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Preparation method of 2-isopropylthioxanthone

A technology of isopropylthioxanthone and propylphenylthio group is applied in the field of preparation of photoinitiator 2-isopropylthioxanthone, which can solve the problem of high sewage treatment pressure, large amount of concentrated sulfuric acid, and poor product appearance. It can achieve the effect of less environmental pressure, less dosage and cost saving.

Active Publication Date: 2019-06-25
SHANDONG JIURI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

First of all, concentrated sulfuric acid is both a catalyst and a solvent, and the production of water in the reaction process will affect the catalytic effect of concentrated sulfuric acid, so the consumption of concentrated sulfuric acid is very large, a large amount of waste acid is produced, and the sewage treatment pressure is high; secondly, the appearance of the product is not good, the color dim

Method used

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  • Preparation method of 2-isopropylthioxanthone
  • Preparation method of 2-isopropylthioxanthone

Examples

Experimental program
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Embodiment 1

[0032] Embodiment 1: Preparation of 2-(4-cumylthio)benzoic acid

[0033] Heat 120.3g (0.79mol) of o-chlorobenzoic acid, 120g (0.79mol) of 4-isopropylthiophenol, and 68.0g (1.70mol) of sodium hydroxide to 80°C and stir for 0.5 hours, add 520mL of toluene, and heat Reflux for dehydration, after removing 14mL of water. Protect the obtained solution with nitrogen, seal and pressurize at 1 MPa, heat to 210°C, react for 10 hours, cool down, recover toluene from the solvent, adjust the pH of the solution to 2 with dilute hydrochloric acid or dilute sulfuric acid, filter with suction and dry to prepare 204 g of 2-(4-isopropylphenylthio)benzoic acid, melting point 149-151°C.

Embodiment 2

[0034] Embodiment 2: Preparation of 2-isopropylthioxanthone

[0035] Take 136.2g (0.50mol) of 2-(4-isopropylphenylsulfanyl)benzoic acid and dissolve it in 250mL of dichloroethane, and slowly add 125.0g of 98% sulfuric acid (1.25mol) dropwise under a water bath for 30 minutes, slowly Heat up, reflux for dehydration, monitor the reaction according to the amount of separated water by TLC or liquid phase, after the reaction is complete, lower the temperature and add 150mL of water, stir for 30min, let stand for stratification, separate the organic phase, and the acidic water phase for later use. The organic phase was washed with 150 mL of water, and then the solvent was recovered by distillation. The residue was recrystallized with 250 mL of absolute ethanol to obtain 114.5 g of a light yellow solid, namely: 2-isopropylthioxanthone with a content of 99.4%.

Embodiment 3

[0036] Embodiment 3: Preparation of 2-isopropylthioxanthone

[0037] Take 136.2g (0.50mol) of 2-(4-isopropylphenylsulfanyl)benzoic acid and disperse it in 400mL of cyclohexane, slowly add 125.0g of 98% sulfuric acid (1.25mol) dropwise in a water bath, after 30min, slowly heat Heat up, reflux and dehydrate, monitor the reaction according to the amount of separated water by TLC or liquid phase, after the reaction is complete, cool down and add 150mL of water, stir for 30min, let stand for stratification, separate the organic phase, then wash with 150mL of water, and then distill to recover the solvent. The material was recrystallized with 250 mL of absolute ethanol to obtain 115.8 g of a light yellow solid, namely: 2-isopropylthioxanthone, with a content of 99.3%.

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Abstract

The invention relates to a preparation method of a photoinitiator 2-isopropylthioxanthone. The method is concretely characterized in that 2-(4-isopropylthiophenyl)benzoic acid undergoes a ring-closingreaction under a refluxing dehydration condition to prepare the 2-isopropylthioxanthone. The method has the advantages of small use amount of concentrated sulfuric acid, small environmental pressureand good product appearance.

Description

technical field [0001] The invention relates to a preparation method of a photoinitiator 2-isopropylthioxanthone, in particular to the preparation of 2-isopropylthioxanthone by ring-closing reaction of 2-(4-isopropylphenylthio)benzoic acid under reflux dehydration conditions. Propylthioxanthone. Background technique [0002] 2-Isopropylthioxanthone is a high-efficiency free radical type II photoinitiator, suitable for photocurable materials composed of unsaturated polyester and acrylic monomers, and can be used for colorless or colored UV curable inks, wood Furniture, decorative coatings, adhesives, automotive metal parts coatings, optical fiber manufacturing, printed luminescent materials, etc. It acts as a sensitizer when used together with a cationic photoinitiator, and can also be used as a photosensitizer to enhance the curing performance of photoinitiator 907. [0003] According to the difference of raw materials used, at present, the preparation methods of 2-isoprop...

Claims

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Application Information

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IPC IPC(8): C07D335/16
Inventor 吕振波李可毛桂红罗想石智铭张廷付陈波闫云祥张齐
Owner SHANDONG JIURI CHEM TECH CO LTD
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