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Preparation process of 2-isopropylthioxanthone

A technology of isopropylthioxanthone and p-isopropylthioxanthone is applied in the field of preparation of photoinitiator 2-isopropylthioxanthone, which can solve the problem of many synthesis process steps, high equipment requirements and many equipments. and other problems, to achieve the effect of high reaction yield, high product purity and high production efficiency

Inactive Publication Date: 2009-11-04
江苏省中兴化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, Shanghai Taihe Co., Ltd. uses H2SO4-SO3 as a catalyst, which requires high equipment and produces more sewage
Changzhou Huati chemical synthesis process has many steps, many equipments and low yield

Method used

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  • Preparation process of 2-isopropylthioxanthone
  • Preparation process of 2-isopropylthioxanthone
  • Preparation process of 2-isopropylthioxanthone

Examples

Experimental program
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Effect test

example 1

[0013] Add 76 g of p-isopropyl thiophenol, 82 g of o-chlorobenzoic acid, 66 g of lithium hydroxide containing crystal water, and 150 ml of tetralin into a four-necked flask equipped with a reflux condenser. Separate the water, keep it at 180-190℃ for 6 hours, evaporate the tetralin under reduced pressure, then add 30% hydrochloric acid to neutralize and adjust the pH to 2-3, suction and filter, the filtrate recovers lithium chloride, and the filter cake is dried to obtain 133 Grams.

[0014] Add 270 ml of concentrated sulfuric acid to a dry three-necked flask, stir with ice water to cool to 10°C, and then add 133 g of the dried product in the previous step over 2 hours in batches. After adding and keeping warm for 2 hours, drain into water, add 150ml of toluene, let the layer separate, remove the acid water layer, add water to the oil layer and adjust the PH value to 7-8 with baking soda, divide the water layer, and use after the oil layer is stripped of toluene Recrystallization ...

example 2

[0016] Add 76 g of p-isopropylthiophenol, 75 g of o-chlorobenzoic acid, 66 g of lithium hydroxide containing crystal water, and 150 ml of tetralin into a four-necked flask equipped with a reflux condenser. Separate the water, keep it at 180-190℃ for 6 hours, evaporate the tetralin under reduced pressure, then add 30% hydrochloric acid to neutralize the pH to 2-3, filter with suction, recover the lithium chloride from the filtrate, and dry the filter cake to get 125 Grams.

[0017] Add 270 ml of concentrated sulfuric acid to a dry three-necked flask, stir with ice water to cool to 10°C, and then add 125 g of the dried product in the previous step over 2 hours in batches. After adding and keeping warm for 2 hours, drain into water, add 150ml of toluene, let the layer separate, remove the acid water layer, add water to the oil layer and adjust the PH value to 7-8 with baking soda, divide the water layer, and use after the oil layer is stripped of toluene Recrystallization from 150 ml...

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Abstract

The invention relates to a preparation process of 2-isopropylthioxanthone of light trigger, in particular to a process for preparing 2-isopropylthioxanthone by using 4-isopropylbenzenethiol and 2-chlorobenzoic acid as the main raw material through the reaction steps of condensation, exsolution, neutralization, cyclization, hydrolyzation, recrystallization, and the like. The preparation process is characterized in that the 4-isopropylbenzenethiol and the 2-chlorobenzoic acid are used as the raw materials and are condensed by using tetraline as solvent under the alkaline (lithium hydroxide) condition, the mol ratio of the 4-isopropylbenzenethiol, the 2-chlorobenzoic acid and the lithium hydroxide is 1:1-1.5:2-2.5, and preference for 1:1.05:2.1; the condensation temperature is 180-190 DEG C, the product is prepared by the reaction steps of exsolution, neutralization, cyclization, hydrolyzation, recrystallization, and the like after the reaction is performed for 6h. The invention has easily obtained raw materials, can improve the performability of the process, can greatly lower the production cost because the produced lithium hydroxide of the side product can be sold through the treatment and has high purity of produced products without isomer.

Description

Technical field [0001] The invention relates to a process for preparing a photoinitiator 2-isopropylthioxanthone, in particular to a process that takes p-isopropylthiophenol and o-chlorobenzoic acid as the main raw materials and undergoes condensation, desolvation and neutralization. , Cyclization, hydrolysis, recrystallization and other reaction steps to prepare 2-isopropyl thioxanthone. [0002] Background technique [0003] 2-Isopropyl thioxanthone is a highly efficient free radical type II photoinitiator, used for UV polymerization and curing of corresponding resins and tertiary amine complexing agents. It is generally used in screen printing inks, varnishes, lithographic printing inks, and flexographic printing. Inks, electronic products, wood coatings, etc. [0004] The synthesis of 2-isopropyl thioxanthone by Shanghai Taihe Co., Ltd. is: using dithiosalicylic acid as the raw material, under the catalysis of H2SO4-SO3, the synthesis of 2-isopropyl thioxanthone, the total ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D335/16
Inventor 彭广荣
Owner 江苏省中兴化工有限公司
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