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A kind of bio-based epoxy resin curing agent and preparation method thereof

A technology based on epoxy resin and curing agent, applied in the field of bio-based epoxy resin curing agent and its preparation, can solve the problems of environmental pollution, waste of resources, etc., and achieve the reduction of molecular weight, increase of active sites, and increase of active hydroxyl content Effect

Active Publication Date: 2021-03-16
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, traditional epoxy resin curing agents are derived from non-renewable petrochemical resources, resulting in resource waste and environmental pollution.

Method used

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  • A kind of bio-based epoxy resin curing agent and preparation method thereof
  • A kind of bio-based epoxy resin curing agent and preparation method thereof
  • A kind of bio-based epoxy resin curing agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: Degradation-acidolysis of lignin

[0030] In a 50 mL reaction flask, 5 g of lignin was added and dissolved in 20 mL of DMF, and 5 g of HBr (mass fraction: 10%) was added, and reacted in a microwave reactor at 90° C. for 30 min. After the reaction, the reactant was cooled to room temperature, added dropwise to 200 mL of 2% hydrochloric acid solution, stirred for 30 min, centrifuged, the precipitate was taken, washed with distilled water, washed until the supernatant was neutral, freeze-dried, By NMR ( figure 2 ) and GPC to detect changes in molecular weight and phenolic hydroxyl before and after acid hydrolysis, the results are shown in Table 1.

[0031] figure 2 Using p-nitrobenzaldehyde as the internal standard, the -ArOH peak in the figure was integrated, and the phenolic hydroxyl content in the acid-hydrolyzed lignin was calculated to be 4.52%, while the phenolic hydroxyl content in the original lignin was 3.15%. [1] .

Embodiment 2

[0032] Example 2: Pyrolysis of lignin

[0033] 1.5 g of lignin was pyrolyzed at 200° C. for 3 hours to obtain pyrolyzed lignin. By NMR ( figure 1 ) and GPC to detect changes in molecular weight and phenolic hydroxyl content before and after pyrolysis, the results are shown in Table 1.

Embodiment 3

[0034] Example 3: Hydrogenolysis

[0035] In a 50mL reaction flask, add 1.5g of lignin and dissolve it in 20mL of methanol, then add 0.1g of (Pd) catalyst, feed the mixed solution into a high-pressure reaction kettle with a capacity of 100mL, and pass in 2MPa hydrogen, at 160°C Reaction 6h. After the reaction, the reactant was cooled to room temperature, filtered, and the filtrate was dried by rotary evaporation to obtain a sample. The changes in molecular weight and phenolic hydroxyl content before and after hydrogenolysis were detected by NMR and GPC, and the results are shown in Table 1 below.

[0036] Table 1 Changes in molecular weight and phenolic hydroxyl groups of lignin before and after acidolysis

[0037] sample Phenolic hydroxyl content (wt%) Alcohol hydroxyl content (wt%) Molecular weight (Da) Original lignin 3.15 2.81 3387 Lignin after acid hydrolysis 4.52 3.52 2010 lignin after hydrogenolysis 4.24 3.73 2127 Lignin af...

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Abstract

The invention discloses a bio-based epoxy resin curing agent and a preparation method thereof. The preparation method comprises the following steps: degraded lignin and amino acid are subjected to a condensation reaction to obtain an aminated lignin solution; nanofiltration and drying are conducted to obtain aminated lignin; and a curing reaction is carried out on the obtained aminated lignin andepoxy resin to obtain the bio-based epoxy resin curing agent. The preparation method has the main advantages that (1) the aminated lignin is proposed and prepared for the first time and is applied tothe epoxy resin curing agent according to the structural characteristics of the aminated lignin so as to replace the traditional aromatic amine curing agents 590 #, 701 # and 702 #; and (2) after pretreatment, the molecular weight is reduced, the content of active hydroxyl is increased, active sites capable of reacting with amino acid are increased, and the activity of a corresponding curing agentis increased; meanwhile, the lignin has good ultraviolet resistance, so that the prepared epoxy resin curing agent has stronger ultraviolet aging resistance.

Description

technical field [0001] The invention belongs to the technical field of biochemical industry, and in particular relates to a bio-based epoxy resin curing agent and a preparation method thereof. Background technique [0002] Epoxy resin is a commonly used thermosetting resin, which has good heat resistance, adhesiveness, chemical stability and dimensional stability, excellent mechanical properties, easy processing and molding, and is widely used in coatings, adhesives, electronic packaging materials, Composite materials and other fields. In order to obtain the required properties of the epoxy resin, the curing agent acts as a catalyst or reacts with the epoxy group through polyaddition or copolymerization to obtain a thermosetting network structure. This thermosetting three-dimensional network structure depends on the epoxy resin and curing agent. [0003] In the curing process of epoxy resin, the curing agent of addition polymerization type includes polyamine type, acid anh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/44C08H7/00
CPCC08G59/44C08H6/00
Inventor 沈涛蔺熙珃朱晨杰应汉杰庄伟李明胡瑞佳黎明晖
Owner NANJING TECH UNIV
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