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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 only acylphosphine, thioxanthone, and aminoketone The three photoinitiators have absorption in the UV-LED radiation wavelength range, but also have the disadvantage of weak absorption and need to increase the amount of initiator added

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Embodiment 1: the preparation of photoinitiator P6511

[0047]

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

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

[0050] b. Protonation

[0051] At 98°C-100°C, tert-butanol (14.8g 0.2mol) was added dropwise to the above yellow suspension, and the reaction was refluxed until all the sodium was reacted, and the product was directly subjected to the next reaction without purification.

[0052] c. Condensation

[0053] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol)...

Embodiment 2

[0056] Embodiment 2: the preparation of photoinitiator P6512

[0057]

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

[0059] Under an inert gas atmosphere, suspend sodium block (9.2g, 0.4mol) in toluene (500ml) at room temperature, raise the temperature to reflux, start vigorous stirring when the temperature reaches 98°C, disperse into small sodium droplets and add dropwise P,P-dichlorophenylphosphine (17.8g, 0.1mol) was used for more than one hour, and then heated under reflux for 16h to form a yellow suspension, which was directly carried out to the next step without purification.

[0060] b. Protonation

[0061] At 98°C-100°C, tert-butanol (14.8g 0.2mol) was added dropwise to the above yellow suspension, and the reaction was refluxed until all the sodium was reacted, and the product was directly subjected to the next reaction without purification.

[0062] c. Condensation

[0063] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol)...

Embodiment 3

[0066] Embodiment 3: the preparation of photoinitiator P6513

[0067]

[0068] a. Metal substitution of P,P-dichloromethylphosphine in toluene at 98°C-100°C

[0069] Under an inert gas atmosphere, suspend sodium block (9.2g, 0.4mol) in toluene (500ml) at room temperature, raise the temperature to reflux, start vigorous stirring when the temperature reaches 98°C, disperse into small sodium droplets and add dropwise P,P-dichloromethylphosphine (11.6g, 0.1mol) was used for more than one hour, and then heated under reflux for 16h to form a yellow suspension, which was directly carried out to the next step without purification.

[0070] b. Protonation

[0071] At 98°C-100°C, tert-butanol (14.8g 0.2mol) was added dropwise to the above yellow suspension, and the reaction was refluxed until all the sodium was reacted, and the product was directly subjected to the next reaction without purification.

[0072] c. Condensation

[0073] Add p-dimethylaminobenzaldehyde (29.8g, 0.2mol)...

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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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