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Method of deep eutectic solvent modified lignin for epoxy resin curing agent

A technology of epoxy resin curing and low eutectic solvent, applied in the field of epoxy resin curing agent, can solve problems such as no reports yet, and achieve the effects of low price, easy reaction control, excellent operability and usability

Active Publication Date: 2019-02-22
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

DES modified lignin is a relatively new method of lignin modification. Xu Xudong et al. used choline chloride / urea deep eutectic solvent to modify lignin, and found that the solvent can reduce the methoxyl group in lignin. Hydroxyl formation, chemical activity can be improved, which can effectively replace part of phenol for phenolic resin adhesive, but DES has not been reported in the modification and application of epoxy resin curing agent

Method used

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  • Method of deep eutectic solvent modified lignin for epoxy resin curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 69.8g of choline chloride (abbreviated as ChCl) and 60.0g of urea (abbreviated as U), add them into a sealed container, and stir for about 10min at 55°C until the reaction liquid is transparent, that is, choline chloride / urea Deep eutectic solvent (referred to as ChCl / UDES). Cool ChCl / U DES to 25°C and measure its viscosity to be 1205mPa·s. Weigh 3.9g of corncob enzymatic lignin (CL for short) and add it to ChCl / U DES, stir evenly, raise the temperature to 90°C, and react for 6h to obtain a mixture of choline chloride / urea deep eutectic solvent modified lignin. system (ChCl / U DES-CL for short), this mixed system is the curing agent for epoxy resin, and its viscosity at 25°C is measured to be 884mPa·s.

[0020] Weigh 7.5g of ChCl / U DES-CL curing agent, add it to 60.0g of epoxy resin E-51 and stir evenly, and pour the mixture into the preheated In a good mold, first pre-cured at 140°C for 2 hours, then cured at 150°C for 2 hours, and then naturally cooled to room ...

Embodiment 2

[0022] According to the preparation method of ChCl / U DES-CL in Example 1, ChCl / U DES-CL curing agent was prepared.

[0023] Weigh 7.5g of ChCl / U DES-CL curing agent, add it into 60.0g of epoxy resin E-51 and stir evenly, and pour the mixture into the pre- In the heated mold, pre-cure at 140°C for 2 hours, then heat-cure at 160°C for 2 hours, and then cool to room temperature naturally to prepare a cured resin sample. The measured tensile strength is 55.2MPa, elongation at break It is 10.2%, and the tensile modulus of elasticity is 591.0MPa.

Embodiment 3

[0025] According to the preparation method of ChCl / U DES-CL in Example 1, ChCl / U DES-CL curing agent was prepared.

[0026] Weigh 8.6g of ChCl / U DES-CL curing agent, add it to 60.0g of epoxy resin E-51 and stir evenly, and pour the mixture into the pre- In the heated mold, pre-cured at 140°C for 2 hours, then cured at 160°C for 2 hours, and then cooled to room temperature naturally to prepare a cured resin sample. The measured tensile strength was 24.6MPa, and the elongation at break was 4.8%, and the tensile modulus of elasticity is 488.4MPa.

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Abstract

The invention relates to a preparation method of deep eutectic solvent modified lignin for an epoxy resin curing agent. The preparation method comprises the following steps: adding choline chloride and another raw material into a sealed container in a certain molar ratio, and stirring at 30-100 DEG C until reaction liquid is transparent, so as to obtain a deep eutectic solvent (DES); processing lignin at 60-140 DEG C for 1-12 hours, so as to obtain a mixture of modified lignin and DES, namely the epoxy resin curing agent. The preparation method is characterized in that after lignin is processed by virtue of multiple synergistic effects of salvation, catalysis, activation and the like of cheap and non-toxic choline chloride series DES, lignin can be directly taken as the epoxy resin curingagent without being separated, so that the separation, washing and regeneration steps after traditional activation treatment of lignin are reduced, and the process is simple and easy to control; and the prepared epoxy resin curing agent has the advantages of no toxin, low viscosity, use amount and price and good operability and usability.

Description

technical field [0001] The invention belongs to the field of epoxy resin curing agents, and in particular relates to a method for using deep eutectic solvent modified lignin in epoxy resin curing agents. Background technique [0002] Epoxy resin is an oligomer containing two or more epoxy groups in a molecule, with aliphatic, alicyclic or aromatic rings as the skeleton and capable of forming a thermosetting resin through the reaction of epoxy groups. Because of its good adhesion, low shrinkage, electrical insulation, chemical stability, wear resistance, high and low temperature resistance and other excellent properties, it is widely used in construction, machinery, electronics, aerospace and other fields. However, the epoxy resin itself has a linear structure, and its excellent performance must be achieved through the crosslinking of the curing agent. Therefore, the selection of the type and amount of the curing agent is an important part of the application of the epoxy resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/40C08H7/00
CPCC08G59/4007C08H6/00
Inventor 连海兰刘天勤洪枢
Owner NANJING FORESTRY UNIV
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