Enzymatic hydrolysis lignin epoxy resin material formula and its preparation method

A technology of plain epoxy resin and enzymatic lignin, which is applied in the field of comprehensive utilization of biomass resources and epoxy resin manufacturing industry, can solve the problems of high impurity content, adverse effects on the performance of epoxy resin, and high price, and achieve high purity. Effect

Active Publication Date: 2009-08-19
重庆兆演化工产品有限公司
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  • 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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  • Enzymatic hydrolysis lignin epoxy resin material formula and its preparation method

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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 hydrolyzed lignin, pour it into the flask, heat to 50℃, 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, then stir and reflux for 1 hour, in the pressure range 5-10mmHg, 1.5-2.0 hours, the excess epichlorohydrin is distilled off under reduced pressure at a temperature of 90℃ to obtain 10ml epichlorohydrin and a brown solid which is insoluble in water and has a certain degree of elasticity, which is obtained by washing and drying 10.85g brittle brown solid enzymatically hydrolyze lignin epoxy resin.

Embodiment 2

[0026] Measure 25ml epichlorohydrin and 15ml ethanol, add to a clean 250ml three-necked flask, weigh 5g enzymatically hydrolyzed lignin, pour it into the flask container, add 0.3g nano silica, heat to 50°C, 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, Stir and reflux for another 1 hour. Under the conditions of pressure range of 5-10mmHg, time of 1.5-2.0 hours, and temperature of 90℃, excess epichlorohydrin is distilled off under reduced pressure to obtain a brown solid with certain elasticity, which is washed and dried to obtain 10.60 g Nano-silica toughened and modified enzymatically hydrolyzed lignin epoxy resin.

Embodiment 3

[0028] Measure 25ml epichlorohydrin, add it to a clean 250ml three-necked flask, weigh 3g enzymatically hydrolyzed lignin and 2.5g bisphenol A, pour into the flask container, heat to 50℃, stir for 30min, let lignin and epoxy The chloropropane is fully dissolved and mixed. Within 20 minutes, add 0.8ml of 30% NaOH solution, heat up to 55-60°C, stir and reflux for 1 hour, heat up to 70°C, add 2ml of 30% NaOH solution within 20 minutes, then stir to reflux For 1 hour, the excess epichlorohydrin was evaporated under reduced pressure under the conditions of pressure range of 5-10mmHg, time of 1.5-2.0 hours and temperature of 90℃ to obtain 10ml of epichlorohydrin and a solid that is insoluble in water and has certain elasticity. After washing and drying, 11.30g of light brown solid enzymatically hydrolyzed lignin epoxy resin was obtained.

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Abstract

The invention provides a raw material formula of enzymatic lignin epoxy resin and its preparation method. The formula is enzymatic lignin or its derivatives, bisphenol A compound, epichlorohydrin or its mixed solution with an organic solvent, and a catalyst , curing agent, filler; the preparation method is to add enzymatic lignin or its derivatives to epichlorohydrin solution or its mixed solution with organic solvent, stir and dissolve, then add catalyst and add curing agent or curing agent and filler at the same time The mixture is heated to complete the reaction, and the final reactant is evaporated under reduced pressure to remove excess epichlorohydrin or organic solvent to obtain a water-insoluble brown solid, which is washed with water and dried to obtain an enzymatic lignin epoxy resin. The enzymatic lignin used in this method is a natural polymer material extracted from wood chips, bamboo, and grass straw, which not only effectively utilizes biological resources but also can replace petrochemical raw materials. The enzymatic lignin epoxy resin prepared can be used for engineering materials, Adhesives, coatings or modifiers of polymer materials have broad application prospects.

Description

Technical field [0001] The invention relates to the comprehensive utilization of biomass resources and epoxy resin manufacturing, and more specifically to a preparation method using enzymatic hydrolysis of lignin and its derivatives as the main raw material of lignin epoxy resin. Background technique [0002] Previous research reports on the preparation of epoxy resins have used lignosulfonate as a raw material. However, lignosulfonate is extracted from traditional papermaking "black liquor", which not only contains high impurity content, but also plant The natural lignin in the raw material undergoes major structural changes after the alkali and sulfite cooking, and the chemical activity is significantly reduced. The preparation of epoxy resin must undergo complex acidification, phenol modification and other complex modification treatments and purification processes. Only by reacting with epichlorohydrin can the lignin epoxy resin be obtained, and it will have a large adverse ef...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14C07G1/00C08L63/00C08H7/00
Inventor 程贤甦
Owner 重庆兆演化工产品有限公司
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