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Preparation method of self-emulsified water-based photoinitiator and water-based photoinitiator

A water-based photoinitiator, self-emulsifying technology, applied in the direction of coating, etc., can solve the problems such as the decline of the main resin performance, the low photoinitiation efficiency, the increase of the dosage, etc., to achieve good compatibility, reduce the amount of solvent, and facilitate the Emulsifying effect

Active Publication Date: 2018-05-04
深圳市嘉卓成科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has not yet been seen that polyisocyanate is the starting group, and after the introduction of hydrophilic groups, the photoinitiator 2-hydroxyl-methylphenylpropan-1-one is embedded to obtain branched multifunctional water-based macromolecular photoinitiators. to report
[0004] Water-based macromolecular initiators can overcome the shortcomings of small-molecule photoinitiators such as easy migration, odor and poor resin compatibility to a certain extent, but water-based long-chain macromolecules are prone to occur due to the low molar concentration of photoinitiator groups. The problem of low photoinitiation efficiency caused by the increase of its dosage increases the cost, and there will also be the problem of decreased performance of the main resin due to the increase of its dosage.

Method used

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  • Preparation method of self-emulsified water-based photoinitiator and water-based photoinitiator
  • Preparation method of self-emulsified water-based photoinitiator and water-based photoinitiator
  • Preparation method of self-emulsified water-based photoinitiator and water-based photoinitiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of preparation method of self-emulsifying type aqueous photoinitiator, comprises the steps:

[0025] S1. Add 15 grams of dimethylolpropionic acid and 18 grams of dimethylamide into a four-necked flask equipped with a thermometer, a reflux condenser, and a mechanical stirring rod, blow nitrogen gas, and heat up to 65°C. The acid dissolves completely;

[0026] S2, drop into the mixture of 21 grams of 1,6-hexamethylene diisocyanate trimer and 0.01 grams of dibutyltin dilaurate, the time of dropping is 1 hour, and the constant temperature reaction is 3 hours;

[0027] S3. Cool down to 45° C., drop in a mixture of 27 g of isophorone diisocyanate and 0.01 g of dibutyltin dilaurate, add the mixture for 0.5 hours, keep warm for 2 hours until the isocyanate group reaches the theoretical value;

[0028] S4. Heat up to 70°C, add 18.97 grams of 2-hydroxy-methylphenylpropan-1-one and 0.01 grams of dibutyltin dilaurate to react until the isocyanate group completely disappears...

Embodiment 2

[0032] A kind of preparation method of self-emulsifying type aqueous photoinitiator, comprises the steps:

[0033] S1. Add 17 grams of dimethylolpropionic acid and 17 grams of dimethylamide into a four-necked flask equipped with a thermometer, a reflux condenser, and a mechanical stirring rod, blow nitrogen, raise the temperature to 65°C, and dissolve the dimethylolpropionic acid The acid dissolves completely;

[0034] S2, drop in the mixture of 22.76 grams of 1,6-hexamethylene diisocyanate trimer and 0.08 grams of dibutyltin dilaurate, the dropping time is 0.5 hours, and the constant temperature reaction is 2 hours;

[0035] S3. Cool down to 45°C, drop in a mixture of 25 g of isophorone diisocyanate and 0.08 g of dibutyltin dilaurate, add the mixture for 1 hour, keep warm for 1.5 hours until the isocyanate group reaches the theoretical value;

[0036] S4. Heat up to 80°C, add 18 grams of 2-hydroxy-methylphenylpropan-1-one and 0.08 grams of dibutyltin dilaurate to react until...

Embodiment 3

[0040] A kind of preparation method of self-emulsifying type aqueous photoinitiator, comprises the steps:

[0041] S1. Add 18 grams of dimethylol propionic acid and 15 grams of N-methylpyrrolidone into a four-necked flask equipped with a thermometer, a reflux condenser, and a mechanical stirring rod, blow nitrogen, and heat up to 50°C. Propionic acid is completely dissolved;

[0042] S2, drop into the mixture of 27 grams of toluene diisocyanate trimer and 0.1 gram of dibutyltin dilaurate, the dropping time is 45 minutes, constant temperature reaction for 3 hours;

[0043] S3. Cool down to 40°C, add dropwise a mixture of 20.7 g of 2,4-toluene diisocyanate and 0.1 g of dibutyltin dilaurate, add the mixture for 1 hour, and keep warm for 2 hours until the isocyanate group reaches the theoretical value;

[0044] S4. Heat up to 75°C, add 19 grams of 2-hydroxy-methylphenylpropan-1-one and 0.1 grams of dibutyltin dilaurate to react until the isocyanate group completely disappears, and ...

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Abstract

The invention provides a preparation method of a self-emulsified water-based photoinitiator. The method comprises the following steps: S1, adding 15-18% of dimethylolpropionic acid and 15-18% of a solvent according to weight ratio into a reaction kettle, filling nitrogen for protecting, and dissolving dimethylolpropionic acid; S2, dropwise adding a mixed solution prepared from 21-27% of polyisocyanate and 0.01-0.12% of a catalyst according to weight ratio into the reaction kettle for reacting; S3, dropwise adding a mixed solution prepared from 20-27% of diisocyanate and 0.01-0.12% of a catalyst according to weight ratio for reacting; S4, dropwise adding a mixed solution prepared from 18-21% of 2-hydroxy-methyl phenyl propane-1-ketone and 0.01-0.12% of a catalyst according to weight ratio for reacting to obtain a semi-finished product photoinitiator A; S5, adding triethylamine into the semi-finished product photoinitiator A for neutralizing; and S6, adding deionized water, shearing anddispersing at high speed through an emulsifying machine to obtain the self-emulsified water-based photoinitiator. The coating film appearance, the hardness, the water boiling resistance and the relative mobility of the prepared self-emulsified water-based photoinitiator are superior to that of the conventional coating prepared from the small-molecular photoinitiator.

Description

technical field [0001] The invention relates to the field of polymer materials, in particular to a preparation method of a water-based photoinitiator for a water-based ultraviolet radiation curing coating and the water-based photoinitiator. technical background [0002] Since the beginning of the 21st century, as people have paid more and more attention to environmental protection issues, water-based light-curing coatings have the advantages of being environmentally friendly with water as the dispersion medium, basically no VOC emissions, and no monomer residues on the basis of inheriting the traditional light-curing technology. And favored by people. [0003] In the water-based photo-curing system, the photoinitiator is an important part. Although the traditional oil-based small molecule photo-initiator can be used in the water-based photo-curing system, it still has easy migration, odor, and compatibility with the system resin. Not good and many other disadvantages. Comp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/79C08G18/75C08G18/76C08G18/34C08G18/83C08F2/48C09D7/00
CPCC08F2/48C08G18/0823C08G18/348C08G18/721C08G18/755C08G18/7614C08G18/792C08G18/794C08G18/831C09D7/00
Inventor 吴小浩黄立标黄杰良
Owner 深圳市嘉卓成科技发展有限公司
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