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Acylphosphine photoinitiator and preparation method thereof

A technology of photoinitiator and acylphosphine, which is applied in the field of acylphosphine photoinitiator and its preparation, to achieve the effects of mild reaction conditions, strong light absorption ability and enhanced matching

Active Publication Date: 2021-01-29
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to improve the initiating efficiency of TPO, a large number of documents have reported structural modification of TPO, but so far, research on structural modification of TPO has mainly focused on modifying the benzene ring structure in the benzoyl group (the right side in formula V frame structure), the research on the modification of the benzene ring structure (the frame structure on the left side in formula V) in the phosphono group has not yet been reported

Method used

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  • Acylphosphine photoinitiator and preparation method thereof
  • Acylphosphine photoinitiator and preparation method thereof
  • Acylphosphine photoinitiator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] The structural formula of 2,4,6-trimethylbenzoyl-diphenylphosphine oxide (TPO) is as follows

[0053]

[0054] In a dry three-necked flask (50 ml) equipped with a magnetic stirrer, a thermometer, a reflux condenser, and a nitrogen gas conduit, feed dry nitrogen to remove the air in the three-necked flask. Put 17.4g of aluminum trichloride, 17.9g of phenylphosphine dichloride, and 11g of benzene into a three-necked flask in sequence, and slowly raise the temperature of the oil bath to the set temperature of 90°C, and keep the reaction for 12h. After the unreacted raw material was evaporated under reduced pressure, it was cooled to room temperature; the reaction liquid was slowly added dropwise to 100 g of ice-water mixture for hydrolysis, and the reaction was continued for 4 hours after the hydrolysis was completed. 120 g of toluene was put into the reaction solution for extraction, and the organic layer was washed with alkali and water to obtain a toluene solution of...

Embodiment 2

[0057] The structural formula of 2,4,6-trimethylbenzoyl-4-tolylphenylphosphine oxide (4-MTPO) is as follows:

[0058]

[0059] In a dry three-necked flask (50 ml) equipped with a magnetic stirrer, a thermometer, a reflux condenser, and a nitrogen gas conduit, feed dry nitrogen to remove the air in the three-necked flask. Put 17.4g of aluminum trichloride, 17.9g of phenylphosphine dichloride, and 12.9g of toluene into a three-necked flask in sequence, and slowly raise the temperature of the oil bath to the set temperature of 90°C, and keep the reaction for 12h. After the unreacted raw material was evaporated under reduced pressure, it was cooled to room temperature; the reaction liquid was slowly added dropwise to 100 g of ice-water mixture for hydrolysis, and the reaction was continued for 4 hours after the hydrolysis was completed. 120 g of toluene was put into the reaction solution for extraction, and the organic layer was washed with alkali and water to obtain a toluene ...

Embodiment 3

[0062] The structural formula of 2,4,6-trimethylbenzoyl-2,,4-xylylphenylphosphine oxide (2,4-DMTPO) is as follows:

[0063]

[0064] In a dry three-necked flask (50 ml) equipped with a magnetic stirrer, a thermometer, a reflux condenser, and a nitrogen gas conduit, feed dry nitrogen to remove the air in the three-necked flask. Put 17.4g of aluminum trichloride, 17.9g of phenylphosphine dichloride, and 14.9g of m-xylene into a three-necked flask in sequence, and slowly raise the temperature of the oil bath to the set temperature of 90°C, and keep the reaction for 12h. After the unreacted raw material was evaporated under reduced pressure, it was cooled to room temperature; the reaction liquid was slowly added dropwise to 100 g of ice-water mixture for hydrolysis, and the reaction was continued for 4 hours after the hydrolysis was completed. 120 g of toluene was put into the reaction solution for extraction, and the organic layer was washed with alkali and water to obtain a t...

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Abstract

The invention provides an acylphosphine photoinitiator of which the chemical structural formula is shown as a formula (I), and also provides a preparation method of the acylphosphine photoinitiator, which comprises the following steps: (1) putting aryl phosphine dichloride or derivatives thereof, aromatic hydrocarbon or derivatives thereof and a catalyst into a reaction flask to obtain a complex of diarylphosphine chloride and the catalyst; (2) slowly dropwise adding the mixture obtained in the step (1) into water, continuously reacting, adding an extraction agent for extraction, and separating out an organic layer for later use; (3) putting the obtained organic layer into the reaction flask, and putting aromatic aldehyde or derivatives thereof at 10-25 DEG C for reaction; and (4) adding acatalyst and an oxidant into the reaction solution obtained in the step (3) at a certain temperature to prepare the acylphosphine photoinitiator. The phenyl ring on the phosphonyl side in the acylphosphine initiator structure is subjected to structural modification for the first time, the reaction conditions are mild, the treatment process is simple, and the method is green and environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and application, and in particular relates to an acylphosphine photoinitiator and a preparation method thereof. Background technique [0002] Compared with traditional curing technology, light curing technology has the characteristics of high efficiency, energy saving, environmental protection, economy, and wide applicability. It is more and more used in the curing of coatings, inks, and adhesives. The photocuring system generally includes: a light source, a monomer and an initiator, wherein the matching of the wavelength of the light source and the initiator determines the quality of the curing formula. Compared with UV light initiation, near-UV light and visible light initiation are safer and more energy-saving. At the same time, long-wavelength light can be applied to the curing of thick coatings. One of the research hotspots in this field. [0003] 2,4,6-Trimethylbenzoyl-diphenylph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C07F9/53
CPCC08F2/48C07F9/5337
Inventor 段好东冷康威徐晓磊于青王忠卫孟雨婷黄伟侯计金庄春艳武军
Owner SHANDONG UNIV OF SCI & TECH
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