Enzymatic hydrolysis lignin based epoxy resin preparation method

A technology for enzymatic hydrolysis of lignin and epoxy resin, applied in the direction of epoxy resin glue, adhesive type, adhesive, etc., can solve the problems of difficult processing, complex process, high environmental risk, etc. The effect of tensile strength, high chemical reactivity and wide application prospects

Active Publication Date: 2017-06-23
山西生物质新材料产业研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN101348558A discloses an enzymatic lignin epoxy resin and its preparation method: under the action of a catalyst, the hydroxyl contained in the enzymatic lignin or its derivatives is used for the reverse esterification reaction with dianhydride to generate lignin and diacid anhydride. The prepolymer of acid anhydride is then reacted with glycidyl ether, through etherification, ring closure reaction to obtain enzymatic lignin-polyester type epoxy resin, this method needs to carry out carboxylation modification to enzymatic lignin, at the same time in epoxy A large amount of organic solvents such as toluene are used in the chemical process, which leads to high industrial processing costs and high environmental risks
CN100528926C discloses a raw material formula of enzymolysis lignin epoxy resin and its preparation method. It mainly reacts enzymolysis lignin and bisphenol A with epichlorohydrin to synthesize epoxy resin. The disadvantage of difficult post-processing, and still not getting rid of the use of bisphenol A
In this preparation method, enzymatic hydrolysis of lignin requires hydroxymethylation, and the synthesis process is complex and costly, which is not conducive to industrialization
[0005] Therefore, the current method of using lignin to prepare epoxy resin still has problems such as high raw material cost, low quality, complicated process and high environmental risk.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh 10g of enzymatic lignin, 2g of tetrabutylammonium bromide, add to 118g of epichlorohydrin, stir evenly, add 2g of sodium hydroxide, stir at 80°C for 5h, cool down to 60°C, add 25g dropwise 20wt% lye, dropwise added to complete the reaction, and reacted for 3 hours. The upper organic phase was taken, washed three times with water, and dried to obtain the resin. The resin cured product can be obtained by adopting low molecular weight curing agent polyamide and diluent ethylene glycol diglycidyl ether to carry out curing reaction under high temperature and high pressure.

Embodiment 2

[0016] Weigh 10g of enzymatic lignin, 2g of tetrabutylammonium bromide, add to 118g of epichlorohydrin, stir evenly, add 2g of sodium hydroxide, stir at 80°C for 5h, cool down to 60°C, add 25g dropwise 20wt% lye, dropwise added to complete the reaction, and reacted for 3 hours. The upper organic phase was taken, washed three times with water, and dried to obtain the resin. Using triethylenetetramine as a curing agent to carry out curing reaction under high temperature and high pressure can obtain a resin cured product.

Embodiment 3

[0018] Weigh 15g of enzymatic lignin, 3.5g of tetrabutylammonium bromide, add to 210g of epichlorohydrin, stir evenly, add 3g of sodium hydroxide, reflux at 80°C for 5h, cool down to 60°C, drop by drop 40g of 20wt% lye was added dropwise and reacted for 3 hours. The upper organic phase was taken, washed three times with water, and dried to obtain the resin. The resin cured product can be obtained by adopting low molecular weight curing agent polyamide and diluent ethylene glycol diglycidyl ether to carry out curing reaction under high temperature and high pressure.

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PUM

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Abstract

The invention discloses an enzymatic hydrolysis lignin based epoxy resin preparation method which comprises the following steps of adding 10 to 20 weight parts of enzymatic hydrolysis lignin and 2 to 5 weight parts of a phase transfer reagent into 118 to 302 weight parts of epoxy chloropropane solution, heating to 50 to 100 DEG C, fully stirring so that the materials are evenly mixed, adding 7 to 15 weight parts of a catalyst, performing reflux reaction for 3 to 8 hours, washing reactant for 3 to 5 times after the reaction finishes, taking an organic layer, performing reduced pressure distillation under the condition of temperature being 20 to 100 DEG C, and removing residual epoxy chloropropane and deionized water to obtain enzymatic hydrolysis lignin based epoxy resin. The method has the advantage of preventing poisonous and harmful reagent from being used; furthermore, a synthesizing technology is simpler, cost is lower, and industrialization is facilitated.

Description

technical field [0001] The invention relates to the technical field of epoxy resin production, in particular to a preparation method of enzymatically decomposing lignin-based epoxy resin. Background technique [0002] Lignin is a renewable and degradable natural polymer material second only to cellulose in nature. There are a large number of highly active groups such as phenolic hydroxyl groups and alcoholic hydroxyl groups in the molecular structure of enzymatic lignin, which can be directly used in a series of chemical reactions to synthesize new polymer materials and expand the types, properties and application prospects of polymer materials. The use of lignin to replace bisphenol A to synthesize epoxy resin was proposed in the 1970s, but it has not been industrialized. The main reason is that it is difficult and costly to extract highly active lignin from plants. [0003] The existing industrial lignin on the market mainly includes alkali lignin, sulfate lignin and lign...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/04C08H7/00C08H8/00C08L63/00C09J163/00
CPCC08G59/04C08H8/00C08L63/00C09J163/00
Inventor 陈璐王骞
Owner 山西生物质新材料产业研究院有限公司
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