Epoxy resin adhesive synthesized by alkali lignin through in-situ autocatalysis and preparation method of epoxy resin adhesive

A technology of alkali lignin and epoxy resin, applied in the field of materials and chemical industry, can solve the problems of agglomeration, reduced activity, difficulty in dissolution, etc., and achieve the effects of reducing production cost, improving lignin activity, and low free phenol content

Active Publication Date: 2017-07-25
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of difficult dissolution, agglomeration and activity reduction caused by lignin solid acid precipitation and re-dissolution after drying in the traditional method, and to remove miscellaneous sugars and metal ions by pretreating biomass raw materials The method eliminates the process of acid-precipitating lignin and its re-drying; overcomes the complex process of adding catalysts repeatedly in the modification of lig

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Mix sulfuric acid and rice husk, heat under stirring, then filter while hot, wash, and dry the filter residue; the mass fraction of the sulfuric acid is 4%, the heating temperature is 105°C, and the heating time is 4h, solid-liquid Mass ratio 1:7;

[0020] (2) mix the lye with the filter residue obtained in step (1), heat under stirring, collect the filtrate by filtration, and obtain the alkali lignin stock solution, wherein the lye is sodium hydroxide, and the concentration of the lye is 3mol / L, the heating temperature is 100°C, the heating time is 3h, and the solid-liquid mass ratio is 1:6;

[0021] (3) Bisphenol A is added to the alkali lignin stock solution obtained in step (2), and the alkali lignin is modified in situ with bisphenol A under stirring and heating conditions to obtain a phenolized modified alkali lignin solution , where the heating temperature is 70°C, the heating time is 2h, and the lignin substitution rate m 木质素 / (m 酚 +m 木质素 ) = 40%;

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Embodiment 2

[0026] (1) Mix sulfuric acid and straw residue, heat under stirring, then filter while hot, wash, and dry the filter residue; the mass fraction of the sulfuric acid is 8%, the heating temperature is 110°C, and the heating time is 4h, solid-liquid Mass ratio 1:8;

[0027] (2) The lye is mixed with the filter residue obtained in step (1), heated under stirring, and the filtrate is collected by filtration to obtain the alkali lignin stock solution, wherein the lye is potassium hydroxide, and the concentration of the lye is 5mol / L, the heating temperature is 100°C, the heating time is 4h, and the solid-liquid mass ratio is 1:8;

[0028] (3) Bisphenol A is added to the alkali lignin stock solution obtained in step (2), and the alkali lignin is modified in situ with phenol under stirring and heating conditions to obtain a phenolized modified alkali lignin solution, wherein , the heating temperature is 60°C, the heating time is 1.5h, the lignin substitution rate m 木质素 / (m 酚 +m 木...

Embodiment 3

[0033] (1) Mix sulfuric acid and bagasse, heat under stirring, then filter while hot, wash, and dry the filter residue; the mass fraction of the sulfuric acid is 6%, the heating temperature is 85°C, and the heating time is 3h, solid-liquid Mass ratio 1:6;

[0034] (2) Mix the lye with the filter residue obtained in step (1), heat under stirring, collect the filtrate by filtration, and obtain the alkali lignin stock solution, wherein the lye is a mixed solution of calcium hydroxide and sodium hydroxide, and the alkali The concentration of the liquid is 2mol / L, the heating temperature is 75°C, the heating time is 4h, and the solid-liquid mass ratio is 1:4;

[0035] (3) Bisphenol A is added to the alkali lignin stock solution obtained in step (2), and the alkali lignin is modified in situ with phenol under stirring and heating conditions to obtain a phenolized modified alkali lignin solution, wherein , the heating temperature is 70°C, the heating time is 1.5h, the lignin substit...

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Abstract

The invention relates to an epoxy resin adhesive synthesized by alkali lignin through in-situ autocatalysis. A preparation method comprises the following steps: step I, pickling a biomass raw material with sulfuric acid, and filtering and drying the pickled biomass raw material to obtain filter residues; step II, carrying out reaction on alkali liquor with the filter residues, and filtering a reactant to obtain an alkali lignin stock solution; step III, directly adding a phenolic compound in the alkali lignin stock solution, and carrying out in-situ phenolate modification; step IV, directly adding epoxy chloropropane or a derivative thereof in a phenolate lignin solution, and carrying out molecule in-situ polymerization; and step V, rapidly adding cold deionized water in reaction liquid, and brewing obtained precipitates with hot deionized water to obtain final residual viscous substances as the lignin modified epoxy resin adhesive. Processes of alkali lignin molecule extraction, in-situ modification and epoxy resin adhesive synthesis, involved in the invention, are continuous, and the efficiency is greatly improved. Meanwhile, in the alkali lignin in-situ modification and epoxy resin synthesis processes, a catalyst does not need to be added additionally, and autocatalytic reaction is realized.

Description

technical field [0001] The invention relates to the fields of materials and chemicals, in particular to an epoxy resin adhesive obtained by extracting alkali lignin molecules, in-situ autocatalytic modification and autocatalytic synthesis and a preparation method thereof. Background technique [0002] Epoxy resin adhesives have excellent bonding properties, mechanical properties, electrical properties and good versatility, and are widely used in various industries. At present, most epoxy resins with excellent performance are prepared from bisphenol A, which is expensive and highly toxic, causing serious pollution and harm to the environment. Therefore, it is of great practical significance to find a new environmentally friendly and cheap raw material to replace bisphenol A. [0003] Lignin is a renewable aromatic non-petroleum resource natural high polymer, which has high carbon content and is rich in various functional groups, and can undergo various chemical reactions. Th...

Claims

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Application Information

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IPC IPC(8): C08G59/06C08H7/00C09J163/00
CPCC08G59/063C08H6/00C09J163/00
Inventor 石刚李赢白绘宇王大伟倪才华周雪映
Owner JIANGNAN UNIV
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