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Epoxy curing agent taking bark as raw material and preparation method thereof

A technology of epoxy curing agent and bark, which is applied in the field of epoxy curing agent and its preparation, can solve the problems of low bark utilization level, and achieve the effect of promoting high value-added utilization, simple extraction, and low energy consumption

Active Publication Date: 2017-09-15
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the utilization level of bark in the current wood residue resources is still very low, except for a small amount of fuel and wood-based panel raw materials, most of them are treated as garbage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] In the first step, the American black pine bark is dried and crushed, and then passed through a 40-mesh sieve to obtain bark powder. After mixing the bark powder with NaOH and water in a weight ratio of 1:9:90, keep the temperature at 95°C for 3 hour, filter the residue, and obtain the bark extract after the liquid is spray-dried.

[0016] In the second step, 90g of bark extract, 900g of epichlorohydrin, 900g of 1,4-dioxane and 0.5g of benzyltriethylammonium chloride are added to a tank equipped with a mechanical stirring blade, a thermometer and a reflux condenser. In a three-necked flask, heat up to 75°C and stir thoroughly for 6 hours, then lower the temperature to 60°C, add 20g of sodium hydroxide and 12g of calcium oxide, stir for 9 hours, add 500mL of acetone to the mixture to dilute, then filter to remove solid salt, and then add acetone and excess After the epichlorohydrin is reclaimed by vacuum distillation, a kind of bark powder source epoxy compound (Bark-epo...

Embodiment 2

[0018] In the first step, the bark of the masson pine bark is dried and crushed and sieved through a 40-mesh sieve to obtain the bark powder. After mixing the bark powder with KOH and water in a weight ratio of 1:10:100, keep the temperature at 100°C for 3 hours , filter the residue, and obtain the bark extract after the liquid is spray-dried.

[0019] In the second step, in a 500mL three-necked flask equipped with a mechanical stirrer, a water separator and a thermometer, add 4.6g of bark extract and 6.5g of aminoethylpiperazine and mix evenly, then raise the temperature to 80°C, and dissolve 12g of 37% formaldehyde solution was added dropwise, and after 6 hours of reaction, the temperature was raised to 120°C to collect excess water in the water separator to obtain a Mannich base curing agent.

Embodiment 3

[0021] In the first step, the Korean pine bark is sun-dried and crushed and sieved through a 40-mesh sieve to obtain the bark powder. After mixing the bark powder and ethylenediamine in a weight ratio of 1:15, keep the temperature at 95°C for 3 hours, and filter The residue, the liquid is spray dried to obtain the bark extract.

[0022] In the second step, 90g of bark extract, 900g of epichlorohydrin, 900g of 1,4-dioxane and 12.5mL of tetrabutylammonium hydroxide were added in a three-necked flask equipped with a mechanical stirring paddle, a thermometer and a reflux condenser, After raising the temperature to 60°C, fully stir for 7 hours, then lower the temperature to 60°C, add 40g of sodium hydroxide and 1g of calcium oxide, and stir for 5 hours, add 500mL of acetone to the mixture to dilute, then filter to remove solid salt, then add acetone and excess epoxy chlorine After the propane is recovered by distillation under reduced pressure, a kind of bark powder source epoxy co...

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Abstract

The invention relates to an epoxy curing agent taking bark as a raw material and a preparation method thereof. The method comprises the following steps: crushing bark, adopting a 40-mesh sieve for sieving and then mixing with alkali, keeping temperature at 90 DEG C for 2-4 hours and then filtering residue, performing spray-drying treatment on the liquid and then acquiring a bark extract; performing Mannich condensation reaction on the bark extract, formaldehyde and polyamine, thereby acquiring a Mannich base curing agent; or enabling maleic anhydride to react with an epoxy compound which is prepared from the reaction of the bark extract and the epoxy chloropropane, thereby acquiring an acidic curing agent; or enabling polyamine to react with the epoxy compound which is prepared from the reaction of the bark extract and the epoxy chloropropane, thereby acquiring an amine curing agent. Natural renewable resource bark is selected as the raw material for preparing the epoxy curing agent product, the promotion of the high additional value utilization of the green renewable agriculture and forestry resources is benefited and the epoxy curing agent meets the requirements of green, environment-friendly and sustainable development.

Description

technical field [0001] The invention belongs to the field of epoxy curing agents, in particular to an epoxy curing agent using bark as a raw material and a preparation method thereof. Background technique [0002] Epoxy resin is a kind of thermosetting material widely used in national production and life. However, epoxy resin itself is a kind of thermoplastic resin material. Since its molecular structure is linearly distributed, the solid resin will soften and melt after heating, and the viscosity of liquid resin will decrease when heated. Therefore, in practical applications, Pure epoxy resin has no great practical value. Only after adding curing agent and other modified components to form a high polymer material with a three-dimensional network structure can a series of excellent physical and mechanical properties be obtained. [0003] Currently commonly used epoxy resin curing agents are mainly divided into two categories, including obvious curing agents and latent curin...

Claims

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Application Information

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IPC IPC(8): C08G59/40C08G59/62C08G59/64C08G59/42C08G59/50
CPCC08G59/40C08G59/42C08G59/50C08G59/62C08G59/64
Inventor 李梅夏建陵李守海丁海阳杨小华张燕
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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