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Enzymatic hydrolysis lignin epoxy resin material formula and its preparation method

A technology of plain epoxy resin and enzymatic hydrolysis of lignin, which is applied in the fields of comprehensive utilization of biomass resources and epoxy resin manufacturing industry, can solve the problems of high impurity content, high price, high energy consumption of high-boiling alcohol solvent, etc. high purity effect

Active Publication Date: 2007-05-23
重庆辉泰化工销售有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There is a precedent for using lignosulfonate as a raw material in previous research reports on the preparation of epoxy resins, but lignosulfonate is extracted from traditional papermaking "black liquor", which not only contains high impurities, but also plants The natural lignin in the raw material undergoes major structural changes after cooking with alkali and sulfite, and its chemical activity is significantly reduced. The preparation of epoxy resin must undergo complex modification and purification processes such as acidification and phenolization modification. Then react with epichlorohydrin to get lignin epoxy resin, and it will have a greater adverse effect on the performance of epoxy resin
In addition, a new method of preparing epoxy resin from high boiling alcohol lignin prepared by high boiling alcohol solvent method has been studied. The preparation of epoxy resin from high boiling alcohol lignin has many improvements compared with using lignin sulfonate as raw material, but high boiling alcohol The solvent method process needs to use higher-priced high-boiling alcohols when preparing lignin, and the recovery of high-boiling alcohol solvents requires more energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Measure 21ml of epichlorohydrin, add it to a clean 250ml three-necked flask, weigh 5g of enzymatically decomposed lignin, pour it into the flask container, raise the temperature to 50°C, stir for 30min, let the lignin and epichlorohydrin fully dissolve and mix, Add 0.8ml of 30% NaOH solution within 20 minutes, raise the temperature to 55-60°C, stir and reflux for 1 hour, raise the temperature to 70°C, add 2ml of 30% NaOH solution within 20 minutes, and stir and reflux for 1 hour. 5-10mmHg, the time is 1.5-2.0 hours, and the excess epichlorohydrin is evaporated under reduced pressure at a temperature of 90°C to obtain 10ml of epichlorohydrin and a brown solid that is insoluble in water and has a certain elasticity, which is washed and dried to obtain 10.85g brittle brown solid enzymatic lignin epoxy resin.

Embodiment 2

[0026] Measure 25ml of epichlorohydrin and 15ml of ethanol, add them into a clean 250ml three-neck flask, weigh 5g of enzymatic lignin, pour it into the flask container, add 0.3g of nano-silica, heat up to 50°C, and stir for 30min. Let the lignin and epichlorohydrin fully dissolve and mix, add 2.0ml of 30% NaOH solution within 20 minutes, heat up to 55-60°C, stir and reflux for 1 hour, add 0.4g of ethylenediamine curing agent and heat up to 70°C, Then stir and reflux for 1 hour, under the conditions of pressure range 5-10mmHg, time 1.5-2.0 hours, and temperature 90°C, excess epichlorohydrin is evaporated under reduced pressure to obtain a brown solid with certain elasticity, which is washed and dried to obtain 10.60 g nanosilica toughened modified enzymatic lignin epoxy resin.

Embodiment 3

[0028] Measure 25ml of epichlorohydrin, add it to a clean 250ml three-neck flask, weigh 3g of enzymatic lignin and 2.5g of bisphenol A, pour it into the flask container, raise the temperature to 50°C, and stir for 30min to let the lignin and epoxy Fully dissolve and mix the chloropropane, add 0.8ml of 30% NaOH solution within 20 minutes, raise the temperature to 55-60°C, stir and reflux for 1 hour, raise the temperature to 70°C, add 2ml of 30% NaOH solution within 20 minutes, and then stir and reflux For 1 hour, under the conditions of a pressure range of 5-10mmHg, a time of 1.5-2.0 hours, and a temperature of 90°C, distill off excess epichlorohydrin under reduced pressure to obtain 10ml of epichlorohydrin and a water-insoluble solid with certain elasticity , washed with water and dried to obtain 11.30 g of light brown solid enzymatic lignin epoxy resin.

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Abstract

The invention provides a raw materials formula of enzymolysis lignin epoxy resin and its fabrication method. The formula includes enzymolysis lignin or its derivatives, bisphenol A-type compound, epichlorohydrin or its mixture with organic solvent, catalyst, curing agent, and filler. The preparation method includes adding enzymolysis lignin or its derivatives into epichlorohydrin solution or its mixture with organic solvent, stirring and adding catalyst, curing agent or the mixture of curing agent and filler, heating and reacting completely, vacuum-distilling to remove the excessive epichlorohydrin or organic solvent to obtain brown solid insoluble in water, washing, and drying to obtain enzymolysis lignin epoxy resin. The adopted enzymolysis lignin is the natural polymer material extracted from wood, bamboo and straw, which not only effectively use the biological resources, but also can replace petrochemical raw materials. The prepared enzymolysis lignin epoxy resin can be used for engineering materials, adhesives, coating or polymer materials modifier, which has a broad application prospect.

Description

technical field [0001] The invention relates to comprehensive utilization of biomass resources and epoxy resin manufacturing, and more specifically to a preparation method using enzymatically hydrolyzed lignin and its derivatives as the main raw material of lignin epoxy resin. Background technique [0002] There is a precedent for using lignosulfonate as a raw material in previous research reports on the preparation of epoxy resins, but lignosulfonate is extracted from traditional papermaking "black liquor", which not only contains high impurities, but also plants The natural lignin in the raw material undergoes major structural changes after cooking with alkali and sulfite, and its chemical activity is significantly reduced. The preparation of epoxy resin must undergo complex modification and purification processes such as acidification and phenolization modification. Then react with epichlorohydrin to obtain lignin epoxy resin, and it will have a greater adverse effect on ...

Claims

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Application Information

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IPC IPC(8): C08G59/14C08H7/00
Inventor 程贤甦
Owner 重庆辉泰化工销售有限公司
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