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Preparation method of perfluorobutane sulfonic acid p-phenyliodonium salt

A technology of perfluorobutanesulfonic acid and phenyliodonium salt, which is applied in the field of preparation of perfluorobutanesulfonic acid p-phenyliodonium salt, can solve the problems of reducing the cost of photoresists, achieve shortening of reaction time, Low reaction cost and cost reduction effect

Pending Publication Date: 2021-07-23
河北凯诺中星科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant literature report on the synthesis of perfluorobutanesulfonic acid p-phenyliodonium salt, and the development of high-purity perfluorobutanesulfonic acid p-phenyliodonium salt with high atom economy and high yield Photoacid generators for photoresist are imminent, which can reduce the cost of photoresist production

Method used

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  • Preparation method of perfluorobutane sulfonic acid p-phenyliodonium salt
  • Preparation method of perfluorobutane sulfonic acid p-phenyliodonium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add a mixed solution of 398mL toluene and 70mL water as a composite solvent into a 1L four-necked flask equipped with a stirring paddle, a condenser, and a thermometer, start stirring, and add bis[4-(1,1-dimethylethyl)benzene to the system. Base] 156g of bromoiodide salt, slowly add 108g of sodium perfluorobutane sulfonate to the reaction system, raise the temperature to 70°C, keep it warm for 6h, monitor the reaction progress, take samples to detect the reaction is complete, cool down to 0°C ± 2°C, and centrifuge to obtain Wet product of perfluorobutanesulfonic acid p-phenyliodonium salt crude product, under stirring, the crude product passes through a mixed solution of recrystallization solvent 628mL dichloromethane and 70mL water, heats at 25°C for 30min for recrystallization, and cools to 0 After -5°C, the separated solid was dried below 80°C to obtain 200.45 g of solid product. The product yield is 86.19%.

[0032] The final product perfluorobutanesulfonic acid p-...

Embodiment 2

[0045] Add a mixed solution of composite solvent 562mL toluene and 62mL water into a 1L four-neck flask equipped with a stirring paddle, a condenser, and a thermometer, start stirring, and add bis[4-(1,1-dimethylethyl)benzene to the system Base] 156g of bromoiodide salt, slowly add 109g of sodium perfluorobutane sulfonate to the reaction system, raise the temperature to 75°C, keep it warm for 7h, monitor the reaction progress, take samples to detect the reaction is complete, cool down to 0°C ± 2°C, and centrifuge to obtain The wet product of p-phenyliodonium salt of perfluorobutane sulfonate, under stirring, passes through the mixed solution of recrystallization solvent 846.5mL dichloromethane and 83.7mL water, and recrystallizes at 30°C for 30min, cooling After reaching 0-5°C, the separated solid was dried below 80°C to obtain 200.38 g of solid product. The product yield is 86.16%.

Embodiment 3

[0047] Add a mixed solution of 741mL toluene and 39mL water as a composite solvent into a 1L four-neck flask equipped with a stirring paddle, a condenser, and a thermometer, start stirring, and add bis[4-(1,1-dimethylethyl)benzene to the system. Base] 156g of bromoiodide salt, slowly add 110g of sodium perfluorobutane sulfonate to the reaction system, raise the temperature to 80°C, keep it warm for 8h, monitor the reaction progress, take samples to detect the reaction is complete, cool down to 0°C ± 2°C, and centrifuge to obtain The wet product of perfluorobutanesulfonic acid p-phenyliodonium salt crude product, under stirring, the crude product passed through a mixed solution of recrystallization solvent 1070mL dichloromethane and 93mL water, and was recrystallized at 35°C for 30min, and cooled to 0 After -5°C, the separated solid was dried below 80°C to obtain 200.16 g of solid product. The product yield is 86.07%.

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Abstract

The invention relates to a preparation method of perfluorobutane sulfonic acid p-phenyliodonium salt, which comprises the following steps of: (1) dissolving bis[4-(1,1-dimethylethyl)phenyl]bromo-iodized salt and sodium perfluorobutane sulfonate serving as raw materials in a composite solvent, and after the reaction is completed, conducting separating to obtain a crude product of the perfluorobutane sulfonic acid p-phenyliodonium salt; and (2) carrying out recrystallization on the perfluorobutane sulfonic acid p-phenyliodonium salt crude product obtained in the step (1) in a recrystallization solvent to obtain the perfluorobutane sulfonic acid p-phenyliodonium salt. The purity of the product is greater than or equal to 99%, and the reaction yield is greater than or equal to 86%. The process route disclosed by the invention is simple and feasible in operation process and mild and controllable in reaction condition.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of perfluorobutanesulfonic acid p-phenyliodonium salt. Background technique [0002] Electronic chemicals are one of the essential components of the semiconductor field. The most important trade conflict between China and the United States is a technological dispute in the 21st century. It covers everything from artificial intelligence to network equipment, and the most basic battlefield is semiconductors. . Photoresist is the core upstream material of micrographic processing in the field of microelectronic chips and semiconductors. It is the highest point of electronic chemical materials. Its quality and performance are the key factors affecting the performance, yield and reliability of integrated circuits. The acid generator for photoresist is an important material to control its sensitivity to a certain wavelength of light / electron beam / ion b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/06C07C303/32C07C303/44C07C25/18C07C17/392C07C17/35G03F7/004
CPCC07C303/32C07C303/44C07C17/392C07C17/35G03F7/004C07C309/06C07C25/18
Inventor 张琛孙佳伟杜照磊宋扬李石磊
Owner 河北凯诺中星科技有限公司
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