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Ultraviolet-curing hyperbranched polyester polyurethane acrylate resin and preparation method thereof

A technology of urethane acrylate and hyperbranched polyester, applied in the direction of polyurea/polyurethane coatings, coatings, etc., can solve the problems of inability to perform UV curing and do not contain photocurable groups, and achieve excellent solubility and simple raw materials. Ease of availability and reduced dosage

Inactive Publication Date: 2017-10-20
徐州佑季化工材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing hyperbranched polyesters do not contain photocurable groups and cannot be cured by ultraviolet light.

Method used

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  • Ultraviolet-curing hyperbranched polyester polyurethane acrylate resin and preparation method thereof
  • Ultraviolet-curing hyperbranched polyester polyurethane acrylate resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) At room temperature, add 1.2mol isophorone diisocyanate (IPDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl-p-cresol into a dry reaction flask, Add 1.2 mol polycaprolactone acrylate (CA) dropwise under stirring for 1 hour. After the addition, the temperature is raised to 35°C, and the reaction is until the measured -NCO value reaches half of the initial reaction time. Semi-blocked isocyanate IPDI-CA monomer, the synthesis route is as follows figure 1 Shown

[0026] (2) In the reaction flask of step (1), add 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl-p-cresol, and add each hyperbranched molecule dropwise while stirring A mixture of hydroxyl-terminated hyperbranched polyester with a hydroxyl number of 8 and tetrahydrofuran (the amount of tetrahydrofuran is based on the total dissolved hyperbranched polyester), the dripping time is 1 hour, and the heat preservation reaction is completed for 1 hour; then the temperature is slowly raised to 40 ~50℃, ...

Embodiment 2

[0028] (1) At room temperature, add 1.1mol hexamethylene diisocyanate (HDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl-p-cresol into a dry reaction flask, Add 1.0 mol polycaprolactone acrylate (CA) dropwise under stirring for 0.5 hours. After the dropwise addition, the temperature is raised to 45°C, and the reaction is completed until the measured -NCO value reaches half of the initial reaction time. Semi-blocked isocyanate HDI-CA monomer;

[0029] (2) In the reaction flask of step (1), add dropwise a mixture of hydroxyl-terminated hyperbranched polyester with 8 hydroxyl groups on each hyperbranched molecule and tetrahydrofuran under stirring. The dropping time is 1 hour. After holding the reaction for 2 hours; then slowly raising the temperature to 50-60°C and stirring the reaction for 2 hours; then raising the temperature to 70-80°C, stirring the reaction until the measured -NCO value reaches the theoretical value; after removing the solvent tetrahydrofuran under r...

Embodiment 3

[0031] (1) At room temperature, add 1.5mol isophorone diisocyanate (IPDI), 0.05wt% dibutyltin dilaurate, 0.2wt% 2,6-di-tert-butyl-p-cresol into a dry reaction flask, Under stirring, add 1.5 mol of hydroxyethyl acrylate (HEA) dropwise for 1.5 hours. After the addition, the temperature is raised to 40°C, and the reaction is completed until the measured -NCO value reaches half of the initial reaction time, and a semi-sealed is obtained. Terminated isocyanate IPDI-HEA monomer;

[0032] (2) In the reaction flask of step (1), add dropwise a mixture of hydroxyl-terminated hyperbranched polyester with 8 hydroxyl groups on each hyperbranched molecule and tetrahydrofuran under stirring. The dripping time is 2 hours. After completion of the insulation reaction for 4 hours; then slowly increase the temperature to 60-70°C and stir the reaction for 4 hours; then increase the temperature to 80-90°C and stir the reaction until the measured -NCO value reaches the theoretical value; after removing...

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Abstract

The invention discloses a preparation method of ultraviolet-curing hyperbranched polyester polyurethane acrylate resin, which comprises the steps of (1) adding diisocyanate, a catalyst and a polymerization inhibitor to a reaction flask at a room temperature, dropwise adding monohydroxyl-terminated acrylate while stirring, performing temperature rise to be 40-50 DEG C, and performing a reaction until a measured NCO value reaches one half during reaction start to form a semi-blocked isocyanate monomer, and (2) keeping a stirring state and dropwise adding hyperbranched polyester and tetrahydrofuran mixed liquid to the reaction flask in Step (1), performing a thermal insulation reaction for 1-8h, performing slow temperature rise to be 40-90 DEG C, performing a stirring reaction for 1-6h, performing temperature rise to be 60-100 DEG C, performing a stirring reaction until the measured NCO value reaches a theoretical value, and removing a solvent. The invention further discloses the ultraviolet-curing hyperbranched polyester polyurethane acrylate resin prepared by the method. The method is simple to operate; raw materials are easy to obtain; and the prepared resin is good in wear resistance and high in curing rate.

Description

Technical field [0001] The invention belongs to the technical field of light curing resins, and specifically relates to an ultraviolet light curing hyperbranched polyester polyurethane acrylate resin and a preparation method thereof. Background technique [0002] UV curing means that under the irradiation of UV light, the photoinitiator generates free radicals or cations, which initiates the polymerization of compounds (polymers, prepolymers and monomers) with unsaturated double bonds or epoxy groups in the system , So that the system changes from liquid to solid in a short time. It is a green curing technology that has developed rapidly since 1960. Compared with traditional curing methods, it has the advantages of 5E, namely Economical, Environmentally Friendly, Efficient, Energy Saving, and Widely Adaptable (Enabling). [0003] Hyperbranched polymers are macromolecules with highly branched structures, which have the advantages of high functionality, no entanglement in and betwe...

Claims

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Application Information

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IPC IPC(8): C08G18/75C08G18/73C08G18/76C08G18/68C08G18/67C08G18/42C08G18/10C09D175/14
CPCC08G18/755C08G18/10C08G18/672C08G18/68C08G18/73C08G18/7614C08G18/7671C09D175/14C08G18/42
Inventor 余立挺王贵富张弢杜鹏张绳延
Owner 徐州佑季化工材料有限公司
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