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Method for preparing polymer type michler's ketone photoinitiator

A photoinitiator and polymer-based technology, applied in the field of photochemistry, can solve the problems of no significant improvement in initiation performance, limited application fields, and reduced initiation efficiency, and achieve the effects of improving photoinitiation efficiency, broad application prospects, and improving performance

Inactive Publication Date: 2010-07-28
SHANGHAI JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Commercially a large number of benzophenones used as high-efficiency photoinitiators have poor compatibility with the polymerization system and require the presence of co-initiator amines to initiate polymerization, which reduces the initiation efficiency and limits the application field.
Michlone is a derivative of benzophenone. Although it has introduced a co-initiator amine in its molecule, because it is connected to the benzene ring, the reactivity of the amine is low, and the initiation performance has not been significantly improved, and it is compatible with the polymerization system. Capacitance is still poor

Method used

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  • Method for preparing polymer type michler's ketone photoinitiator
  • Method for preparing polymer type michler's ketone photoinitiator
  • Method for preparing polymer type michler's ketone photoinitiator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] a) In a 100ml three-neck flask with magnetic stirring and nitrogen gas, add 0.02mol (4.36g) of 4,4'-difluorobenzophenone, 0.2mol (17.23g) of piperazine, 0.05mol (6.95g) in anhydrous potassium carbonate and 25ml dimethyl sulfoxide, reacted at 160°C in the dark for 50 hours, cooled to room temperature, then poured into 10 times the volume of water to obtain a yellow precipitate, filtered, and put the filter cake at 80°C Vacuum-dried to obtain 2.27 g of a small molecule photoinitiator 4,4'-dipiperazine benzophenone with a yield of 66%.

[0031] b) Add 2mmol (1.0492g) of polyoxyethylene glycidyl ether to 10ml of N,N-dimethylformamide to dissolve completely, and add 1.9mmol (0.6634g) of 4,4'-dipiperazine diphenyl under nitrogen protection Methanone was heated to 75° C. for 8 hours, cooled to room temperature, then poured into 10 times the volume of anhydrous ether, filtered, and the obtained solid was vacuum-dried to obtain 1.30 g of a polymer-type michroketone photoinitiato...

Embodiment 2

[0033] a) In a 100ml three-neck flask with magnetic stirring and nitrogen gas, add 0.02mol (4.36g) of 4,4'-difluorobenzophenone, 0.2mol (17.23g) of piperazine, 0.05mol (6.95g) in anhydrous potassium carbonate and 25ml dimethyl sulfoxide, reacted at 160°C in the dark for 50 hours, cooled to room temperature, then poured into 10 times the volume of water to obtain a yellow precipitate, filtered, and put the filter cake at 80°C Vacuum-dried to obtain 2.27 g of a small molecule photoinitiator 4,4'-dipiperazine benzophenone with a yield of 66%.

[0034] b) Dissolve 2mmol (0.4084g) glycerol diglycidyl ether completely in 10ml ethanol, then add 1.9mmol (0.6659g) 4,4'-dipiperazine benzophenone under nitrogen protection, and heat up to 80 ℃, reacted for 5 hours, cooled to room temperature, and then poured into 10 times the volume of anhydrous ether, poured out the liquid after the precipitation was complete, and dried in vacuum. Obtain 0.91 g of high-molecular-weight michketone photoi...

Embodiment 3

[0036] a) In a 100ml three-neck flask with magnetic stirring and nitrogen gas, add 0.02mol (4.36g) of 4,4'-difluorobenzophenone, 0.2mol (17.23g) of piperazine, 0.05mol (6.95g) in anhydrous potassium carbonate and 25ml dimethyl sulfoxide, reacted at 160°C in the dark for 50 hours, cooled to room temperature, then poured into 10 times the volume of water to obtain a yellow precipitate, filtered, and put the filter cake at 80°C Vacuum-dried to obtain 2.27 g of a small molecule photoinitiator 4,4'-dipiperazine benzophenone with a yield of 66%.

[0037]b) Add 2mmol (1.28g) polypropylene oxide glycidyl ether to 10ml ethanol to dissolve completely, add 1.9mmol (0.6634g) 4,4'-dipiperazine benzophenone under nitrogen protection, and heat up to 75°C , reacted for 6 hours, cooled to room temperature, and then poured into 10 times the volume of anhydrous ether to obtain a yellow viscous liquid, which was dried in vacuum to obtain 1.55 g of macromolecular micone photoinitiator, with a yiel...

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Abstract

The invention discloses a method for preparing polymer Michler's ketone photoinitiators, which is shown in the following formula. The method comprises the following steps: synthesizing Michler's ketone containing two methyl tertiary amines by using 4,4'-difluorobenzophenone and piperazine as raw materials, dissolving the resulting Michler's ketone and a diepoxy monomer in an organic solvent, and allowing polymerization reaction for several hours under heating to produce the polymer Michler's ketone photoinitiator. The photoinitiator contains both Michler's ketone and amine co-initiator in themain chain and exhibits excellent photoinitiation property. Compared with the micromolecular photoinitiators, the polymer photoinitiator has the advantages of low mobility and toxicity and is widely used in painting, microelectronics and optical fields.

Description

technical field [0001] The present invention relates to a kind of preparation method of photoinitiator, especially a kind of preparation method of macromolecule michrone photoinitiator. It belongs to the field of photochemical technology. Background technique [0002] The wide application of UV curing technology in industrial fields such as photocurable coatings, photoresists, photocurable inks, electronic packaging materials, adhesives, CD duplication, and paper glazing has shown good development prospects. In the progress of photocuring technology, the research and development of photoinitiator system occupies an important position. [0003] With the development of science and technology, the requirements for the performance of photoinitiators (initiation speed, compatibility with photocuring system, toxicity, storage stability) are also getting higher and higher. For the photocuring system, during long-term storage, small molecule photoinitiators are prone to volatiliza...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02C08F2/50
Inventor 温延娜姜学松印杰
Owner SHANGHAI JIAOTONG UNIV
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