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A kind of method utilizing lignin to prepare heat-resistant epoxy resin

A technology of epoxy resin and lignin, applied in chemical recycling, fermentation and other directions, can solve the problems of not showing performance, not showing technical advantages, etc., and achieve the effect of high glass transition temperature and good heat resistance

Active Publication Date: 2018-01-30
HUANGSHAN HUIZHOU TIANMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned method of preparing epoxy resin with modified lignin as raw material has been improved based on many shortcomings of the prior art, the process is more simplified and the cost is reduced, and the yield of the epoxy resin is higher, but, for The preparation of some epoxy resins with special performance requirements does not show better performance. For example, in some fields, the preparation of epoxy resins with higher heat resistance requirements does not show its superior performance Technical advantages

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The method for preparing heat-resistant epoxy resin with lignin described in this embodiment comprises the following steps:

[0025] (1) Get the lignin and pulverize it, and carry out impurity pretreatment in a conventional way to remove the inorganic salt impurities in the lignin, and set aside;

[0026] Take 3kg of treated lignin, add 10kg of enzyme preparation solution with a mass concentration of 1wt%, and mix evenly. The enzyme preparation solution contains catalase and β-glucosidase with a mass ratio of 1:3; the reaction system is controlled at Carry out enzyme modification treatment at a temperature of 40°C, and separate solid-liquid to obtain lignin after enzyme modification treatment;

[0027] (2) Get the lignin 2kg after the above-mentioned enzyme modification treatment and mix with epichlorohydrin 4kg, adjust reaction system pH with NaOH solution to be 8-9, and add 12g HY type molecular sieve catalyst (silicon-aluminum ratio SiO 2 / Al 2 o 3 6), control the...

Embodiment 2

[0029] The method for preparing heat-resistant epoxy resin with lignin described in this embodiment comprises the following steps:

[0030] (1) Get the lignin and pulverize it, and carry out impurity pretreatment in a conventional way to remove the inorganic salt impurities in the lignin, and set aside;

[0031]Take 3kg of treated lignin, add 15kg of enzyme preparation solution with a mass concentration of 0.8wt%, and mix evenly. The enzyme preparation solution contains catalase and β-glucosidase with a mass ratio of 3:1; control the reaction system Carry out enzyme modification treatment at a temperature of 60°C, and separate solid and liquid to obtain lignin after enzyme modification treatment;

[0032] (2) Get the lignin 2kg after the above-mentioned enzyme modification treatment and mix with epichlorohydrin 6kg, regulate reaction system pH with NaOH solution to be 8-9, and add 80g HY type molecular sieve catalyst (silicon-aluminum ratio SiO 2 / Al 2 o 3 10), control the ...

Embodiment 3

[0034] The method for preparing heat-resistant epoxy resin with lignin described in this embodiment comprises the following steps:

[0035] (1) Get the lignin and pulverize it, and carry out impurity pretreatment in a conventional way to remove the inorganic salt impurities in the lignin, and set aside;

[0036] Take 5 kg of treated lignin, and add 10 kg of enzyme preparation solution with a mass concentration of 0.5 wt % to mix evenly. The enzyme preparation solution contains catalase and β-glucosidase with a mass ratio of 1:1; control the reaction system Enzyme modification treatment is carried out at a temperature of 50°C, and solid-liquid separation is carried out to obtain lignin after enzyme modification treatment;

[0037] (2) Get the lignin 3kg after the above-mentioned enzyme modification treatment and mix with epichlorohydrin 4kg, adjust reaction system pH with NaOH solution to be 8-9, and add 140g HY type molecular sieve catalyst (silicon-aluminum ratio SiO 2 / Al ...

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Abstract

The invention belongs to the technical field of epoxy resin synthesis, and in particular relates to a method for preparing heat-resistant epoxy resin by using lignin. The method for preparing heat-resistant epoxy resin described in the present invention uses common industrial by-product lignin as raw material processing, carries out enzyme modification treatment through the enzyme preparation solution containing at least catalase and β-glucosidase, and selects The HY-type molecular sieve catalyst is used to catalyze the epoxidation reaction, not only the catalyst is easy to obtain and can be recycled, but also the yield of the prepared epoxy resin can reach more than 99%, and the epoxy value of the product and the viscosity of the product are both high. and the prepared epoxy resin has higher glass transition temperature and better heat resistance, which is obviously higher than that of products prepared from general lignin in the prior art and bisphenol A type epoxy resin products, It can meet the heat resistance requirements of epoxy resin in some special fields.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin synthesis, and in particular relates to a method for preparing heat-resistant epoxy resin by using lignin. Background technique [0002] Epoxy resins generally refer to organic compounds containing two or more epoxy groups in their molecules. All polymer compounds containing epoxy groups in their molecular structures are collectively referred to as epoxy resins. Except for a few, their relative molecules The quality is not high. The molecular structure of epoxy resin is characterized by active epoxy groups in the molecular chain, and the epoxy groups can be located at the end, middle or ring structure of the molecular chain. Due to the active epoxy groups in the molecular structure, they can undergo cross-linking reactions with various types of curing agents to form insoluble polymers with a three-way network structure. [0003] Due to the unique epoxy group, hydroxyl group, ether bond and o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/04C08H7/00C12P1/00
CPCY02P20/584
Inventor 马万升程明光程鹏飞
Owner HUANGSHAN HUIZHOU TIANMA CHEM
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