Method for efficiently and recyclably synthesizing 2,4,6-trimethylbenzoyldiphenyl phosphine oxide

A technology of trimethylbenzoyl and diphenylphosphine oxide, which is applied in chemical instruments and methods, chemical recovery, organic chemistry, etc., can solve the problems of shortening the preparation process, catalysts that cannot be reused, and complicated post-treatment methods. Achieve the effect of simple process, low cost and easy operation

Active Publication Date: 2017-06-23
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has the advantages of low cost, easy operation, and greatly shortens the preparation process, but the catalyst cannot be reused, and the post-treatment method is relatively complicated

Method used

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  • Method for efficiently and recyclably synthesizing 2,4,6-trimethylbenzoyldiphenyl phosphine oxide
  • Method for efficiently and recyclably synthesizing 2,4,6-trimethylbenzoyldiphenyl phosphine oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Will 3.24g V 2 o 5 Solid-phase grinding with 43.55g MCM-41 molecular sieve for 0.5h and roasting to obtain vanadium molecular sieve (V-MCM-41). Add 37.61g of 2,4,6-trimethylbenzaldehyde and 56.17g of diphenylphosphine oxide into a three-necked flask containing 450mL of dichloromethane, stir and react at room temperature for 6 hours, and then put the three-necked flask into a low-temperature water bath Cool to 8-10°C, add 3.23g vanadium molecular sieves (4% vanadium load) and 37mL tert-butanol peroxide in sequence, react at low temperature for 0.5 hours, then place at room temperature for stirring, and react for 5 hours.

[0028] After the reaction is finished, vanadium molecular sieves are recovered by filtration. Add 5% Na to the filtrate 2 S 2 o 3 The aqueous solution neutralized the unreacted tert-butanol peroxide, extracted, collected the organic layer, washed three times with saturated brine, then added anhydrous sodium sulfate to remove water, then recrystall...

Embodiment 2

[0031] 4.17g NH 4 VO 3 Solid phase grinding with 43.55g ZSM-5 molecular sieve for 0.5h and then roasting to obtain vanadium molecular sieve (V-ZSM-5-N). Add 37.61g of 2,4,6-trimethylbenzaldehyde and 56.17g of diphenylphosphine oxide into a three-necked flask containing 450mL of dichloromethane, stir and react at room temperature for 6 hours, and then put the three-necked flask into a low-temperature water bath Cool to 8-10°C, add 3.23g of vanadium molecular sieves (4% vanadium load), 37mL of tert-butanol peroxide, react at low temperature for 0.5 hours, then place at room temperature for stirring, and react for 4 hours.

[0032] After the reaction is finished, vanadium molecular sieves are recovered by filtration. Add 5% Na to the filtrate 2 S 2 o 3 The aqueous solution neutralized the unreacted tert-butanol peroxide, extracted, collected the organic layer, washed three times with saturated brine, then added anhydrous sodium sulfate to remove water, then recrystallized, s...

Embodiment 3

[0035] vanadyl sulfate (VOSO 4 ) to make a 1mol / L solution, mix 35.63mL of the solution with 43.55g of ZSM-5 molecular sieve, stir for 4 hours, and roast to obtain vanadium molecular sieve. Add 37.61g of 2,4,6-trimethylbenzaldehyde and 56.17g of diphenylphosphine oxide into a three-necked flask containing 450mL of dichloromethane and stir, react at room temperature for 6 hours, and then put the three-necked flask into a low-temperature water bath Cool in medium to 8-10°C, add 3.23g vanadium molecular sieve (4% vanadium load) and 37mL tert-butanol peroxide in sequence, react at low temperature for 0.5 hours, then place at room temperature for stirring, and react for 5 hours.

[0036] After the reaction is finished, vanadium molecular sieves are recovered by filtration. Add 5% Na to the filtrate 2 S 2 o 3 The aqueous solution neutralized the unreacted tert-butanol peroxide, extracted, collected the organic layer, washed three times with saturated brine, then added anhydrous ...

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Abstract

The invention discloses a method for efficiently and recyclably synthesizing 2,4,6-trimethylbenzoyldiphenyl phosphine oxide. The method comprises the following steps of a, selecting a vanadium source and a molecular sieve as reaction raw materials to prepare a vanadium molecular sieve catalyst; b, adding 2,4,6-trimethylbenzaldehyde and diphenyl phosphine oxide into a three-opening bottle in which dichloromethane is contained, and stirring at normal temperature to react for 6 hours; c, cooling the three-opening bottle in a low-temperature water bath to 8 to 10 DEG C, sequentially adding the vanadium molecular sieve catalyst and tert-butyl hydroperoxide into the three-opening bottle, stirring to react for 0.5 hour, and continuously stirring at normal temperature for 3 to 5 hours to obtain reaction liquid; and d, filtering the reaction liquid, recycling a vanadium molecular sieve, treating the obtained filtrate by aqueous solution of sodium thiosulfate to remove unreacted oxide, and performing post treatment to obtain a TPO (2,4,6-trimethylbenzoyldiphenyl phosphine oxide) product. As the vanadium molecular sieve serves as the catalyst and is matched with the tert-butyl hydroperoxide to prepare the TPO, the yield of the target product is increased, and the catalyst is environment friendly and recyclable.

Description

technical field [0001] The invention relates to a synthesis process of monoacyl phosphine oxide, in particular to an efficient and recyclable method for synthesizing 2,4,6-trimethylbenzoyl-diphenyl phosphine oxide, which belongs to the technical field of organic synthesis. Background technique [0002] Photoinitiator is a key component of photocurable materials, and its photocuring speed plays a decisive role. A photoinitiator is a substance that can absorb radiation energy, undergo photochemical changes after being excited, and produce active intermediates (free radicals or cations) with the ability to initiate polymerization. Photoinitiators are mainly used for the initiation of monomers in radiation (UV) curing coatings. Since Bayer, Germany, launched the first UV-curing coating product in the late 1960s, the application of UV-curing coating technology has experienced With the rapid development, with people's constant pursuit of high-performance and high-quality products...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
CPCY02P20/584C07F9/5337
Inventor 于青王婷婷赵君静王忠卫
Owner SHANDONG UNIV OF SCI & TECH
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