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Polyurethane acrylate oligomer and preparation method thereof

A technology of urethane acrylate and hydroxy acrylate, applied in the field of urethane acrylate and its preparation, can solve the problems of high volume shrinkage, low volume shrinkage, poor adhesion, etc., and achieve the effect of excellent application performance

Active Publication Date: 2014-11-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the field of photocuring, one of the biggest disadvantages is its large volume shrinkage, which leads to poor adhesion and limits the application of photocuring technology. Therefore, it is of great significance to synthesize polyurethane acrylate with low volume shrinkage.

Method used

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  • Polyurethane acrylate oligomer and preparation method thereof
  • Polyurethane acrylate oligomer and preparation method thereof
  • Polyurethane acrylate oligomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) In a four-necked flask equipped with a mechanical stirring paddle, a thermometer, a condenser and a constant pressure funnel, add 20g of isophorone diisocyanate (IPDI), 0.0398g of catalyst dibutyltin dilaurate (DBTDL), 0.0284g Inhibitor p-hydroxyanisole (MEHQ), diluent 1,6-hexanediol diacrylate (HDDA11.36g), stir evenly, and control the temperature at 40°C. 16.22 g of polycaprolactone ring-opening trihydric alcohol, whose number-average molecular weight Mn=540 g / mol, was added dropwise through a constant pressure funnel, stirred evenly, and heated to 50° C. to continue the reaction. Through infrared monitoring, the wave number on the spectrum is 3200 -1 -3600cm -1 The interval is differentiated. Before the end of the reaction, there are two peaks of amino group and hydroxyl group. After the reaction, only one peak of amino group remains. When the interval changes from two peaks to one peak, the reaction of this step ends.

[0039](2) Lower the temperature to 40°C,...

Embodiment 2

[0051] (1) Add 20g of IPDI, 0.0440g of catalyst DBTDL, 0.0314g of inhibitor MEHQ, and diluent TPGDA12.5585g into a four-necked flask equipped with a mechanical stirring paddle, a thermometer, a condenser and a constant pressure funnel, and stir Evenly, and the temperature is controlled at 40°C. 16.22 g of polycaprolactone ring-opening trihydric alcohol was added dropwise through a constant pressure funnel, stirred evenly, and the temperature was raised to 50° C. to continue the reaction. The end point of this step reaction was determined by the di-n-butylamine method, and when the remaining -NCO was 50%, the step reaction ended.

[0052] (2) Lower the temperature to 40°C, add HEA6.9670 dropwise with a dropping funnel, stir evenly after the dropwise addition, and raise the temperature to 70°C to continue the reaction. Through infrared monitoring, the end point of this step reaction was determined by the di-n-butylamine method. When the remaining -NCO was 17%, the step reaction...

Embodiment 3

[0056] (1) Add 20g of IPDI, 0.0471g of catalyst DBTDL, 0.0337g of inhibitor hydroquinone, and diluent HDDA13 into a four-neck flask equipped with a mechanical stirring paddle, a thermometer, a condenser and a constant pressure funnel. 46g, stir evenly, and control the temperature at 40°C. 16.22 g of polycaprolactone ring-opening trihydric alcohol was added dropwise through a constant pressure funnel, stirred evenly, and the temperature was raised to 50° C. to continue the reaction. Through infrared monitoring, the 3200 -1 -3600 -1 The interval is differentiated. When this interval changes from two peaks to one peak, the reaction of this step ends.

[0057] (2) Lower the temperature to 40°C, add 7.2808g of cetyl alcohol in batches, stir evenly after the addition, and raise the temperature to 70°C to continue the reaction. Through infrared monitoring, the 3200 -1 -3600 -1 The interval is differentiated. When this interval changes from two peaks to one peak, the reaction of ...

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Abstract

The invention relates to polyurethane acrylate and a preparation method of polyurethane acrylate. The oligomer is prepared by reacting polyol, diisocyanate, acrylate or hydroxy methacrylate and chain-type saturated fatty alcohol; the solidified film of the oligomer has excellent performance, and has the characteristics of low volume shrinkage, high adhesion, high hardness, good flexibility, solvent resistance and the like; and furthermore, research finds that the volume shrinkage of a light polymerization system is lower and lower and the adhesion is higher and higher along with the increase of the chain length of the introduced chain-type saturated fatty alcohol. Polyurethane acrylate has the advantages that the synthesizing raw materials are wide in sources and low in price, is suitable for industrial production, and has great industrial application value when used as main rein of UV (ultraviolet) paint or UV printing ink.

Description

technical field [0001] The invention relates to a polyurethane acrylate and a preparation method thereof, belonging to the field of photocurable oligomers. Background technique [0002] Photocuring technology is a process in which light is used as an energy source to trigger a rapid transformation of a photoreactive liquid substance into a solid state. As an energy-saving and environment-friendly new technology, it has the advantages of high efficiency, economy, energy saving, wide adaptability and environmental friendliness. [0003] The photocuring system is mainly composed of oligomers, reactive diluents and photoinitiators, among which the properties of oligomers determine the properties of the cured coating film, such as hardness, flexibility, volume shrinkage and adhesion. Urethane acrylate is an important light-curable oligomer, which is synthesized from polyisocyanate, long-chain diol and hydroxyl-functionalized acrylate through a two-step reaction. Since polyisocy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/67C08G18/42C08G18/30C08G18/10C07C271/24C07C271/12C07C271/28C07C269/02
Inventor 聂俊秦莉莉何勇
Owner BEIJING UNIV OF CHEM TECH