Macromolecular polymerizable photoinitiator and preparation thereof

A technology for polymerizing photoinitiators and photoinitiators is applied in the field of preparation of macromolecular photoinitiators. Simple steps and operating conditions

Inactive Publication Date: 2012-07-18
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Benzophenone photoinitiator is the most widely used free radical type photoinitiator, but its ultraviolet absorption is low, and initiation effect is poor (R.Liska, Journal of Polymer Science PartA: polymer chemistry, 2002 (40) :1504-1518)
[0005] The above metho

Method used

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  • Macromolecular polymerizable photoinitiator and preparation thereof
  • Macromolecular polymerizable photoinitiator and preparation thereof
  • Macromolecular polymerizable photoinitiator and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Synthesis of Hydrogen-Substituted Macromolecular Polymerizable Photoinitiators

[0024] Add 10g of 4-hydroxybenzophenone and 4.5g of formaldehyde solution into a three-necked flask, add 0.44g of sodium hydroxide, heat and stir to 95°C, and react for 2h; After the end, cool to 105°C to collect the product, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. The obtained light yellow macromolecular photoinitiator containing benzophenone is dissolved in 21.2g methylene chloride, 0.4g boron trifluoride is added, 5.6g epichlorohydrin is dissolved in 11g methylene chloride, within 3 hours Slowly add the mixed solution dropwise to the three-necked flask, the reaction temperature is 0-5°C, after the dropwise addition, stir at 70°C for 3 hours, use a rotary evaporator to remove unreacted epichlorohydrin and dichloromethane from the mixed solution; use 40g ethanol Dissolve the resid...

Embodiment 2

[0028] Synthesis of Methyl Substituted Macromolecular Polymerizable Photoinitiators

[0029] Add 10g of 4-hydroxybenzophenone and 4.5g of formaldehyde solution into a three-necked flask, add 0.44g of sodium hydroxide, heat and stir to 95°C, and react for 2h; After the end, cool to 105°C to collect the product, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. The obtained light yellow macromolecular photoinitiator containing benzophenone is dissolved in 22g of methylene chloride, 0.4g of boron trifluoride is added, 5.6g of epichlorohydrin is dissolved in 13g of methylene chloride, slowly within 3 hours Add the mixed solution dropwise to the three-necked flask, the reaction temperature is 0-5°C, after the dropwise addition, stir at 70°C for 3 hours, use a rotary evaporator to remove unreacted epichlorohydrin and dichloromethane from the mixed solution; use 40g of ethanol to disso...

Embodiment 3

[0033] Synthesis of Methoxyl Substituted Macromolecular Polymerizable Photoinitiators

[0034]Add 10g of 4-hydroxybenzophenone and 4.6g of formaldehyde solution into a three-necked flask, add 0.5g of sodium hydroxide, heat and stir to 95°C, and react for 2h; After the end, cool to 105°C to collect the product, pour the product into water to precipitate, and obtain a light yellow macromolecular photoinitiator containing benzophenone after suction filtration. The obtained pale yellow macromolecular photoinitiator containing benzophenone is dissolved in 21g of methylene chloride, 0.4g of boron trifluoride is added, 5.6g of epichlorohydrin is dissolved in 15g of methylene chloride, slowly within 3 hours Add the mixed solution dropwise to the three-necked flask, the reaction temperature is 0-5°C, after the dropwise addition, stir at 70°C for 3 hours, use a rotary evaporator to remove unreacted epichlorohydrin and dichloromethane from the mixed solution; use 40g of ethanol to dissol...

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Abstract

The invention discloses a macromolecular polymerizable photoinitiator and a preparation thereof. The method comprises the following steps of: adding 4-hydroxybenzophenone and methanal to a three-necked flask, heating to 95 DEG C, reacting for 2 hours, heating to 150DEG C, leaching under at reduced pressure for 20 minutes, cooling to 105 DEG C, collecting products, pouring products into water, leaching to obtain a macromolecular photoinitiator, dissolving the macromolecular photoinitiator in an organic solvent, dissolving epoxy chloropropane in the solvent under catalysis of boron trifluoride,dropwise adding mixed liquid, reacting at a temperature of 0-5 DEG C, then stirring for 3 hours at a temperature of 70 DEG C, removing epoxy chloropropane and solvent, dissolving residues with a solvent, adding alkali and reacting for 0.5 hour at a temperature of 40 DEG C, removing salt and the solvent, re-dissolving residues with a solvent, washing with water and drying, adding crylic acid, p-hydroxyanisole and tetrabutylammonium bromide, heating for reacting for 6 hours, and then removing the solvent so as to obtain macromolecular polymerizable photoinitiator. The macromolecular polymerizable photoinitiator prepared by the method has the advantages of large molecular weight, weak mobility and good polymerizability.

Description

technical field [0001] The invention belongs to the field of photosensitive molecular materials, and in particular relates to a preparation method of a polymerizable macromolecular photoinitiator containing benzophenone. Background technique [0002] Light (ultraviolet or visible light) is irradiated on light-sensitive compounds, causing a series of photophysical and photochemical reactions to generate active fragments, which in turn trigger the polymerization of liquid oligomers (including monomers), and finally The process in which the liquid coating is instantly transformed into a solid polymer material is called photopolymerization (also known as photocuring). With the continuous development of science and technology and the increasing emphasis on environmental protection, photopolymerization technology has developed rapidly. Photopolymerization technology has practical application value in the fields of coatings, inks, adhesives, microelectronics, dental restoration and...

Claims

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Application Information

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IPC IPC(8): C08F2/48C08G8/36C08G8/30C08G8/08
Inventor 马贵平聂俊姜苹路健
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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