Cation photoinitiator 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate preparation method

A cationic photoinitiation and isobutylphenyl technology, which is applied in the preparation of halogenated hydrocarbons, chemical instruments and methods, organic chemistry, etc., can solve the problems of trifluoromethanesulfonic acid, such as strong corrosion, high price, and miscellaneous reaction products. , to achieve the effect of convenient preparation and purification, easy purification and convenient separation

Inactive Publication Date: 2015-05-20
上海予利生物科技股份有限公司
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Problems solved by technology

[0014] Method 1: The reaction product of Beringer synthesis method is relatively miscellaneous, and there are certain difficulties in separation and purification, while method 2: Widdowson synthesis method uses phenylboronic acid compound, which is relatively expensive, and trifluoromethanesulfonic acid is relatively corrosive, and the operation risk is high

Method used

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  • Cation photoinitiator 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate preparation method
  • Cation photoinitiator 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate preparation method
  • Cation photoinitiator 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) the preparation of p-methyliodobenzene diacetate comprises the following steps:

[0027] In a 5L reaction flask, add 750 grams (3.45mol) of p-methyl iodobenzene and start to drop 1800 milliliters of 35% peracetic acid at room temperature, add it in about 3 hours, heat it to 35-40 degrees, and then keep it warm at 40 React at -45°C for 12 hours, then cool to room temperature, and p-methyliodobenzene diacetate precipitates as light yellow powder, yielding 695 g, yield 60%.

[0028] (2) The preparation of 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonate comprises the following steps:

[0029] Add 33.6 g (0.1 mol) of p-methyliodobenzene diacetate to 300 ml of trifluoroethanol, stir and dissolve at room temperature, then add 51.6 g (0.3 mol) of p-toluenesulfonic acid, keep the reaction temperature at room temperature, and react for 1-2 hours. Add 39.9 g (0.3 mol) of isobutylbenzene and continue to react at room temperature for 4-24 hours. After concentrating ...

Embodiment 2

[0033] (1) The preparation of 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonate, the method may further comprise the steps:

[0034] Add 504 grams (1.5 mol) of p-methyliodobenzene diacetate to 1800 milliliters of trifluoroethanol, stir and dissolve at room temperature, then add 516 grams (3 mol) of p-toluenesulfonic acid, and keep the reaction temperature at room temperature. After reacting for 1-2 hours, add 300 g (2.25 mol) of isobutylbenzene and then continue to react at room temperature for 4-24 hours. After concentrating and recovering trifluoroethanol, add petroleum ether to crystallize to obtain 620 g, yield 78.9%, white powder.

[0035] (2) The preparation of 4-isobutylphenyl-4'-methylphenyliodonium hexafluorophosphate, the method may further comprise the steps:

[0036] 52.3 grams (0.1mol) of 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonate, add 1000 ml of acetone, then add 22.1 grams (0.12mol) of potassium hexafluorophosphate at room temperature,...

Embodiment 3

[0038] (1) The preparation of 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonate, the method may further comprise the steps:

[0039] Add 336 grams (1 mol) of p-methyliodobenzene diacetate to 1008 milliliters of trifluoroethanol, stir and dissolve at room temperature, then add 172 grams (1 mol) of p-toluenesulfonic acid, and keep the reaction temperature at room temperature. After reacting for 1-2 hours, add iso 133 grams (1mol) of butylbenzene, then continue to react at room temperature for 4-24 hours, concentrate and recover trifluoroethanol, add petroleum ether to crystallize to obtain 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonic acid Salt.

[0040] (2) The preparation of 4-isobutylphenyl-4'-methylphenyliodonium hexafluorophosphate, the method may further comprise the steps:

[0041] 52.3 grams (0.1mol) of 4-isobutylphenyl-4'-methylphenyliodonium p-toluenesulfonate, add 1000 ml of acetone, then add 22.1 grams (0.12mol) of potassium hexafluorophosphat...

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Abstract

The present invention relates to a cation photoinitiator 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate preparation method. According to the preparation method, in a solvent, p-iodotoluene diacetate and isobutyl benzene are subjected to a one-step reaction in the presence of p-toluene sulfonic acid, wherein the reaction temperature is a room temperature, and the reaction time is 4-24 h; concentration is performed after completing the reaction so as to remove the solvent; petroleum ether is added to crystallize to obtain the 4-isopropylphenyl-4'-methylphenyl iodonium p-toluene sulfonate; and finally the 4-isopropylphenyl-4'-methylphenyl iodonium p-toluene sulfonate and potassium hexafluorophosphate are subjected to ion exchange to obtain the product. Compared with the technology in the prior art, the preparation method of the present invention has characteristics of reasonable process, simple operation, and safe production, is suitable for industrial mass production, and provides favorable conditions for industrial production of the 4-isobutylphenyl-4'-methylphenyl iodonium hexafluorophosphate.

Description

technical field [0001] The invention relates to a preparation method of cationic photoinitiator asymmetric diaromatic hydrocarbon iodonium salt, in particular to a preparation method of 4-isobutylphenyl-4'-methylphenyliodonium hexafluorophosphate. Background technique [0002] Radiation curing is a process in which chemical formulations (coatings, inks and adhesives) are converted from liquid to solid by irradiation with energy. The most commonly used radiation curing is ultraviolet (UV) photocuring. Photoinitiator is one of the important components in the photocuring system, which plays a decisive role in the curing rate. After the photoinitiator is irradiated by ultraviolet light, it absorbs the energy of light, splits into two active free radicals, triggers the chain polymerization of the photosensitive resin and the reactive diluent, and makes the adhesive cross-linked and cured. It is characterized by rapidity, environmental protection, and energy saving. According to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/18C07C17/35C07C17/12
Inventor 严承飞俞建新顾建良
Owner 上海予利生物科技股份有限公司
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