Preparation method of UV LED photoinitiator

A photoinitiator and solvent technology, applied in the field of UVLED photoinitiator preparation, can solve the problems of unsatisfactory curing effect, large amount of photoinitiator, cost pressure, etc., and achieve high yield, high initiation rate and low mobility Effect

Pending Publication Date: 2022-05-13
深圳市科信新材料科技有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, the photoinitiators used by people in order to cooperate with UV-LED light sources are generally several combinations of traditional aminoketones, acylphosphoryl oxides, thioxanthones, and tertiary amine co-initiators; patent CN102532967 discloses a UV- -The paint cured by LED light source, its components mainly include mercapto-modified acrylic resin, monomer, photoinitiator TPO, active amine co-initiator and corresponding auxiliary agents and pigments; patent CN102863848 discloses a class of UV-LED curing Ink formula, the ink is suitable for graphic printing on lithographic printing machines, letterpress printing machines and flexographic printing machines. The photoinitiators used include: 369, TPO, TEPO, 907 and PBZ, etc., with a large amount (15% to 20 %); patent CN103396689 discloses a UV-LED light-curing coating, the components include 30-65% acrylate oligomers, 20-50% monomers, 2-8% photoinitiators, etc., the composition For thick film coatings, the photoinitiators used include ITX, DETX, TPO and combinations thereof; patent CN102719143 discloses an outdoor screen printing ink composition cured by UV-LED surface light source, wherein the combination of photoinitiators is: Initiator 819, TPO, ITX, EDB combination, the proportion of each initiator component is 2 to 4%; although the current formula design can barely meet the requirements of UV-LED light source, the general amount of photoinitiator is large , causing cost pressure, if the amount of photoinitiator is reduced, the curing effect is not ideal; therefore, it is necessary to propose a preparation method of UV LED photoinitiator to at least partly solve the problems existing in the prior art

Method used

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  • Preparation method of UV LED photoinitiator

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Effect test

Embodiment 1

[0022] A preparation method for UV LED photoinitiator, comprising the following steps:

[0023] (1) Dissolve polyester acrylate (120mmol) in ethanol (2400mmol), add potassium hydroxide (320mmol) and stir for 1h, add isobornyl acrylate (140mmol), after reacting for 13h, add 4-hydroxybenzophenone 5ml quenched the reaction, extracted 3 times with N,N-dimethylformamide, combined the organic phases, washed the organic phase once with saturated brine, dried over anhydrous sodium sulfate, distilled off a large amount of solvent under reduced pressure, and obtained polydimethylformamide Siloxane was used as the mobile phase, and silica gel was used as the stationary phase to perform column chromatography to obtain a white solid with a yield of 98%.

[0024] (2) Dissolve the product from the previous step (50mmol) in chlorobenzene (520mmol), add 2,4,6-trimethylbenzoylphosphonic acid ethyl ester (150mmol), cool to 0°C and add p-cresol dropwise (150 mmol), after the dropwise addition wa...

Embodiment 2

[0028] A preparation method for UV LED photoinitiator, comprising the following steps:

[0029] (1) Dissolve epoxy acrylate (120mmol) in 1,2-dichloromethane (2600mmol), add sodium hydroxide (320mmol) and stir for 3h, add lauric acid acrylate (180mmol), after reacting for 10h, add 4 5ml of -hydroxybenzophenone quenched the reaction, extracted 3 times with N,N-dimethylformamide, combined the organic phases, washed the organic phase with saturated brine once, dried over anhydrous sodium sulfate, and distilled off a large amount of As a solvent, polydimethylsiloxane was used as mobile phase and silica gel was used as stationary phase to perform column chromatography to obtain a white solid with a yield of 96%.

[0030] (2) Dissolve the product from the previous step (50mmol) in 1,2-dichloromethane (550mmol), add 2,4,6-trimethylbenzoylphosphonic acid ethyl ester (180mmol), and cool to 3°C P-cresol (180 mmol) was added dropwise, and after the dropwise addition was completed, stirri...

Embodiment 3

[0034] A preparation method for UV LED photoinitiator, comprising the following steps:

[0035] (1) Dissolve polyether acrylate (120mmol) in chloroform (3600mmol), add sodium hydride (240mmol) and stir for 5h, add 3,3,5-trimethylcyclohexane acrylate (220mmol), react After 15 hours, 5ml of 4-hydroxybenzophenone was added to quench the reaction, extracted three times with N,N-dimethylformamide, the organic phase was combined, washed once with saturated brine, dried over anhydrous sodium sulfate, A large amount of solvent was distilled off under reduced pressure, and column chromatography was performed with polydimethylsiloxane as mobile phase and silica gel as stationary phase to obtain a white solid with a yield of 97%.

[0036] (2) Dissolve the previous step product (50mmol) in chlorobenzene (500mmol) and 1,2-dichloromethane mixed solvent (250mmol), add 2,4,6-trimethylbenzoylphosphonic acid ethyl ester (165mmol ), after cooling to 6°C, p-cresol (165 mmol) was added dropwise, ...

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Abstract

The invention discloses a UV LED photoinitiator preparation method, which comprises: (1) dissolving a carbazole derivative in an organic solvent, adding an inorganic alkali, stirring, adding a bromo-alkenyl derivative, completely reacting, carrying out a quenching reaction, and purifying to obtain a product 1; (2) dissolving the product 1 in the step (1) in an organic solvent, adding into 2, 4, 6-trimethylbenzoyl ethyl phosphonate, dropwise adding p-cresol, and stirring; performing reflux reaction and purification to obtain a product 2; (3) dissolving the product 2 in the step (2) and methyltriphenylphosphonium bromide in N, N-dimethylformamide, stirring and reacting, and purifying to obtain a product 3; and (4) dissolving the product 3 in the step (3) in an organic solvent, adding zinc trichloride, stirring for reaction, and purifying to obtain the UV LED photoinitiator. The compound is used for a UV-LED photocuring coating and has the advantages of being low in migration rate, high in initiation rate, easy to dissolve and the like, and the synthesis method is high in yield.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, in particular to a preparation method of a UV LED photoinitiator. Background technique [0002] At present, the photoinitiators used by people in order to cooperate with UV-LED light sources are generally several combinations of traditional aminoketones, acylphosphoryl oxides, thioxanthones, and tertiary amine co-initiators; patent CN102532967 discloses a UV- -The paint cured by LED light source, its components mainly include mercapto-modified acrylic resin, monomer, photoinitiator TPO, active amine co-initiator and corresponding auxiliary agents and pigments; patent CN102863848 discloses a class of UV-LED curing Ink formula, the ink is suitable for graphic printing on lithographic printing machines, letterpress printing machines and flexographic printing machines. The photoinitiators used include: 369, TPO, TEPO, 907 and PBZ, etc., with a large amount (15% to 20 %); patent CN103396689...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C08F283/01C08F283/10C08F283/06C08F220/18
CPCC08F2/48C08F283/01C08F283/105C08F283/065C08F220/1811C08F220/1812C08F220/1809
Inventor 郭新明任德磊
Owner 深圳市科信新材料科技有限公司
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