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Thioxanthone acetylfluorene photoinitiator and preparation method thereof

A kind of technology of thioxanthone acetyl fluorene and photoinitiator

Inactive Publication Date: 2015-02-25
JINYU HENAN PACKAGING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molar absorptivity of the reported thioxanthone-based photoinitiators in the near-ultraviolet region is small, and the initiation effect is not ideal

Method used

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  • Thioxanthone acetylfluorene photoinitiator and preparation method thereof
  • Thioxanthone acetylfluorene photoinitiator and preparation method thereof
  • Thioxanthone acetylfluorene photoinitiator and preparation method thereof

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Effect test

Embodiment 1

[0024] The preparation method of photoinitiator thioxanthone acetylfluorene of the present invention, its detailed steps are as follows:

[0025] A, add 40mL vitriol oil (mass percentage concentration is 98%) in the four-neck flask that agitator, thermometer and condenser tube are housed, add 2.93g (19mmol) thiosalicylic acid under the condition of 20 ℃, stir and dissolve, Then 11.81g (57mmol) of 2-acetyl fluorene was added to the above solution, stirred and reacted at 20°C for 2h; then the reaction system was heated to 75°C for reaction, and the reaction progress was monitored by TLC. After 2h, the reaction was completed to obtain the reaction solution ;

[0026] b. After cooling the reaction solution, pour it into 300mL boiling water and cook for 5min, then slowly add sodium hydroxide to adjust to neutrality; cool and filter, and the obtained filter cake is washed with 80°C hot water (30mL for each washing) to constant weight, and the obtained The crude product was recrysta...

Embodiment 2

[0031] The preparation method of photoinitiator thioxanthone acetylfluorene of the present invention, its detailed steps are as follows:

[0032] A, add 40mL vitriol oil (mass percentage concentration is 98%) in the four-neck flask that stirrer, thermometer and condenser tube are housed, add 2.93g (19mmol) thiosalicylic acid under 10 ℃ of conditions, stir and dissolve, Then 11.81g (57mmol) of 2-acetylfluorene was added to the above solution, stirred and reacted at 10°C for 2h; then the reaction system was heated to 75°C for reaction, and the reaction progress was monitored by TLC. After 1.5h, the reaction was completed to obtain a reaction solution;

[0033] b. After cooling the reaction solution, pour it into 400mL boiling water and cook for 5min, then slowly add sodium hydroxide to adjust to neutrality; cool and filter, and wash the obtained filter cake with hot water at 80°C (30mL each time) to constant weight, and obtain the crude product A mixed solvent of dioxane and wat...

Embodiment 3

[0035] The preparation method of photoinitiator thioxanthone acetylfluorene of the present invention, its detailed steps are as follows:

[0036] A, add 40mL vitriol oil (mass percentage concentration is 98%) in the four-neck flask that stirrer, thermometer and condenser tube are housed, add 2.93g (19mmol) thiosalicylic acid under 10 ℃ of conditions, stir and dissolve, Then 11.81g (57mmol) of 2-acetylfluorene was added to the above solution, stirred and reacted at 10°C for 3h; then the reaction system was heated to 120°C for reaction, and the reaction progress was monitored by TLC. After 1h of reaction, the reaction solution was obtained;

[0037] b. After cooling the reaction solution, pour it into 300mL boiling water and cook for 5min, then slowly add sodium hydroxide to adjust to neutrality; cool and filter, the obtained filter cake is washed with hot water at 80°C (30mL each time) to constant weight, and the obtained crude product Adopt the mixed solvent of dioxane and wat...

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Abstract

The invention discloses a thioxanthone acetylfluorene photoinitiator and a preparation method thereof. The preparation method comprises the following steps: adding a solvent, thiosalicylic acid and 2-acetylfluorene in a reactor, reacting under the condition of heating until the reaction is finished; and cooling reaction liquid obtained after reaction, carrying out aftertreatment including washing and recrystallizing to obtain thioxanthone acetylfluorene. Under the same light condition, the thioxanthone photoinitiator with larger molar absorption coefficient has stronger photo-initiation function. The synthesis method of the thioxanthone acetylfluorene photoinitiator is simple; the thioxanthone acetylfluorene photoinitiator has an absorption platform in a near ultraviolet light region, and has a molar absorption coefficient of 7983L.mol<-1>.cm<-1> at the wavelength of 398nm; as an efficient near ultraviolet photoinitiator, the thioxanthone acetylfluorene photoinitiator can be capable of greatly improving the photo-initiation efficiency and has the beneficial effects of conservation of energy sources and improvement of the output and quality of related products.

Description

1. Technical field: [0001] The invention relates to a photoinitiator and a preparation method thereof, belonging to the field of photochemistry. In particular, it relates to a photoinitiator thioxanthone acetylfluorene and a preparation method thereof. 2. Background technology: [0002] Photocuring technology, also known as photopolymerization technology, has been widely used in many fields such as the preparation of new materials. At the North American Radiation Curing International Conference held in May 2004, it was summarized as an industrial technology with "5E" characteristics: Efficient (high efficiency), Enabling (wide adaptability), Economical (economical), Energy Saving (energy saving) and Environmental Friendly (environmentally friendly). Photoinitiator is an important part of the photocuring system, which generates active groups by absorbing light energy, thereby initiating photopolymerization. Thioxanthone compounds have certain light-absorbing properties, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/48C07D335/04
Inventor 张帅王经武李中灵郑世军李飞王毛力
Owner JINYU HENAN PACKAGING
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