Acyl phosphine photoinitiator

A technology of photoinitiator and acylphosphine, which is applied in the field of UV-LED curing photoinitiator and its preparation, can solve the problems of single radiation peak and weak absorption, and achieve the effects of good solubility, strong absorption and fast initiation rate

Active Publication Date: 2017-04-05
CHANGSHANG NEWSUN CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the single characteristic of the radiation peak of the UV-LED light source (main wavelengths at 365nm and 395nm) also limits the types of photoinitiators to choose from. Among the existing photoinitiator products, there are o

Method used

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  • Acyl phosphine photoinitiator
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  • Acyl phosphine photoinitiator

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0046] Example 1: Preparation of photoinitiator P6511

[0047]

[0048] a. Metal substitution of P, P-dichloroethoxyphosphine in toluene at 98℃-100℃

[0049] Under an inert gas atmosphere, suspend the sodium block (9.2g, 0.4mol) in toluene (500ml) at room temperature, heat up to reflux, when the temperature reaches 98°C, start stirring vigorously, disperse into small droplets of sodium and add dropwise P,P-dichloroethoxyphosphine (14.7g, 0.1mol) for more than one hour, and then refluxing for 16h to form a yellow suspension, and proceed directly to the next step without purification.

[0050] b. Protonation

[0051] Add tert-butanol (14.8g 0.2mol) dropwise to the yellow suspension at 98°C-100°C, and react under reflux until all the sodium is reacted. The product does not need to be purified and proceed to the next step directly.

[0052] c, condensation

[0053] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol) to the reaction solution of b, dropwise add triethylamine (20.2g, 0.2mol), reac...

Example Embodiment

[0056] Example 2: Preparation of photoinitiator P6512

[0057]

[0058] a. Metal substitution of P,P-dichlorophenylphosphine in toluene at 98℃-100℃

[0059] Under an inert gas atmosphere, suspend the sodium block (9.2g, 0.4mol) in toluene (500ml) at room temperature, heat up to reflux, when the temperature reaches 98℃, start stirring vigorously, disperse into small droplets of sodium and add dropwise P,P-Dichlorophenylphosphine (17.8g, 0.1mol) for more than one hour, and then reflux and heat the reaction for 16h to form a yellow suspension, and proceed directly to the next step without purification.

[0060] b. Protonation

[0061] Add tert-butanol (14.8g 0.2mol) dropwise to the yellow suspension at 98°C-100°C, and react under reflux until all the sodium is reacted. The product does not need to be purified and proceed to the next step directly.

[0062] c, condensation

[0063] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol) to the reaction solution of b, dropwise add triethylamine (20....

Example Embodiment

[0066] Example 3: Preparation of photoinitiator P6513

[0067]

[0068] a. Metal substitution of P, P-dichloromethyl phosphine in toluene at 98℃-100℃

[0069] Under an inert gas atmosphere, suspend the sodium block (9.2g, 0.4mol) in toluene (500ml) at room temperature, heat up to reflux, when the temperature reaches 98℃, start stirring vigorously, disperse into small droplets of sodium and add dropwise P,P-Dichloromethylphosphine (11.6g, 0.1mol) for more than one hour, and then reflux and heat the reaction for 16h to form a yellow suspension, and proceed directly to the next step without purification.

[0070] b. Protonation

[0071] Add tert-butanol (14.8g 0.2mol) dropwise to the yellow suspension at 98°C-100°C, and react under reflux until all the sodium is reacted. The product does not need to be purified and proceed to the next step directly.

[0072] c, condensation

[0073] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol) to the reaction solution of b, dropwise add triethylamine (2...

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Abstract

The invention discloses an acyl phosphine photoinitiator shown as a specification and a preparation method thereof. The bifunctional acyl phosphine photoinitiator has a macro-molecule structure, eliminates migratory aptitude of the photoinitiator during a usage process, improves yellowing phenomenon, and couples a tertiary amine structure on an aromatic ring compound, the UV absorption wavelength shows bathochromic shift to 380-395 nm, polymerization of a unsaturated monomer is effectively initiated under radiation of a UV-LED lamp; in addition, the compound has good dissolvability in various resins and an oligomer, and is the novel macro-molecule acyl phosphine photoinitiator.

Description

technical field [0001] The invention relates to an acylphosphine photoinitiator and a preparation method thereof, in particular to a photoinitiator suitable for UV-LED curing and a preparation method thereof. [0002] technical background [0003] At present, the light curing technology mainly adopts ultraviolet light curing, and most of the ultraviolet light sources still use high-pressure mercury lamps; there are some obvious disadvantages in high-pressure mercury lamp curing: [0004] High power, large heat release during use, requires a strong cooling medium; [0005] High energy consumption during curing; [0006] Long startup time and slow warm-up; [0007] High requirements on the base material; [0008] There is mercury contamination. [0009] The emerging UV-LED light source has obvious advantages over high-pressure mercury lamps: [0010] Cold light source, low power, low energy consumption, wide range of substrate applications; [0011] Ready to use, no prehe...

Claims

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Application Information

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IPC IPC(8): C08F2/48C07F9/32
CPCC07F9/3241C08F2/48
Inventor 叶正培周潭王辉明
Owner CHANGSHANG NEWSUN CHEM IND
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