Enzymatic hydrolysis lignin epoxide resin and preparation thereof

A technology of plain epoxy resin and enzymatic hydrolysis of lignin, which is applied in the field of enzymatic hydrolysis of lignin epoxy resin and its preparation, can solve the problems of high price and high boiling alcohol, consume more energy, change structure and the like, and reduce production cost. , the effect of improving competitiveness and improving performance

Active Publication Date: 2009-01-21
重庆辉泰化工销售有限公司
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  • Abstract
  • Description
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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, there is also a new method for preparing epoxy resin from high-boiling alcohol lignin prepared by high-boiling alcohol solvent method. High-boiling alcohol lignin is used to prepare epoxy resin (national invention patent ZL200410061295.X) than using lignosulfonate as raw material There are many improvements, but the high-boiling alcohol solvent method needs to use high-boiling alcohol with high price when preparing lignin, and the recovery of high-boiling alcohol solvent needs to consume more energy

Method used

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preparation example Construction

[0036] The preparation method of the enzymatic lignin-dianhydride prepolymer is as follows: according to the formula ratio, the enzymatic lignin and dianhydride are dissolved in ethylene glycol, and then put into the Mix well in the reactor, add sulfuric acid catalyst, control the reaction temperature at 110-145°C, react under constant stirring for 1-8h, take it out and let it cool down, neutralize the reaction product with NaOH solution until the pH value is equal to 7, and use decompression The water is distilled off to obtain the enzymatic lignin-dianhydride prepolymer.

[0037] The enzymatic lignin-dianhydride prepolymer that has been prepared is reacted with glycidyl ether under the action of a catalyst for etherification and ring closure reaction to obtain enzymatic lignin-polyester epoxy resin: the enzymatic lignin The preparation method of plain epoxy resin is as follows: react the already prepared enzymatic lignin-dianhydride prepolymer with glycidyl ether under the a...

Embodiment 1

[0042] Dissolve 50 grams of enzymatic lignin and 100 grams of maleic anhydride in 50 grams of ethylene glycol, then add 15 grams of sulfuric acid aqueous solution with a weight concentration of 50% as a catalyst, and then put it into a mixture equipped with a magnetic stirrer, a thermometer, Fully mix in a three-necked round bottom flask with a reflux condenser, heat to control the reaction temperature to 130°C, turn on nitrogen protection, react for 5 hours under constant stirring, take it out and cool to room temperature, neutralize the reaction product with 6.2 grams of NaOH solution, and use a decompression Distillation removes water, obtains 186.4 grams of prepolymers; the prepolymers are divided into five parts, and ethylene glycol diglycidyl ether, 10 grams of toluene and 3.5 grams of hydroxide are added to each part of the prepolymers according to the ratio shown in Table 1. Sodium catalyst, after reacting at 80°C for 2.0h, take it out, cool to room temperature; wash th...

Embodiment 2

[0046] Dissolve 25 grams of enzymatic lignin and 40 grams of glutaric anhydride in 30 grams of ethylene glycol, then add 6 grams of sulfuric acid aqueous solution with a weight concentration of 50% as a catalyst, then put it into a mixture equipped with a magnetic stirrer, a thermometer, and reflux condensation Mix well in a three-necked round-bottomed flask, heat to control the reaction temperature to 140°C, turn on nitrogen protection, react under constant stirring for 4 hours, take it out and cool to room temperature to obtain 90.4 grams of prepolymer; then add 180 grams of ethylene glycol Diglycidyl ether, 25 grams of toluene and 5.5 grams of sodium hydroxide catalyst were reacted at 80°C for 2.0h, then taken out and cooled to room temperature; the product was washed with pure water to remove water-soluble components, and placed at 60°C for vacuum drying Drying in an oven to obtain a brown high-viscosity liquid, that is, to obtain polyester lignin epoxy resin. Add 35 grams...

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Abstract

The invention provides an enzymolysis lignin epoxy resin and a preparation method thereof. The raw materials include: an enzymolysis lignin-dianhydride prepolymer, a glycidol ether, a catalyst, a curing agent and a filler. The preparation method comprises the following steps that: under the action of the catalyst, an etherification of a hydroxyl group contained in the enzymolysis lignin or a derivative of the enzymolysis lignin and dianhydride is carried to synthesize a prepolymer of enzymolysis lignin-dianhydride; then the prepolymer reacts with the glycidol ether and undergoes etherification and ring closing reaction to obtain an enzymolysis lignin--polyester type epoxy resin. The enzymolysis lignin adopted by the method is natural macromolecular material extracted from the residues which is produced in the preparation of alcohol through the fermentation of wood chips, bamboo and stalk, thereby not only effectively utilizing biological resources, but also replacing petrochemical raw materials. The enzymolysis lignin epoxy resin which can be used as a modifier for engineering materials, adhesives, paints and macromolecular materials has a broad application prospect.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of biomass resources and epoxy resin production, and more specifically relates to an enzymolysis lignin epoxy resin and a preparation method thereof. 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 the performance of epoxy resin....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/02C08H5/02
Inventor 程贤甦陈为健
Owner 重庆辉泰化工销售有限公司
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