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One-component polysiloxane photoinitiator capable of overcoming oxygen inhibition and preparation method thereof

A technology of photoinitiator and polysiloxane, which is applied in the field of photoinitiator, can solve the problems of affecting effect and poor compatibility, and achieve the effect of convenient cost control, high initiation efficiency and conventional raw materials

Active Publication Date: 2021-06-04
WUHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is a problem of poor compatibility between low-polarity hydrogen-containing polysiloxane and active monomers, which makes the physically added hydrogen-containing polysiloxane easy to phase-separate from the photopolymerization system and affect its effect

Method used

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  • One-component polysiloxane photoinitiator capable of overcoming oxygen inhibition and preparation method thereof
  • One-component polysiloxane photoinitiator capable of overcoming oxygen inhibition and preparation method thereof
  • One-component polysiloxane photoinitiator capable of overcoming oxygen inhibition and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041]

[0042] Preparation method: Weigh 0.14g (0.5mmol) 2-(N-methyl-N-allyl)thioxanthone and 0.7g 0.30wt% hydrogen-containing polysiloxane (x=0.75 , y+z=0.25, n=28), under an argon atmosphere, add 30 mL of anhydrous tetrahydrofuran and a system of 500 ppm [Pt] Karstedt catalyst, stir the reaction at 25 ° C, and wait for 2-(N-methyl-N-ene After the reaction of propyl)thioxanthone was complete, the tetrahydrofuran was removed under reduced pressure to obtain a single-component polysiloxane photoinitiator capable of overcoming oxygen inhibition, which weighed 0.84 g after drying.

[0043] Proton NMR spectrum:

[0044] 1 H NMR (CDCl3 ,300MHz)δppm: -0.25~0.30(br,40H,Si-CH 3 ),0.35~0.60(br,2H,SiCH 2 ),1.16~1.36(br,2H,SiCH 2 CH 2 ),2.89~3.12(br,3H,NCH 3 ),3.18~3.49(br,2H,NCH 2 ), 4.68(s, 0.67H, Si-H), 6.90~7.15(br, 1H, Ar-H), 7.31~7.48(br, 2H, Ar-H), 7.49~7.66(br, 2H, Ar- H), 7.70-7.90 (br, 1H, Ar-H), 8.56-8.72 (br, 1H, Ar-H). FT-IR (film, cm -1 ):ν=2154(Si-H), 1594(C=...

Embodiment 2

[0048]

[0049] Preparation method: weigh 0.32g (1.0mmol) 4-(N-methyl-N-allyl)-N-(2-methoxyethyl) naphthalene diimide and 0.28g 0.70wt% hydrogen-containing polysiloxane (x=0, y+z=1, n=2), under an argon atmosphere, add 20 mL of anhydrous dioxane and a system of 100 ppm [Pt] Sperier's catalyst, control The reaction temperature was 40°C. After the reaction of 4-(N-methyl-N-allyl)-N-(2-methoxyethyl)naphthalene diimide was completed, it was cooled to room temperature under an argon atmosphere. The dioxane was removed under reduced pressure to obtain a one-component polysiloxane photoinitiator capable of overcoming oxygen inhibition, which weighed 0.60 g after drying.

[0050] Proton NMR spectrum:

[0051] 1 H NMR (CDCl 3 ,300MHz) δppm: -0.01~0.210 (Si-CH 3 ),0.84~0.93(SiCH 2 ), 1.17~1.24 (SiCH 2 CH 2 ), 3.04 (NCH 3 ), 3.37 (OCH 3 ),3.67~3.78(NCH 2 ,CH 3 NCH 2 ),4.41~4.46(OCH 2 ), 4.67(Si-H), 7.12~7.16(Ar-H), 7.61~7.67(Ar-H), 8.40~8.43(Ar-H), 8.47~8.49(Ar-H), 8.56~8...

Embodiment 3

[0055]

[0056] Preparation method: Weigh 0.13g (0.5mmol) 2-(allyloxy)thioxanthone and 0.89g0.14wt% hydrogen-containing polysiloxane (x=0.9, y+z=0.1 , n=200), under argon atmosphere, add 20mL of anhydrous tetrahydrofuran and the Sperier's catalyst of system 500ppm [Pt], control the reaction temperature to tetrahydrofuran reflux, after the reaction of 2-(allyloxy)thioxanthone is complete , cooled to room temperature under argon atmosphere. The tetrahydrofuran was removed under reduced pressure to obtain a one-component polysiloxane photoinitiator capable of overcoming oxygen inhibition, which weighed 1.00 g after drying.

[0057] Proton NMR spectrum:

[0058] 1 H NMR (CDCl 3 ,300MHz) δppm: -0.01~0.21(Si-CH 3 ), 0.72 (SiCH 2 ), 1.62 (SiCH 2 CH 2 ), 3.90 (O-CH 2 ), 6.94(Ar-H), 7.09(Ar-H), 7.26(Ar-H), 7.35(Ar-H), 7.42(Ar-H), 7.51(Ar-H), 7.58(Ar-H) .

[0059] UV maximum absorption peak: λ max = 402nm.

[0060] It can be seen from the spectrum data that 0.72(SiCH 2 )...

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Abstract

The invention discloses a single-component polysiloxane photoinitiator capable of overcoming oxygen inhibition. The specific structure is: wherein R is a photoinitiator. The initiator introduces a photoinitiator on the hydrogen-containing polyoxysilane side chain and retains a certain amount of silicon-hydrogen bonds, and uses the silicon-hydrogen bonds as hydrogen donors to overcome oxygen inhibition. At the same time, the preparation method of the single-component polysiloxane photoinitiator that can overcome oxygen inhibition is disclosed: the photoinitiator containing terminal alkenes is mixed with hydrogen-containing polysiloxane in an argon atmosphere, and then dissolved in a solvent , add an appropriate amount of hydrosilylation catalyst, react at a certain temperature, and remove the solvent under reduced pressure after the reaction is completed. The photoinitiator has good compatibility with the photocuring system, no additional co-initiator is needed during the photocuring process, the initiation efficiency is high, and the polymerization can be completed under aerobic conditions, which is environmentally friendly and energy-saving, and meets the requirements of green chemistry. It has broad application prospects in the field of photocuring.

Description

technical field [0001] The invention relates to the field of photoinitiators, in particular to a single-component polysiloxane initiator capable of overcoming oxygen inhibition. Background technique [0002] Photopolymerization technology is widely used in many fields such as photocurable coatings, adhesives, inks, microelectronics, and photoresists. However, in the process of use, some inherent difficulties or shortcomings also affect its use, such as the oxygen inhibition effect in the free radical photocuring system. [0003] In the free radical photocuring system, the ground state of the general substance is a singlet state, and the O 2 The stable state of , however, is a triplet state, with two unpaired electrons with the same spin direction. Therefore, it competes with free radical polymerization and consumes free radicals. Oxygen inhibition is mainly manifested in the air curing process, which often leads to the curing of the bottom layer of the coating, and the su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F283/12C08F226/02C08F226/06C08F216/14C08F220/30C08F122/14C08F2/48C08G18/16
Inventor 唐红定杨建静武青青熊英
Owner WUHAN UNIV
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