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Photoinitiator suitable for solidifying LED as well as preparation method and application of photoinitiator

A photoinitiator and compound technology, applied in the field of 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

Inactive Publication Date: 2017-08-11
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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  • Photoinitiator suitable for solidifying LED as well as preparation method and application of photoinitiator
  • Photoinitiator suitable for solidifying LED as well as preparation method and application of photoinitiator
  • Photoinitiator suitable for solidifying LED as well as preparation method and application of photoinitiator

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1: the preparation of photoinitiator P6601

[0052]

[0053] a. Ethyl phenylphosphonate

[0054]With stirring, 179g (1.0mol) of phenylphosphine dichloride was added dropwise to 138g (3.0mol) of absolute ethanol cooled with ice and kept at 5-10°C. After the dropwise addition, react at room temperature for 3 hours, then evaporate the volatile components under reduced pressure with a water pump, and distill the remaining liquid under reduced pressure to collect 120 g of b.p.120°C / 0.4kpa fraction, with a yield of 70%.

[0055] b. Condensation

[0056] Dissolve 34.0g of ethyl phenylphosphonate and p-dimethylaminobenzaldehyde (29.8g, 0.2mol) in 200ml of tetrahydrofuran, slowly add triethylamine (20.2g, 0.2mol) dropwise under stirring at room temperature, dropwise After completion, the reaction at room temperature was continued for 4 hours. After the reaction was detected by TLC, the solvent was removed and recrystallized to obtain 59.6 g of the intermediate, w...

Embodiment 2

[0059] Embodiment 2: the preparation of photoinitiator P6610

[0060]

[0061] a. S-Ethylphenylphosphinosulfate

[0062] With stirring, 179g (1.0mol) of phenylphosphine dichloride was added dropwise to 186.4g (3.0mol) of anhydrous ethanethiol cooled with ice and kept at 5-10°C. After the dropwise addition, react at room temperature for 3 hours, then evaporate the volatile components under reduced pressure with a water pump, and distill the remaining liquid under reduced pressure to collect 144.6 g of b.p.120°C / 0.4kpa fraction, with a yield of 73.2%.

[0063] b. Condensation

[0064] Dissolve 37.2g of S-ethylphenylphosphinosulfate and p-dimethylaminobenzaldehyde (29.8g, 0.2mol) in 200ml of tetrahydrofuran, slowly add triethylamine (20.2g, 0.2mol) dropwise under normal temperature stirring ), continue to react at room temperature for 4h after the dropwise addition, and after the completion of the TLC detection reaction, remove the solvent and recrystallize to obtain 55.6g o...

Embodiment 3

[0067] Embodiment 3: the application of photoinitiator P6601

[0068] a, the trade mark produced by 25 parts of quality Sartomer company is the four-functional polyester acrylate of CN2203, 20 parts of quality Sartomer company's production mark is the difunctional group bisphenol A epoxy acrylate of CN120, 25 parts of quality The TPGDA produced by the Sartomer company, the TMPTA produced by the Sartomer company of 20 parts of quality are mixed evenly, then the photoinitiator of the present invention that adds 5 parts of quality, the brand that 5 parts of quality BYK companies produce are the leveling agent that is 361, Mix evenly to obtain LED cured coating.

[0069] b. Apply the LED curable coating prepared in this example on a glass sheet, and cure it under the radiation of a UV-LED lamp with a wavelength of 395nm for 1s, 3s, 5s, 10s, 30s, 60s, and 120s, and judge the curing by finger pressure method The tack of the film was used to characterize the curing speed.

[0070] ...

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Abstract

The invention discloses photoinitiator suitable for solidifying an LED as well as a preparation method and application of the photoinitiator. An electron-donating group is coupled to an acyl phosphorus skeleton structure, so that absorption wavelength red shifts to 385nm, and polymerization of unsaturated monomers can be effectively induced under the radiation of a UV-LED lamp; the photoinitiator has good dissolubility in various types of resin monomers, low polymers and diluents, is high in induction velocity and is especially applicable to surface solidification of coatings, ink and the like.

Description

technical field [0001] The invention relates to a photoinitiator suitable for LED curing and a preparation method thereof, in particular to an organic phosphorus compound 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 preheatin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32C08F2/48C09D167/06C09D163/10C09D7/12
CPCC07F9/3252C08F2/48C09D7/63C09D167/06C08L63/10
Inventor 叶正培范业成辜艳华
Owner CHANGSHANG NEWSUN CHEM IND
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