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Synthetic method of mixed sulfonium salt

A synthesis method and technology of sulfonium salts, which are applied in the synthesis of mixed sulfonium salts and the field of sulfonium salt photoinitiators, can solve the problems of poor solubility, poor photosensitivity, and low yield, and achieve improved safety performance Effect

Pending Publication Date: 2021-09-03
泰兴先先化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to overcome the problems of low yield, poor solubility, and poor photosensitivity in the above-mentioned prior art, the present invention provides a mixed-type sulfonium salt and a synthesis method to realize one-step synthesis of monosulfonium salt and bissulfonium salt with arbitrarily set ratios. mixed sulfonium salt

Method used

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  • Synthetic method of mixed sulfonium salt
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  • Synthetic method of mixed sulfonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 1. Put 372g of aluminum trichloride, 50g of benzene, and 130g of diphenyl sulfide into the flask in sequence, and control the internal temperature to 28°C.

[0021] 2. Add a total of 282 g of diphenyl sulfoxide to the flask in batches at a rate of 1 g every 2 minutes. After the feeding is completed, keep the temperature at 25°C for 8 hours, and after the reaction is completed, aluminum trichloride is hydrolyzed, washed with water, and separated into layers;

[0022] 3. The organic layer was exchanged by adding 800g of dichloromethane and 170g of potassium hexafluorophosphate. After the exchange, it was washed with water, distilled and crystallized with methanol, and dried to obtain a mixed sulfonium salt; HPLC detection showed that the molar ratio of single and double salts was 45.3:54.4, and the yield 94.5%.

Embodiment 2

[0024] 1. Put 307g of aluminum trichloride, 60g of benzene, and 150g of diphenyl sulfide into the flask in sequence, and control the internal temperature to 28°C.

[0025] 2. Add a total of 232 g of diphenyl sulfoxide to the flask in batches at a rate of 1 g every 2 minutes, and the addition is completed in about 7.5 hours. After the feeding is completed, keep the temperature at 25°C for 8 hours, and after the reaction is completed, aluminum trichloride is hydrolyzed, washed with water, and separated into layers;

[0026] 3. The organic layer was exchanged by adding 920g of dichloromethane and 198g of potassium hexafluorophosphate. After the exchange, it was washed with water, distilled and crystallized with methanol, and dried to obtain a mixed sulfonium salt; HPLC detection showed that the molar ratio of single and double salts was 70.4:29.2, and the yield 95.3%.

Embodiment 3

[0028] 1. Put 311g of aluminum trichloride, 70g of benzene, and 163g of diphenyl sulfide into the flask in sequence, and control the internal temperature to 26°C.

[0029] 2. Add a total of 236 g of diphenyl sulfoxide to the flask in batches at a rate of 1 g every 2 minutes, and the addition will be completed in about 8 hours. After the feeding is completed, keep the temperature at 25°C for 8 hours, and after the reaction is completed, aluminum trichloride is hydrolyzed, washed with water, and separated into layers;

[0030] 3. The organic layer was exchanged by adding 960g of dichloromethane and 202g of potassium hexafluorophosphate. After the exchange, it was washed with water, distilled and crystallized with methanol, and dried to obtain a mixed sulfonium salt; HPLC detection showed that the molar ratio of single and double salts was 74.4:24.8, and the yield 93.6%.

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Abstract

The invention discloses a synthetic method of a mixed sulfonium salt. According to the method, substituted diphenyl sulfide and substituted diphenyl sulfoxide are used as main raw materials, aluminum trichloride is used as a catalyst, the high-purity mixed sulfonium salt is prepared by controlling the feeding proportion, the feeding mode, solvent selection, the reaction temperature, the reaction time and the like, the total content of single salt and double salt reaches 99.0% or above, and the proportion of any single salt and double salt can be controlled. Compared with a traditional chlorine gas introduction process, the total effective components are obviously increased, the proportion of single salt and double salt is more controllable, and the used raw materials are safer. The controllability of product components is improved, so that the requirements of different formulas are met.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, relates to a sulfonium salt photoinitiator, and specifically provides a method for synthesizing a mixed type sulfonium salt. Background technique [0002] Sulfonium salt compounds include monosulfonium salts and disulfonium salts, which are substances that generate acids when irradiated by energy rays, and are mainly used as photoacid generators in resist compositions for photolithography, and photo-shaping Cationic polymerization initiators and the like in photopolymerizable compositions such as paints, coatings, and adhesives are used. As a class of commonly used cationic photoinitiators, sulfonium salt compounds have the advantages of small shrinkage of cured coating and good adhesion after application, and compared with diaryliodonium salts, their solubility, storage stability and composition The thermal stability of the film has been improved to a certain extent. Mixed sulfonium ...

Claims

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Application Information

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IPC IPC(8): C07C381/12
CPCC07C381/12
Inventor 朱文斌王兵王丽娟
Owner 泰兴先先化工有限公司
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