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Preparation method of urushiol acrylate photo-cured membrane

A urushiol acrylate and photocuring technology, which is applied in the direction of natural resin coatings, coatings, etc., to achieve the effect of simple process, wide application, and good thermal stability

Active Publication Date: 2018-03-09
NANJING ZHONGSEN BIOLOGICAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are few reports on the use of urushiol to prepare photocurable resins, and UV-curable coatings have the characteristics of high efficiency, energy saving, and environmental protection, and have occupied more and more market shares. Therefore, the preparation of UV-curable coatings Urushiol acrylate coatings have huge social and economic benefits [Wei Jie, Light Curing Coatings, 2013: 1-4.]

Method used

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  • Preparation method of urushiol acrylate photo-cured membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The first step: the purification of urushiol

[0029] Take a certain amount of raw lacquer, filter it with gauze to remove mechanical impurities in the raw lacquer, then add a certain amount of absolute ethanol, stir, let stand, filter, wash, repeat 3 times, combine the filtrate, concentrate in vacuum at 60 ° C, the concentrate is The crude urushiol extract, and repeated extraction of the crude urushiol extract with petroleum ether for 3 times, standing still, separating, combining the extracts, concentrating in vacuo at 60°C, recovering the solvent, and obtaining urushiol with a purity of more than 95%;

[0030] The second step, esterification reaction

[0031] Add urushiol, triethylamine with 2 times the moles of urushiol, and dichloromethane with 200% urushiol mass in the reactor, control the temperature at 0°C, slowly add acryloyl chloride with 2.5 times the moles of urushiol, and keep the temperature low Reaction time 2h.

[0032] The third step, sample purificat...

Embodiment 2

[0039] The first step: the purification of urushiol

[0040] Take a certain amount of raw lacquer, filter it with gauze to remove mechanical impurities in the raw lacquer, then add a certain amount of absolute ethanol, stir, let stand, filter, wash, repeat 4 times, combine the filtrate, and concentrate in vacuum at 60 ° C, the concentrate is The crude urushiol extract, and repeated extraction of the crude urushiol extract with petroleum ether for 3 times, standing still, separating, combining the extracts, concentrating in vacuo at 60°C, recovering the solvent, and obtaining urushiol with a purity of more than 95%;

[0041] The second step, esterification reaction

[0042] Add urushiol, pyridine with 3 times the moles of urushiol, and tetrahydrofuran with 300% urushiol mass into the reactor, control the temperature at -1°C, slowly add acryloyl chloride with 2.5 times the moles of urushiol, and keep the low temperature for 3 hours .

[0043] The third step, sample purificatio...

Embodiment 3

[0050] The first step: the purification of urushiol

[0051] Take a certain amount of raw lacquer, filter it with gauze to remove mechanical impurities in the raw lacquer, then add a certain amount of absolute ethanol, stir, let stand, filter, wash, repeat 4 times, combine the filtrate, and concentrate in vacuum at 60 ° C, the concentrate is The crude urushiol extract, and repeated extraction of the crude urushiol extract with petroleum ether for 3 times, standing still, separating, combining the extracts, concentrating in vacuo at 60°C, recovering the solvent, and obtaining urushiol with a purity of more than 95%;

[0052] The second step, esterification reaction

[0053] Add urushiol, triethylamine with 4 times the moles of urushiol, and toluene with 250% urushiol mass into the reactor, control the temperature at 1°C, slowly add methacryloyl chloride with 2.0 times the moles of urushiol, and keep the temperature low Reaction time 3h.

[0054] The third step, sample purific...

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Abstract

The invention relates to a preparation method of an urushiol acrylate photo-cured membrane. The preparation method includes: simultaneously adding urushiol, an acid-binding agent and a solvent 1 intoa reactor, stirring in a temperature-controlled manner, dropwise adding acyl chloride and performing continuous reaction when the temperature lowers to a certain value, filtering reactants, performingpressure-reducing rotary evaporation to remove the solvent, adding a solvent 2 to perform precipitation, filtering, adding a polymerization inhibitor, and performing pressure-reducing rotary evaporation to obtain urushiol acrylate ultraviolet-curable resin monomers; taking a certain amount of urushiol acrylate, adding a photo-initiator, evenly stirring, using an applicator to coat a glass sheet or a tinplate sheet with the mixture, and curing under an ultraviolet lamp to obtain the urushiol acrylate photo-cured membrane. The preparation method has the advantages that the method is simple, theproduct can be fast cured by ultraviolet curing, application of urushiol derivatives in photo-curable resin can be expanded favorably, the urushiol derivatives can be mixed with various unsaturated photo-curable resin to produce membranes through curing, and the prepared membrane is good in adhesive force, impact resistance and toughness.

Description

technical field [0001] The invention belongs to the field of light-cured coatings, in particular to a preparation method of urushiol acrylate light-cured film. Background technique [0002] Raw lacquer is the secretion of lacquer tree. It is a water-in-oil emulsion. Its main components are 60%-70% urushiol, 20%-30% water, and a small amount of laccase and polysaccharides. Urushiol, the main film-forming substance of raw lacquer, is a derivative of catechol structure, and its side chain is straight-chain hydrocarbons. In addition to saturated alkanes, there are also monoenes, dienes, and trienes. and other structures. The raw lacquer that has just been harvested is milky white, and it is easily oxidized and turns brown or even black after contact with air. Continue to contact with the air, under the conditions of suitable temperature (20°C-30°C) and humidity (80%-90%), the raw lacquer can continuously absorb oxygen, oxidize, cross-link, and finally solidify into a film. The...

Claims

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Application Information

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IPC IPC(8): C09D193/00
CPCC09D193/00
Inventor 王成章方传杰周昊
Owner NANJING ZHONGSEN BIOLOGICAL TECH CO LTD