Preparation method of isopropyl thioxanthone

A technology of isopropylthioxanthone and propylphenyl sulfide, which is applied in the field of preparation of isopropylthioxanthone, can solve the problems of high environmental protection treatment cost, reduced product yield, low product purity and the like, and achieves saving Economical cost, reduction of impurities and carbides, high yield

Inactive Publication Date: 2020-02-21
盐城市大丰区天生联合药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing process for preparing ITX is to react under sulfuric acid system. The strong oxidizing property of concentrated sulfuric acid is easy to produce side reactions to bring impurities, and it is easy to carbonize organic matter, and the acid water produced by hydrolysis with sulfuric acid process needs to be neutralized with a large amount of alkali. And, a large amount of waste salt is produced, thereby reducing the product yield, the product purity is low, and the environmental protection treatment cost is high

Method used

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  • Preparation method of isopropyl thioxanthone
  • Preparation method of isopropyl thioxanthone

Examples

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Embodiment 1

[0047] The invention provides a preparation method of isopropylthioxanthone (ITX), comprising the following steps:

[0048] ① The 2-(4-cumyl thio) benzoic acid and polyphosphoric acid are mixed and reacted according to the weight ratio of 1:1.25 to obtain a reaction solution;

[0049] 2. Add the reaction solution obtained in step 1 into water, stir, heat, add liquid caustic soda after removing the lower layer of water, adjust the pH value of the reaction solution, and separate the lower layer of oil layer;

[0050] 3. dehydration and rectification are carried out to the lower oil layer, and a middle distillate is divided, and the divided middle distillate is heated and cooled in a vacuum to obtain a crude oil phase substance;

[0051] ④ Purify the oil phase obtained in step ③ and methanol under certain conditions to obtain crystals;

[0052] ⑤ Dry the crystal obtained in step ④ to obtain isopropylthioxanthone.

[0053] Preferably in the above technical scheme, in the reactio...

Embodiment 2

[0067] In one embodiment, the preparation method of isopropylthioxanthone (ITX) of the present invention comprises the following steps:

[0068] 1. 2-(4-isopropylphenylthio)benzoic acid and polyphosphoric acid are mixed and reacted in a ratio of 1:1.35 by weight to obtain a reaction solution;

[0069] 2. Add the reaction solution obtained in step 1. into water, stir, heat, add liquid caustic soda after removing the lower layer of water, adjust the pH value of the reaction solution, and separate and take the lower layer of oil layer;

[0070] ③ Dehydrating and rectifying the lower oil layer, fractionating the middle distillate, heating and vacuum cooling the fractionated middle distillate to obtain the crude oil phase;

[0071] ④ refining the oil phase obtained in step ③ with methanol under certain conditions to obtain crystals;

[0072] ⑤ drying the crystals obtained in step ④ to obtain isopropylthioxanthone.

[0073] Preferably in the above technical scheme, in the reaction...

Embodiment 3

[0087] In one embodiment, the preparation method of isopropylthioxanthone (ITX) of the present invention comprises the following steps:

[0088] 1. 2-(4-isopropylphenylthio)benzoic acid and polyphosphoric acid are mixed and reacted in a ratio of 1:1.45 by weight to obtain a reaction solution;

[0089] 2. Add the reaction solution obtained in step 1. into water, stir, heat, add liquid caustic soda after removing the lower layer of water, adjust the pH value of the reaction solution, and separate and take the lower layer of oil layer;

[0090] ③ Dehydrating and rectifying the lower oil layer, fractionating the middle distillate, heating and vacuum cooling the fractionated middle distillate to obtain the crude oil phase;

[0091] ④ refining the oil phase obtained in step ③ with methanol under certain conditions to obtain crystals;

[0092] ⑤ drying the crystals obtained in step ④ to obtain isopropylthioxanthone.

[0093] Preferably in the above technical scheme, in the reaction...

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Abstract

The invention provides a preparation method of isopropyl thioxanthone. The preparation method includes: taking 2-(4-isopropylphenylthio)benzoic acid (ITX-acid) as the raw material, carrying out dehydration ring closing in a polyphosphoric acid system, and performing treatment to obtain isopropyl thioxanthone (ITX), and dehydrating the separated phosphoric acid for further use in next preparation procedure. Compared with the prior art, the ITX prepared by the method provided by the invention has better quality, the consumed materials are few, the subsequent waste treatment links are correspondingly simpler, also the wastewater in the reaction can be utilized to generate polyphosphoric acid for recycling in next ITX-acid cyclization reaction, the raw materials are saved, and the cost investment is reduced.

Description

technical field [0001] The invention relates to the field of photoinitiators, in particular to a preparation method of isopropylthioxanthone (ITX). Background technique [0002] Photoinitiators are key materials that absorb the energy of UV radiation light sources to generate active radicals or cationic acids and other polymerization initiating species. Therefore, there is a continuous technical demand in the industry to develop and industrialize new photoinitiator substances that can cope with Performance improvement, low-cost economic competitiveness, ease of use, and environmental and health-friendly application requirements, while isopropylthioxanthone (ITX) is used as a photoinitiator for UV-curable coatings, and its application value is also it goes without saying. [0003] The existing technology of preparing ITX is to react under the sulfuric acid system, the strong oxidizing property of concentrated sulfuric acid is easy to produce side reactions to bring impuritie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D335/16
CPCC07D335/16
Inventor 陈隽楼彭广荣陈玉庆朱晓波
Owner 盐城市大丰区天生联合药业有限公司
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