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Polymerizable photoinitiator, preparation method and applications thereof

A polymerization photoinitiator and reaction technology, which is applied in the field of photopolymerization, can solve the problems of macromolecular initiator movement ability and system compatibility, and the influence of dosage on product performance, and achieve simple and efficient preparation methods, high energy transfer efficiency, and easy operation. simple effect

Active Publication Date: 2020-05-01
FUYANG XINYIHUA MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the kinetic ability and system compatibility of macromolecular initiators are relatively poor, and a large amount will affect product performance.

Method used

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  • Polymerizable photoinitiator, preparation method and applications thereof
  • Polymerizable photoinitiator, preparation method and applications thereof
  • Polymerizable photoinitiator, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In this embodiment, the preparation method of compound a is provided:

[0036]

[0037] The preparation method comprises the following steps:

[0038] (1) Slowly add 0.01mol thiosalicylic acid to 0.09mol concentrated sulfuric acid, stir well, then add 0.05mol aniline in batches, stir mechanically, react at room temperature for 1 hour, raise the temperature to 80°C for 3 hours, pour the reactant into boiling water , boiled for 15 minutes, filtered with suction, and recrystallized with a mixed solution of ethanol and water (the volume ratio of ethanol and water was 4:1) to obtain the product.

[0039] (2) Add 0.0078 mol of the above product into 50 ml of tetrahydrofuran for dissolution, then add 0.0234 mol of glycidyl methacrylate, add 0.001 mol of anhydrous potassium carbonate to provide alkaline conditions, react at 70 ° C for 5 hours, and remove the solvent by rotary evaporation to obtain target product. The appearance of the hydroxyl peak of the product was obser...

Embodiment 2

[0041] In this example, the preparation method of compound b is provided:

[0042]

[0043] The preparation method comprises the following steps:

[0044](1) Slowly add 0.01mol thiosalicylic acid into 0.10mol concentrated sulfuric acid, stir well, then add 0.06mol benzylamine in batches, stir mechanically, react at room temperature for 1h, raise the temperature to 80°C for 3h, pour the reactant Pour into boiling water, boil for 15 minutes, filter with suction, and recrystallize with a mixed solution of ethanol and water (the volume ratio of ethanol and water is 4:1) to obtain the product.

[0045] (2) Add 0.0082 mol of the above product into 50 ml of tetrahydrofuran for dissolution, then add 0.0164 mol of glycidyl methacrylate, add 0.001 mol of anhydrous potassium carbonate to provide alkaline conditions, react at 70 ° C for 5 hours, and remove the solvent by rotary evaporation to obtain target product. The appearance of the hydroxyl peak of the product was observed by in...

Embodiment 3

[0047] In this embodiment, the preparation method of compound c is provided:

[0048]

[0049] The preparation method comprises the following steps:

[0050] (1) Slowly add 0.01mol thiosalicylic acid into 0.09mol concentrated sulfuric acid, stir well, then add 0.04mol p-benzylamine in batches, stir mechanically, react at room temperature for 1 hour, heat up to 80°C for 3 hours, and dissolve the reactant Pour into boiling water, boil for 15 minutes, filter with suction, and recrystallize with a mixed solution of ethanol and water (the volume ratio of ethanol and water is 4:1) to obtain the product.

[0051] (2) Add 0.0081 mol of the above-mentioned product to 50 ml of tetrahydrofuran for dissolution, then add 0.0162 mol of glycidyl methacrylate, add 0.001 mol of anhydrous potassium carbonate to provide alkaline conditions, react at 70 ° C for 5 hours, and remove the solvent by rotary evaporation to obtain target product. The appearance of the hydroxyl peak of the product w...

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Abstract

The invention provides a polymerizable photoinitiator, a preparation method and applications thereof, wherein the polymerizable photoinitiator has a structure represented by a formula I. According tothe invention, the molecular structure of the polymerizable photoinitiator contains a photoinitiator thioxanthone and an auxiliary initiator amine, so that intermolecular energy transfer is convertedinto intramolecular energy transfer so as to achieve high initiation efficiency; the molecular structure contains polymerizable acryloyloxy double bonds at the same time, so that the advantages of lowconsumption of the micromolecular photoinitiator and high initiation efficiency are retained, the advantage that the macromolecular photoinitiator is not easy to migrate is achieved, and the method has the advantages of readily available preparation raw materials, few reaction steps and simple operation, does not involve toxic raw materials such as halogen compounds and the like, and meets the requirements of industrialization and green chemistry.

Description

technical field [0001] The invention belongs to the technical field of photopolymerization, and relates to a polymerizable photoinitiator, a preparation method and application thereof. Background technique [0002] Photopolymerization is a technology that uses ultraviolet light to trigger the rapid transformation of reactive liquid substances into solid substances. It has the advantages of energy saving, environmental protection and high efficiency. Photoinitiators play an important role in photocuring technology. They can absorb energy of specific wavelengths to generate active species and initiate system polymerization. Free radical photoinitiators are divided into cleavage type and hydrogen abstraction type photoinitiators, and the hydrogen abstraction type needs to provide amine compounds as co-initiators when used. During the photocuring process, the photoinitiator decomposes to produce many small molecular photolytic fragments, which will migrate to the surface and e...

Claims

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Application Information

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IPC IPC(8): C08F2/48C07D335/16
CPCC08F2/48C07D335/16
Inventor 相可创王雪岚
Owner FUYANG XINYIHUA MATERIAL TECH
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