Photosensitive fluorosilicone segmented urethane acrylate oligomer and preparation method thereof
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A polyurethane acrylate and fluorosilicone block technology, which is applied in leather surface treatment, coating, animal husbandry, etc.
Active Publication Date: 2013-03-27
BEIJING UNIV OF CHEM TECH +1
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Problems solved by technology
[0006] The technical problem to be solved by the present invention is to prepare a photosensitive fluorosilicon block urethane acrylate oligomer that can be cured under ultraviolet light irradiation, and improve the high temperature resistance and low temperature folding resistance of the oligomer by introducing organic silicon segments , flexibility; reduce the surface energy of oligomers by introducing organic fluorine segments, and improve their waterproof, oil-proof, stain-resistant and chemical-resistant properties; through the application of ultraviolet curing technology, environmental pollution caused by organic solvents can be improved. , to meet the needs of production and life
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Embodiment 1
[0120] Synthesis of N,N-dihydroxyethyl-3-alanine hexafluorobutyl acrylate, adding hexafluorobutyl acrylate in equal amount to a four-necked flask equipped with a condenser tube, a thermometer, a magnetic stirrer and a dropping funnel 10.00g and diethanolamine 4.45g, 5.00g methanol as solvent. mixture at room temperature and pass N 2 After stirring for 20 minutes under certain conditions, the temperature was raised to 40°C for 5 hours, and then distilled under reduced pressure to remove methanol to obtain light yellow and transparent N, N-dihydroxyethyl-3-aminopropionic acid hexafluorobutyl ester, the reaction formula is as follows:
[0121]
Embodiment 2
[0123] The synthesis of N,N-dihydroxyethyl-3-aminomethyl propionate dodecafluoroheptyl ester, add the same amount of methyl alcohol into a four-necked flask equipped with a condenser tube, a thermometer, a magnetic stirrer and a dropping funnel 10.00 g of dodecafluoroheptyl acrylate, 2.63 g of diethanolamine, and 3.00 g of methanol were used as solvents. mixture at room temperature and pass N 2 After stirring for 20 minutes under certain conditions, the temperature was raised to 40 ° C for 6 hours, and then distilled under reduced pressure to remove methanol to obtain light yellow transparent N, N-dihydroxyethyl-3-aminomethyl propionate hexafluorobutyl ester, the reaction formula is as follows :
[0124]
Embodiment 3
[0126] In a 100mL four-neck flask equipped with a stirrer, dropping funnel, condenser and thermometer, add 15.00g of Q4-3667, 0.03g of catalyst dibutyltin dilaurate (DBTDL), and dropwise add 4.17g of isophorone Diisocyanate (IPDI), react at 45°C, use the di-n-butylamine-acetone method to measure the isocyanate content, monitor the progress of the reaction, when the reaction reaches 50% of the initial value of the isocyanate, add 5.89gN,N -Dihydroxyethyl-3-aminopropionic acid hexafluorobutyl monomer, react at 45°C until the NCO value is 0; then add 4.17g of isophorone diisocyanate (IPDI), and wait for the NCO to react by 50% , then add 2.18g of hydroxyethyl acrylate (HEA) and 0.03g of inhibitor p-methoxyphenol, react until the NCO content is 0 to finish the reaction, and obtain the photosensitive fluorosilicone block polyurethane acrylate oligomer, react The formula is as follows:
[0127]
[0128] Wherein the infrared spectrogram of final product sees appendix figure 1 , ...
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Abstract
The invention relates to a photosensitive fluorosilicone segmented urethane acrylate oligomer and a preparation method of the photosensitive fluorosilicone segmented urethane acrylate oligomer. The preparation method comprises the steps of: (1) adding a fluorinated acrylate monomer and dialkylol amine into a reactor for reaction for 2-6hours at 20-50 DEG C; (2) adding organic silicon, polyisocyanate and a catalyst into the reactor for reaction for 0.25-2hours at 30-60 DEG C; (3) adding a second step product, a first step product, polyisocyanate and the catalyst into the reactor for reaction for 0.25-1hour at 30-60 DEG C; (4) carrying out reaction of a third step product, olefine acid-hydroxyl ester compounds, a polymerization inhibitor and the catalyst for 2-6hours at 30-80 DEG C; and (5) reducing the temperature and cooling to room temperature, discharging, and keeping in a dark place for later use. The invention has the beneficial effects that (1) the synthesized oligomer has the characteristics of better photosensitiveness, high and low temperature resistance, chemical medium resistance, resistance to pollution, flexibility and the like; (2) a ultraviolet cured leather finishing agent prepared by the oligomer has better adhesive force and low temperature hard fold resistance, does not contain organic solvents, is pollution-free and belongs to an environment-friendly material; and (3) the oligomer is simple in synthetic method, mild in reaction condition and easy to operate.
Description
technical field [0001] The invention relates to a photosensitive fluorosilicone block polyurethane acrylate oligomer and a preparation method thereof. This photosensitive fluorosilicone block urethane acrylate oligomer has the characteristics of low surface energy, low viscosity, no organic solvent, fast UV curing speed, excellent low temperature folding resistance, chemical medium resistance and adhesion, and is especially suitable for As a finishing agent for leather or artificial leather. It belongs to the field of fine chemical technology. Background technique [0002] Leather finishing agent is a leather auxiliary agent used to protect and beautify leather on the surface of leather. It is composed of film-forming substances, colorants, auxiliary agents and solvents in a certain proportion. Among them, the film-forming substances are the main body of leather finishing agents. Leather finishing agents play a very important role in the leather manufacturing industry. The...
Claims
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