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Method for synthesizing 4,4-didetergent alkylate iodonium hexafluoro antimonate

A technology of didodecylbenzene and hexafluoroantimonate, which can be used in antimony organic compounds, chemical instruments and methods, preparation of halogenated hydrocarbons, etc., can solve problems such as toxic cations

Inactive Publication Date: 2010-01-06
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Since iodonium salt is insoluble in non-polar solvents, the photopolymerization system using it as an initiator must use a polar solvent to dissolve the monomer, and its cation is poisonous, which limits its application to a large extent.

Method used

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  • Method for synthesizing 4,4-didetergent alkylate iodonium hexafluoro antimonate
  • Method for synthesizing 4,4-didetergent alkylate iodonium hexafluoro antimonate
  • Method for synthesizing 4,4-didetergent alkylate iodonium hexafluoro antimonate

Examples

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example 1

[0030] 1. Preparation of 4,4'-Didodecylphenyliodonium Hydrochloride

[0031] Take 20mL of dodecylbenzene and 20mL of acetic anhydride into a 250mL three-necked reaction flask equipped with a thermometer and an electric stirrer, cool to -5°C at low temperature, then add 20g of potassium iodate, and add 14mL dropwise under stirring. For the mixture of 98% concentrated sulfuric acid and 20mL acetic anhydride, the rate of addition should be kept at a temperature not exceeding -5°C. After the dropwise addition, the reaction temperature rises to room temperature, and the reaction is continued for 8 hours, and then 40mL is added dropwise at a temperature lower than 5°C. Distilled water, standing for stratification, extracting the water layer twice with 20mL toluene, combining the organic layers, adding 10g of barium chloride aqueous solution to the combined toluene solution, a large amount of white precipitates precipitated, filtered, washed with water, and dried the filtrate to obtai...

example 2

[0035] 1. Preparation of 4,4'-Didodecylphenyliodonium Hydrochloride

[0036] Take 100g of dodecylbenzene and 200mL of acetic anhydride into a 500mL three-necked reaction flask equipped with a thermometer and an electric stirrer, cool down to 10--5°C, then add 40g of potassium iodate, and add 60mL dropwise under stirring Concentrated sulfuric acid with a concentration of 98%, the rate of addition should keep the temperature not exceeding -5°C. After the dropwise addition, the reaction temperature rises to room temperature, and the reaction is continued for 5 hours; Separate the layers, extract the water layer twice with 100mL ether, combine the organic layers, add 50g barium chloride aqueous solution to the combined ether solution, a large amount of white precipitate precipitates, filter, wash with water, and dry the filtrate to obtain 4,4'-bis Dodecylphenyliodonium hydrochloride was then recrystallized from anhydrous isopropanol to obtain a white solid with a melting point of ...

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Abstract

The present invention relates to a synthesizing method for 4,4 double hexabromocyclododecane alkyl benzene iodine fluorin antimonite, which is made with the following steps: (1) 4,4 double hexabromocyclododecane alkyl benzene iodine is prepared by the reaction with barium chloride under the function of vitriol taking detergent alkylate and potassium iodate as the material, and acetic anhydride as the solution; (2) 4,4 double hexabromocyclododecane alkyl benzene iodine fluorin antimonite is prepared by the ion reaction between 4,4 double hexabromocyclododecane alkyl benzene iodine and fluorin potassium metaantimonate in cyclohexane, chloroform or dichloroethane solution agent. The 4,4 double hexabromocyclododecane alkyl benzene iodine fluorin antimonite synthesized by the present invention has much better solidified performance to the resin.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and relates to a synthesis method of a cationic photoinitiator, in particular to a synthesis method of 4,4'-didodecylphenyliodonium hexafluoroantimonate. Background technique [0002] With people's general attention to environmental protection, traditional curing is greatly restricted because it needs to use more volatile organic solvents that pollute the environment. Photocuring is widely used for its remarkable advantages such as low curing temperature, fast curing speed, and low pollution. favor. As one of the main components of photocuring composition, photoinitiator has naturally become a hotter research object. In the mid-1970s, Crivello and Lam of General Electric Company reported the research and application of diaryliodonium salts as cationic photoinitiators, which immediately attracted people's attention and were soon commercialized. Diaryliodonium salt not only inh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/92C07C17/093C07C25/18
Inventor 刘安昌肖庆谭珍友刘芳
Owner WUHAN INSTITUTE OF TECHNOLOGY
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