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Aqueous macromolecular photoinitiator and preparation method thereof

A photoinitiator and macromolecular technology, applied in the field of water-based macromolecular photoinitiator and its synthesis, to achieve good photoinitiation efficiency, reduce production costs, and increase content

Inactive Publication Date: 2010-06-16
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Utilize dimethylolpropionic acid to introduce carboxylic acid groups in the side chain of the resin, and then obtain hydrophilicity through neutralization and salt formation; but no small molecule photoinitiator 2-hydroxyl-1-{4-[4-(2 -Hydroxy-2-methyl-propionyl)-benzyl]-phenyl}-2-methyl-propane as a functional monomer, a report on the preparation of water-based macromolecular photoinitiators by chain extension
In addition, in water-based polyurethane, carboxyl groups are usually used as hydrophilic groups, and alkali is added to neutralize the resin to make the resin hydrophilic. However, it has not been seen that after introducing carboxylic acid groups into the resin, the method of chain extension is used to introduce sulfonic acid groups. Add alkali to neutralize, thus prepare the relevant report of a kind of dianionic waterborne macromolecular photoinitiator

Method used

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  • Aqueous macromolecular photoinitiator and preparation method thereof
  • Aqueous macromolecular photoinitiator and preparation method thereof
  • Aqueous macromolecular photoinitiator and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Example 1: Add 8.50 g of 2-hydroxyl-1-{4-[4-(2-hydroxyl-2-methyl-propionyl)-benzyl to a three-necked flask equipped with a thermometer, reflux condenser, and mechanical stirring ]-phenyl}-2-methyl-propane, 23.31g isophorone diisocyanate and 20.00ml acetone, in the 2 Under conditions, 80°C, react for 3 hours; then add 2.92g dimethylol propionic acid, gradually cool down to 75°C, react for 2 hours, add 21.60g polypropylene glycol, 1.34g ethylene glycol, gradually heat up to 80°C, react When the isocyanate group reaches the theoretical value, cool down to 50°C, add 2.20g of triethylamine, neutralize, and set aside; add 0.87g of 4-aminobenzenesulfonic acid to another three-necked flask equipped with a thermometer, reflux condenser, and mechanical stirring , 100g deionized water, heated to 70°C, added prepolymer, reacted until the isocyanate group disappeared completely, added triethylamine to neutralize, adjusted PH=8~9, distilled off acetone, and obtained a water-based sol...

Embodiment 2

[0035] Embodiment two: add 8.50g 2-hydroxyl-1-{4-[4-(2-hydroxyl-2-methyl-propionyl)-benzyl to a three-necked flask equipped with a thermometer, a reflux condenser, and mechanical stirring ]-phenyl}-2-methyl-propane, 18.27g toluene diisocyanate and 20.00ml acetone, in general N 2 Under the conditions, 80°C, react for 3 hours; then add 3.75g dimethylol propionic acid, gradually cool down to 75°C, react for 2 hours, add 18.50g polypropylene glycol, 1.92g neopentyl glycol, gradually heat up to 80°C, React until the isocyanate group reaches the theoretical value, lower the temperature to 50°C, add 2.83g of triethylamine, neutralize, and set aside; add 0.87g of 4-aminobenzenesulfonate to another three-necked flask equipped with a thermometer, reflux condenser, and mechanical stirring Acid, 100g deionized water, heated to 70°C, added prepolymer, reacted until the isocyanate group disappeared completely, added triethylamine to neutralize, adjusted PH=8~9, distilled off acetone to obta...

Embodiment 3

[0036] Embodiment three: add 8.50g 2-hydroxyl-1-{4-[4-(2-hydroxyl-2-methyl-propionyl)-benzyl in a three-necked flask equipped with a thermometer, a reflux condenser, and mechanical stirring ]-phenyl}-2-methyl-propane, 17.01g of hexamethylene diisocyanate and 20.00ml of acetone, in general N 2Under the condition of 80°C, react for 3 hours; then add 3.11g of dimethylolpropionic acid, gradually cool down to 75°C, react for 2 hours, add 20.90g of polypropylene glycol, 1.59g of 1,3-propanediol, and gradually heat up to 80°C, React until the isocyanate group reaches the theoretical value, lower the temperature to 50°C, add 2.34g of triethylamine, neutralize, and set aside; add 0.87g of 4-aminobenzenesulfonate to another three-necked flask equipped with a thermometer, reflux condenser, and mechanical stirring Acid, 100g deionized water, heated to 70°C, added prepolymer, reacted until the isocyanate group disappeared completely, added triethylamine to neutralize, adjusted PH=8~9, dist...

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Abstract

The invention relates to an aqueous macromolecular photoinitiator and a preparation method thereof. The general formula of the aqueous macromolecular photoinitiator is (i). The aqueous macromolecular photoinitiator prepared by the method has the photoinitiating efficiency equivalent to a corresponding micro-molecular photoinitiator and has better compatibility with an aqueous light-cured resin; carboxylate ions and sulfosalt ions exist in a molecular chain simultaneously, so the resin has better water solubility than an aqueous macromolecular photoinitiator only containing carboxylate ions; and in addition, the price of an introduced chain extender (4-aminobenzenesulfonic acid) used for sulfonic acid group is lower than that of a conventional aqueous functional monomer (dihydromethylpropionic acid), so that the cost of products is reduced and the industrial production is facilitated. At the same time, in the method, the chain is extended by using the functional monomer with photoinitiating function, so the content of photoinitiating radicals in the resin per gram is improved and the aqueous macromolecular photoinitiator has better photoinitiating efficiency than the aqueous macromolecular photoinitiator taking end radicals as the photoinitiating radicals.

Description

technical field [0001] The invention relates to a water-based macromolecular photoinitiator and a synthesis method thereof. Background technique [0002] One of the directions for the development of coatings in the 21st century is environmentally friendly coatings, which include high-solids and solvent-free coatings, water-based coatings, powder coatings and radiation-cured coatings. Water-based light-curing coating is a new type of environmentally friendly coating that uses water as a dispersion medium on the basis of inheriting and carrying forward the advantages of traditional light-curing technology. [0003] In the water-based photo-curing system, the photoinitiator is one of the most important components. At present, the traditional oil-based small molecule photo-initiator has been widely used in the water-based photo-curing system, but its many disadvantages also affect the water-based photo-curing system. Final properties of the cured system. Compared with oil-solu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08G18/67C08G18/38C08G18/34C08G18/32C08G18/12
Inventor 胡和丰俞鸣明王宇程齐利万梅陈学春龚德昌孙鑫李瀚文施丁豪何婷
Owner SHANGHAI UNIV
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