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Light mitiator of thioxanthone-2-carboxylic ester

A technology of C1-C12 compounds, applied in the field of novel thioxanthone carboxylate and diester derivatives, can solve problems such as danger and violent reaction, and achieve the effect of improving quality

Active Publication Date: 2005-08-31
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of the Journal of East China University of Science and Technology prepares ethyl ester with a yield of 79.9%. The step is to distill out SOCl 2 After adding alcohol directly, the reaction is violent and dangerous

Method used

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  • Light mitiator of thioxanthone-2-carboxylic ester
  • Light mitiator of thioxanthone-2-carboxylic ester
  • Light mitiator of thioxanthone-2-carboxylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Embodiment 1: the preparation of ethyl thioxanthone-2-carboxylate:

[0067] In a 10L four-necked flask equipped with mechanical stirring, add 445g of thioxanthone-2-carboxylic acid and 2500ml of thionyl chloride, heat to reflux, a large amount of hydrogen chloride gas is generated, and continue to reflux for 5 hours. Heating was stopped, and excess thionyl chloride was distilled off. Add 2.5L of anhydrous toluene to dissolve the residue, add 1500ml of absolute ethanol at room temperature, raise the temperature, reflux for 3-4 hours, distill off the ethanol, quickly add 1000ml of saturated potassium carbonate solution under stirring, separate the water phase, and toluene The phase was filtered, and the filtrate was cooled slowly. 325 g of pale yellow needle-like crystals were obtained, and the toluene solution was concentrated for further crystallization to obtain 155 g. The yield was 91%, and the product purity (HPLC) was 98.67%.

Embodiment 2

[0068] Embodiment 2: Thioxanthone-2-carboxylic acid polytetrahydrofuran-250-diester:

[0069] 28.4 grams (0.1ml) of ethyl thioxanthone-2-carboxylate, 12.5 grams (ml) of polytetrahydrofuran (average molecular weight 250) and 0.5 gram of butyl stannic acid, under nitrogen protection, heated at 170°C for 8 hours, cooled at 150°C to reduce Remove ethanol by pressure for about half an hour, after cooling, add 200ml tetrahydrofuran, heat and reflux for one hour, then add a little activated carbon, cool to room temperature, filter to remove catalyst, mother liquor is firstly removed tetrahydrofuran by rotary evaporation, and then dried at 80°C / 1mbar, leaving 36.18 grams of oily matter, productive rate 97%, HPLC proves product purity,

[0070] Elemental analysis: sulfur: calculated value: 8.82% test value: 8.61%

Embodiment 3

[0071] Example 3: Thioxanthone-2-carboxylic acid polyethylene glycol-400-diester:

[0072] The steps of Example 2 were repeated, except that polyethylene glycol-400 was used instead of polytetrahydrofuran-250 to obtain thioxanthone-2-carboxylic acid polyethylene glycol-400-diester.

[0073] Elemental analysis: sulfur: calculated value: 7.23% test value: 7.45%

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PUM

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Abstract

A thioxanthone-2-carboxylate as an optical trigger in the form of liquid used in optical polymerizing process features low extraction performance, low mobility and low volatility, and ca be used for paint and ink. Its preparing process is also disclosed.

Description

technical field [0001] The invention relates to a novel thioxanthone carboxylate and diester derivatives, preparation and use methods. Background technique [0002] Thioxanthone derivatives are considered to be useful intermediates in the fields of medicine (such as in the field of psychotherapy) and fine chemicals. This compound is used as a photoinitiator in the photopolymerization of ethylenically unsaturated monomers. [0003] At present, widely used commercially available thioxanthone derivatives are mainly 2-chlorothioxanthone (CTX) and 2-, a mixture (ITX) of 4-isopropylthioxanthone or a single component, They are crystalline or powder solids, but when using these thioxanthone photoinitiators in the photopolymerization system, it is necessary to dissolve the compound with other polymerizable monomers, or grind the compound to obtain a complete dispersion, which will increase production costs , also produces an unstable solution where undesired polymerization may occu...

Claims

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Application Information

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IPC IPC(8): C07D335/12C08F2/50C08F10/00
Inventor 解敏雨
Owner TIANJIN JIURI NEW MATERIALS CO LTD
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