Novel cationic photoinitiator as well as preparation method and application

一种光引发剂、阳离子型的技术，应用在新型阳离子型光引发剂及其制备领域，能够解决不能有效利用长波长光源、易黄变、易迁移出小分子化合物等问题

Active Publication Date: 2018-02-16
CHANGZHOU TRONLY NEW ELECTRONICS MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Triarylsulfonium salts are currently the most widely used cationic photoinitiators with better performance. They are superior to diaryliodonium salts in terms of absorption wavelength, thermal stability, and initiating activity. The maximum absorption wavelength of the agent is still less than 300nm, and the long-wavelength light source cannot be effectively used, and there are solubility and migration problems, which limit the use to a certain extent.
People try to improve its structure, such as introducing long-chain alkyl groups to improve its solubility, introducing multifunctional groups to improve initiation efficiency and thermal stability, etc., but in practical applications, these improved structures often have the tendency to migrate out of small molecules. Compounds, easy yellowing and other defects, and the initiation efficiency still needs to be further improved

Method used

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  • Novel cationic photoinitiator as well as preparation method and application
  • Novel cationic photoinitiator as well as preparation method and application
  • Novel cationic photoinitiator as well as preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053]

[0054] (1) Preparation of Intermediate 1a

[0055] Add 83g of raw material 1a, 67g of aluminum trichloride, and 200mL of dichloromethane into a 1000mL four-neck flask, and drop the ice-water bath to 0°C. Dissolve 101g of raw material 1b in 200mL of dichloromethane, then put it into a dropping funnel, control the temperature below 10°C, add the mixed solution of raw material 1b and dichloromethane dropwise into the four-neck flask, dropwise after about 2h, add dropwise Continue to stir for 24 hours, track the liquid phase until the concentration of the raw materials does not change, then slowly pour the material into 800 g of deionized water, stir, and the solid precipitates, and suction filters to obtain a light yellow solid, which is dried in an oven at 80 ° C for 2 hours to obtain 152 g of intermediate 1a , yield 79%, purity 98%.

[0056] (2) Preparation of compound 1

[0057] Dissolve 152g of potassium hexafluorophosphate in 150mL of acetone, then add 115g of ...

Embodiment 2

[0062]

[0063] (1) Preparation of Intermediate 2a

[0064] Add 40g of raw material 2a, 14g of aluminum trichloride, and 50mL of dichloromethane into a 500mL four-neck flask, and drop the ice-water bath to 0°C. Dissolve 31g of raw material 2b in 50mL of dichloromethane, then put it into a dropping funnel, control the temperature below 10°C, add the mixed solution of raw material 2b and dichloromethane dropwise into the four-neck flask, dropwise for about 2 hours, add dropwise Continue to stir for 24 hours, track the liquid phase until the concentration of the raw materials does not change, then slowly pour the material into 200 g of deionized water, stir, the solid precipitates, and suction filters to obtain a light yellow solid, which is dried in an oven at 80 ° C for 2 hours to obtain 46 g of intermediate 2a , yield 64%, purity 98%.

[0065] (2) Preparation of Compound 2

[0066] Dissolve 45g of tetrakis(pentafluorophenyl)sodium borate in 100mL of acetone, then add 43g ...

Embodiment 3

[0070]

[0071] (1) Preparation of Intermediate 3a

[0072] Add 22g of raw material 3a, 28g of aluminum trichloride, and 50mL of dichloromethane into a 500mL four-neck flask, and drop the ice-water bath to 0°C. Dissolve 46g of raw material 3b in 100mL of dichloromethane, then put it into a dropping funnel, control the temperature below 10°C, add the mixed solution of raw material 3b and dichloromethane dropwise into the four-neck flask, dropwise for about 2 hours, and dropwise Continue to stir for 24 hours, track the liquid phase until the raw materials no longer change, then slowly pour the materials into 200 g of deionized water, stir, and the solid precipitates, and suction filters to obtain a light yellow solid, which is dried in an oven at 80°C for 2 hours to obtain 56 g of intermediate 3a. Yield 65%, purity 98%.

[0073] (2) Preparation of Compound 3

[0074]Dissolve 60g of sodium perfluorobutane sulfonate in 100mL of acetone, then add 55g of intermediate 3a prepare...

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Abstract

The invention discloses a novel cationic photoinitiator represented by a general formula (I) in the description. According to the invention, the photoinitiator can match a longer absorption wavelengthin an application process, and has excellent photosensitive properties and the characteristics of being not easy to migrate and having yellowing resistance.

Description

technical field [0001] The invention belongs to the technical field of organic photocuring, and in particular relates to a novel cationic photoinitiator and its preparation method and application. Background technique [0002] Photoinitiator is a key component of photocurable products, and it plays a decisive role in the curing rate of photocurable products. Photoinitiators can be divided into cationic photoinitiators and free radical photoinitiators according to their different initiating mechanisms. Compared with free radical polymerization, cationic photocuring systems have less polymerization inhibition by oxygen and less volume shrinkage during curing. The advantages of small size and wide selection of resin types. In my country, the research and development of cationic light-curing system is late, and there are not many enterprises capable of industrial production. [0003] Triarylsulfonium salts are currently the most widely used cationic photoinitiators with better...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/12C07D333/76C07D335/12C07D327/08
CPCC07C381/12C07D327/08C07D333/76C07D335/12C07D335/16C08F2/50C08G59/68C08K5/36C09K3/00G03F7/004
Inventor 钱晓春胡春青于培培徐仁丰
Owner CHANGZHOU TRONLY NEW ELECTRONICS MATERIALS
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