the annual lignin output of crop rice straw is 500-600 million tons. So far, more than 95% of the recovered lignin is concentrated and then burned, causing serious resource waste and environmental pollution. [0003] Epoxy resins generally refer to orga...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02C08H7/00C07G1/00
CPCC07G1/00C08G59/02C08H6/00
Inventor 王芳蒯君涛朱新宝
Owner NANJING FORESTRY UNIV
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