UV LED photoinitiator and preparation method thereof

A technology of photoinitiator and compound, which is applied in the field of UVLED photoinitiator and its preparation, can solve the problems of increasing initiator and emission wavelength mismatch, and achieve the effects of increasing content, promoting surface curing, and good photosensitivity

Active Publication Date: 2020-12-15
新丰博兴聚合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a kind of UV LED photoinitiator for overcoming above-mentioned prior art described needing to increase initiator dosage, adding auxiliary agent or absorption wavelength and UV LED emission wavelength mismatch, and the UVLED photoinitiator provided is to UVA Ultraviolet light has good photosensitivity, and can achieve a good initiation rate without adding additional hydrogen donor additives, and the photoinitiator will be enriched on the surface of the coating and distributed in a gradient throughout the coating, effectively inhibiting the surface Oxygen inhibition without increasing the amount of photoinitiator

Method used

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  • UV LED photoinitiator and preparation method thereof
  • UV LED photoinitiator and preparation method thereof
  • UV LED photoinitiator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Specific description of the exclusive plan

[0046] The present embodiment provides a kind of UV LED photoinitiator, has formula (M 1 ) shown chemical structure, its preparation method is as follows.

[0047] synthetic route:

[0048]

[0049] Steps:

[0050] S1. Preparation formula (C 1 ) compound

[0051] 90.8g (0.59mol) of thiosalicylic acid was dissolved in 800mL of concentrated sulfuric acid, and 96.63g (0.89mol) of formula (B 1) compound, that is, hydroxymethylbenzene, and then heated to 80° C. for 2 h, and then placed at room temperature for 12 h. The reactant was slowly added to 2L of boiling water, cooled to room temperature, stirred for 1 h, and filtered to obtain a crude product. Thick product dioxane: acetone=3:1 mixed solvent carries out recrystallization, obtains light yellow product formula (C 1 ) compounds.

[0052] S2. Formula (M 1 ) Compound preparation

[0053] Under dark conditions, formula (C 1 ) compound (24.2g, 0.1mol) was dissolved ...

Embodiment 2

[0058] The present embodiment provides a kind of UV LED photoinitiator, has formula (M 2 ) shown chemical structure, its preparation method is as follows.

[0059] synthetic route:

[0060]

[0061] Steps:

[0062] S1. Preparation formula (C 2 ) compound

[0063] 90.8g (0.59mol) of thiosalicylic acid was dissolved in 1000mL of concentrated sulfuric acid, and 160.28g (1.18mol) of formula (B 2 ) compound, that is, m-methyl (hydroxyethyl) benzene, then heated up to 80° C. for 2 h, and left at room temperature for 12 h. The reactant was slowly added to 2.5 L of boiling water, cooled to room temperature, stirred for 1 h, and filtered to obtain a crude product. Thick product dioxane: acetone=3:1 mixed solvent carries out recrystallization, obtains light yellow product formula (C 2 ) compounds.

[0064] S2. Formula (M 2 ) Compound preparation

[0065] Under dark conditions, formula (C 2 ) compound (27.1g, 0.1mol) was dissolved in 240mL chloroform solution, adding formula...

Embodiment 3

[0070] The present embodiment provides a kind of UV LED photoinitiator, has formula (M 3 ) shown chemical structure, its preparation method is as follows.

[0071] synthetic route:

[0072]

[0073] Steps:

[0074] S1. Preparation formula (C 3 ) compound

[0075] 90.8g (0.59mol) of thiosalicylic acid was dissolved in 1000mL of concentrated sulfuric acid, and 177.12g (1.18mol) of formula (B 3 ) compound, then heated up to 80° C. for 2 h, and left at room temperature for 12 h. The reactant was slowly added to 2.5 L of boiling water, cooled to room temperature, stirred for 1 h, and filtered to obtain a crude product. Thick product dioxane: acetone=3:1 mixed solvent carries out recrystallization, obtains light yellow product formula (C 3 ) compounds.

[0076] S2. Formula (M 3 ) Compound preparation

[0077] Under dark conditions, formula (C 3 ) compound (28.4g, 0.1mol) was dissolved in 250mL chloroform solution, adding formula (D 3 ) compound (50.2g, 0.1mol), trifluo...

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Abstract

The present invention discloses a UV LED photoinitiator and a preparation method thereof. The UV LED photoinitiator has a chemical structure represented by a formula (M) as shown in the specification,wherein X is a group shown in the specification, a group shown in the specification or a group shown in the specification, and H represents acetal alpha-H; R1 represents a linear or branched alkylenegroup having a carbon atom number of 0-4; R2 represents a linear or branched alkylene group having a carbon atom number of 1-4; R3, R4 and R5 are each independently a hydrogen atom or a linear or branched alkyl group having a carbon atom number of 1-4; and n is an integer of 6-24. The UV LED photoinitiator disclosed by the invention has good photosensitivity to ultraviolet light in a UVA section,and can be applied to commercial UV LED curing, like photocuring coating or printing ink; an acetal alpha-H group is contained in the structure, so that a good initiation rate can be achieved withoutadditionally adding a hydrogen donor aid; the photoinitiator can be enriched on the surface of a coating and is distributed in the whole coating in a gradient manner, so that the concentration of thephotoinitiator on the surface of the coating is increased, surface oxygen inhibition is effectively inhibited, surface curing is promoted, and the dosage of the photoinitiator does not need to be increased.

Description

technical field [0001] The invention relates to the technical field of photocuring of polymer materials, more specifically, to a UV LED photoinitiator and a preparation method thereof. Background technique [0002] Radiation curing refers to the process of cross-linking and polymerizing liquid oligomers (including monomers) to form solid products under the action of light (including ultraviolet and visible light) or high-energy rays (mainly electron beams). Radiation curing technology has the advantages of fast curing speed, energy saving and environmental protection, and is widely used in coatings, inks, 3D printing, dental materials and other fields. Free radical photocuring technology is the most commonly used technical method in UV curing technology. It has the characteristics of fast curing speed. However, due to the existence of oxygen inhibition, the curing process of free radical photocuring is not complete, and it may even cause the surface of the coating to burn. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D335/16C07D409/12C08F2/48
CPCC07D335/16C07D409/12C08F2/48
Inventor 庞来兴黄李江谢平连柳光
Owner 新丰博兴聚合材料有限公司
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