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Method for preparing lignin anhydride cured epoxy resin by one-pot process

A technology for curing epoxy resin and plain acid anhydride is applied in the field of preparing lignin acid anhydride curing epoxy resin by one-pot method, which can solve the problems of reduced mechanical properties, complexity, and low addition ratio of epoxy resin, and achieves improvement of tensile strength performance. , reducing and energy loss, the effect of reducing material loss

Active Publication Date: 2019-10-22
NANJING FORESTRY UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, lignosulfonate has many impurities, complex structure, and low chemical reactivity. It needs to be modified in multiple steps before it can be used, and the addition ratio of lignosulfonate in epoxy resin is low, and it will lead to epoxy resin Decreased mechanical properties of resin
In recent years, organic solvent lignin and bio-fermentation lignin have been added to epoxy resins. Although the reactivity of lignin and the amount of lignin added have been improved, due to the many and complicated procedures, the energy and The loss of reagents is serious and does not conform to the concept of green environmental protection. Therefore, it is necessary to develop a new preparation method of epoxy resin that is green and environmentally friendly and has fewer processes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) After drying 6g of 40-60 mesh poplar wood powder, add 40g of ethylene glycol and 20g of dioxane, and add 0.9g of 98% concentrated sulfuric acid as a catalyst, react at 140°C for 30 minutes, filter out the residue, and vacuum the filtrate Rotary steaming, lignin is precipitated in water, and after repeated washing, it is freeze-dried for later use.

[0028] (2) Dissolve 1.07g of lignin in 10mL of acetone, add 7.11g of succinic anhydride, add 0.2mL of 1-methylimidazole as a catalyst, and react at 60°C for 12 hours.

[0029] (3) Add 13.26 g of epoxy monomer DER332 to the above reaction system, stir at 80° C. for 30 minutes, and remove the solvent by vacuum rotary evaporation of the uniformly stirred system.

[0030] (4) Add the epoxy resin system obtained after the above rotary evaporation into the mold, and set the curing temperature rise program as follows: 1 hour at 120°C, 4 hours at 160°C, and 1 hour at 180°C to obtain the target product.

Embodiment 2

[0032] (1) After drying 6g of 40-60 mesh poplar wood powder, add 40g of ethylene glycol and 20g of dioxane, and add 0.9g of 98% concentrated sulfuric acid as a catalyst, react at 140°C for 40 minutes, filter off the residue, and vacuum the filtrate Rotary steaming, lignin is precipitated in water, and after repeated washing, it is freeze-dried for later use.

[0033] (2) Dissolve 2.26g of lignin in 20mL of acetone, add 7.11g of succinic anhydride, add 0.2mL of 1-methylimidazole as a catalyst, and react at 60°C for 12 hours.

[0034] (3) Add 13.26 g of epoxy monomer DER332 to the above reaction system, stir at 80° C. for 30 minutes, and remove the solvent by vacuum rotary evaporation of the uniformly stirred system.

[0035] (4) Add the epoxy resin system obtained after the above rotary evaporation into the mold, and set the curing temperature rise program as follows: 1 hour at 120°C, 4 hours at 160°C, and 1 hour at 180°C to obtain the target product.

Embodiment 3

[0037] (1) After drying 6g of 40-60 mesh poplar wood powder, add 40g of ethylene glycol and 20g of dioxane, and add 0.9g of 98% concentrated sulfuric acid as a catalyst, react at 140°C for 30 minutes, filter out the residue, and vacuum the filtrate Rotary steaming, lignin is precipitated in water, and after repeated washing, it is freeze-dried for later use.

[0038] (2) Dissolve 5.07g of lignin in 20mL of acetone, add 7.11g of succinic anhydride, add 0.2mL of 1-methylimidazole as a catalyst, and react at 60°C for 12 hours.

[0039] (3) Add 13.26 g of epoxy monomer DER332 to the above reaction system, stir at 80° C. for 30 minutes, and remove the solvent by vacuum rotary evaporation of the uniformly stirred system.

[0040] (4) Add the epoxy resin system obtained after the above rotary evaporation into the mold, and set the curing temperature rise program as follows: 1 hour at 120°C, 4 hours at 160°C, and 1 hour at 180°C to obtain the target product.

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Abstract

The invention discloses a method for preparing a lignin anhydride cured epoxy resin by a one-pot process, and belongs to the field of biomass recycling and epoxy resin manufacturing. The method comprises the following steps: adding excess acid anhydride to perform carboxylating modification on an organic solvent lignin, and curing an epoxy resin with the remaining acid anhydride and the carboxylated lignin group to prepare the lignin anhydride cured epoxy resin. The whole preparation process is carried out in one pot, the preparation method has the characteristics of few process steps, low cost, greenness and environmental protection, and the obtained epoxy resin has the advantages of large lignin addition, uniform resin and good tensile properties, and has good industrial application prospects and values.

Description

technical field [0001] The invention belongs to the fields of biomass resource utilization and epoxy resin production, and more specifically relates to a method for preparing lignin anhydride-cured epoxy resin in one pot. Background technique [0002] Epoxy resin generally refers to an organic polymer compound containing two or more epoxy groups in the molecule, which can react with various types of curing agents to form an insoluble three-dimensional network polymer. This high polymer has excellent mechanical properties, adhesion, corrosion resistance and thermal stability, so it is widely used in coatings, adhesives, composite materials 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 resin. However, traditional curing agents, such as et...

Claims

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Application Information

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IPC IPC(8): C08G59/42
CPCC08G59/4207C08G59/4223
Inventor 潘晖王浩张永健
Owner NANJING FORESTRY UNIV
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