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A kind of macromolecular photoinitiator and its application and preparation method

A photoinitiator and macromolecular technology, applied in the field of photocuring, can solve the problems of affecting the quality of color glue, difficult to dissolve, low solubility, etc., and achieve the effect of improving the initiation efficiency, increasing the resin content and the appropriate molecular weight

Active Publication Date: 2022-05-03
BEIJING ETERNAL MATERIAL TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing photoinitiators for color glue mostly use solid small molecule photoinitiators, which often have poor compatibility with colorants, resins, monomers, etc., color, easy yellowing, easy aggregation, easy precipitation, low solubility, and poor thermal stability. , Easy to migrate or precipitate from the color glue after light curing, which affects the quality of the color glue and the health of workers on the production line
On the other hand, ordinary macromolecular photoinitiators have the problem of being difficult to dissolve in the color gel system

Method used

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  • A kind of macromolecular photoinitiator and its application and preparation method
  • A kind of macromolecular photoinitiator and its application and preparation method
  • A kind of macromolecular photoinitiator and its application and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1. Poly(4-(2-Acrylomethyl)benzophenone Synthesis

[0050]

[0051] Add 48g methanol (1.5mol) to the 250mL three-necked flask and stir, heat up to reflux, slowly add 42g diketene (0.5mol), continue to react at reflux temperature for 5h, and distill under reduced pressure to obtain methyl acetoacetate 89.4g (0.77mol) .

[0052] Add 200mL of THF and 15.6g of stirred and dispersed NaH (60% dispersed in mineral oil, 0.39mol) to a 500mL there-neck flask under argon protection, and 34.8g of methyl acetoacetate (0.3mol) was added dropwise to the flask at room temperature medium and stir well. When the liquid in the flask became clear, 46.8 g of methyl iodide (0.33 mmol) was added dropwise, the mixture was stirred at 40 °C for 10 h, the reaction solution was quenched with saturated aqueous ammonium chloride and extracted with ethyl acetate three times. The combined organic layers were dried over anhydrous sodium sulfate, and the solvent was spin-dried, and separat...

Embodiment 2

[0069] Example 2. Poly 4-(2-ethyl acrylate) benzophenone F-2 Synthesis

[0070]

[0071] The synthesis process of F-2 is referred to the synthesis of F-1, the difference is that the methanol used in A-1 is replaced by ethanol.

[0072] NMR data of E-2: 1 HNMR (300 Hz) in DMSO: δ 1.07 ppm (t, 3H), 4.00 ppm (q, 2H), 6.19, 6.37 ppm (d, J=58.3, 2H), 7.41-7.84 ppm (m, 9H).

[0073] F-2 molecular weight data: M w = 8500, PDI = 1.49.

Embodiment 3

[0074] Example 3. Poly4'-methoxy, 4-(2-ethyl acrylate) benzophenone F-3 Synthesis

[0075] The synthesis process of F-3 refers to the synthesis of F-1, the difference is that the raw material E-3 for synthesizing F-3 is to use the 4-bromobenzophenone used in E-1 with 4-bromo, 4'-methoxy The base benzophenone C-1 is replaced, and the synthetic method of C-1 is as follows:

[0076]

[0077] Into a 500mL three-necked flask, add 21.95g 4-bromobenzoyl chloride (0.1mol) and 17.3g anhydrous aluminum trichloride (0.13mol), and add 100mL CH 2 Cl 2 The solids were dissolved and placed in a low temperature reaction bath at 10°C with stirring. Mix 140.6 g of anisole (0.13 mol) with 50 ml of CH 2 Cl 2 Mix well, add to constant pressure dropping funnel and start dripping. After the dropwise addition, add 20mL CH2 Cl 2 Rinse the constant-pressure dropping funnel, slowly raise the temperature of the cooling bath to 20°C, and continue stirring. At the end of the reaction, the react...

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Abstract

A macromolecular photoinitiator, which uses hydrogen abstraction type photoinitiator benzophenone as the core, and introduces a (meth)acrylate group into a benzene ring. The (meth)acrylate group is polymerized into a macromolecular photoinitiator with a specific range of molecular weight. On the one hand, it has high solubility and compatibility in ester solvents, and on the other hand, the diphenyl The ketone photosensitive group can initiate the polymerization of active monomers in color gel under ultraviolet light. If the other benzene ring of the benzophenone as a side chain contains a hydrogen-donating group, the hydrogen-donating group can significantly improve the initiation efficiency of the photoinitiator and the polymerization speed of the system.

Description

technical field [0001] The invention relates to the technical field of photocuring, and in particular provides a benzophenone macromolecular photoinitiator and an application and preparation method thereof. Background technique [0002] Photoresist, also known as photoresist, is a light-sensitive mixture composed of photosensitive resin, photoinitiator and solvent. Under the irradiation of ultraviolet light beam, it can undergo cross-linking curing or degradation reaction (called photolithography). Color photoresist (or color photosensitive / photosensitive resin composition) is made by adding colorants (red, green and blue) to photoresist. The color filter is made by coating the color photoresist on the glass substrate to form a film and then lithography by ultraviolet light to form a color pattern. [0003] The photoinitiator is the core component of the color photosensitive resin composition, and is a necessary material for the composition to be cured under ultraviolet li...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/26C08F120/34C08F2/48
CPCC08F120/26C08F120/34C08F2/48
Inventor 桑伟刘永祥侯少堃王晓青孙涛
Owner BEIJING ETERNAL MATERIAL TECH