Copolymerized macromolecular photoinitiator and preparation method thereof

A technology of photoinitiator and macromolecule, which is applied in the field of photoinitiator synthesis, can solve the problems affecting the performance of water-based photocuring system, and achieve the effect of improving the problem of oxygen inhibition and low migration

Active Publication Date: 2019-07-09
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, traditional small molecule photoinitiators have been widely used in water-based light-curing systems, but many of their drawbacks also affect the final performance of water-based light-curing systems

Method used

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  • Copolymerized macromolecular photoinitiator and preparation method thereof
  • Copolymerized macromolecular photoinitiator and preparation method thereof
  • Copolymerized macromolecular photoinitiator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of a copolymerized macromolecular photoinitiator, comprising the following steps:

[0037] (1) Weigh 1mol furfuraldehyde and 1mol N-vinylpyrrolidone and dissolve them in 20mL of ethyl acetate, and mix them uniformly under stirring;

[0038] (2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0039] (3) The light yellow crystals of step (2) are washed with dichloromethane, dried in vacuo to remove the solvent, and the pure light yellow product 2-furan vinyl-N-vinylpyrrolidone is obtained, and its structural formula is

[0040] (4) Dissolve 1mol 2-furyl vinyl-N-vinylpyrrolidone and 0.5mol 1-allylpiperazine in ethanol, add 3-5 drops of saturated sodium hydroxide solution dropwise, blow nitrogen, and heat in a water bath to 50 ℃, reflux, and magne...

Embodiment 2

[0045] A preparation method of a copolymerized macromolecular photoinitiator, comprising the following steps:

[0046] (1) Weigh 1mol of N-ethylcarbazole-3-carbaldehyde and 1mol of N-vinylpyrrolidone, dissolve them in 20mL of ethyl acetate, and mix evenly under stirring;

[0047] (2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0048] (3) Wash the light yellow crystals in step (2) with dichloromethane, dry in vacuo to remove the solvent, and obtain a pure light yellow product, which is 2-ethylcarbazolevinyl-N-vinylpyrrolidone, whose structural formula is

[0049] (4) Dissolve the product 2-ethylcarbazolevinyl-N-vinylpyrrolidone obtained in step (3) in methanol, add 3-5 drops of saturated sodium hydroxide solution dropwise, nitrogen, and heat in a water bath to 50 ℃, r...

Embodiment 3

[0054] A preparation method of a copolymerized macromolecular photoinitiator, comprising the following steps:

[0055] (1) Weigh 1mol 3,4-ethylenedioxythiophene-2-carbaldehyde and 1mol N-vinylpyrrolidone, dissolve them in 20mL of ethyl acetate, and mix them uniformly under stirring;

[0056](2) Add 3-5 drops of 5% NaOH aqueous solution (0.5gNaOH, 9.5g water) to the mixed solution prepared in step (1), adjust the pH value to 13, react for 3h at 30°C, pass Enter nitrogen, use ice bath to continue reaction 3h, separate out light yellow crystal;

[0057] (3) Wash the light yellow crystals in step (2) with dichloromethane, dry in vacuo to remove the solvent, and obtain a pure light yellow product, which is 2-(3,4-ethylenedioxythiophene) vinyl-(N-ethylene Base) pyrrolidone, its structural formula is

[0058] (4) Dissolve the product 2-(3,4-ethylenedioxythiophene) vinyl-(N-vinyl)pyrrolidone and 1mol4-vinyl triphenylphosphineamine in methanol, drop Add 3-5 drops of saturated sodi...

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Abstract

The invention discloses a copolymerized macromolecular photoinitiator, and relates to the technical field of synthesizing photoinitiators in the field of photopolymerization. and the photoinitiator has a structural formula shown in the specification. The present invention also provides a preparation method for preparing the above photoinitiator. The beneficial effect is that the prepared copolymerized macromolecular photoinitiator of the invention can be copolymerized with different comonomers to improve the oxygen inhibition problem, and can provide a hydrogen donor as a one-component multi-faceted photoinitiator.

Description

technical field [0001] The invention relates to the technical field of synthesis of photoinitiators in the field of photopolymerization, in particular to a copolymerization macromolecular photoinitiator and a preparation method thereof. Background technique [0002] Since 1946, a company in the United States first published the patent of unsaturated polyester / styrene ultraviolet light UV curing technology. , paper glazing and other industrial fields have been widely used, and light curing technology has maintained rapid development. [0003] Photoinitiator is one of the important factors affecting photopolymerization. It can absorb ultraviolet light or visible light radiation energy, so that oligomers and diluents can quickly change from liquid to solid compounds. In recent years, there have been many reports in the literature on the introduction of polysiloxane into free radical photoinitiators to obtain polysiloxane-modified macromolecular photoinitiators, endowing the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F226/06C08F230/02C08F212/14C08F2/48
CPCC08F2/48C08F226/06C08F230/02C08F212/14
Inventor 朱晓群钟美娟聂俊赵翔晨杨帆
Owner BEIJING UNIV OF CHEM TECH
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