162881-26-7Relevant articles and documents
A simple straightforward synthesis of phenylphosphane and the photoinitiator bis(mesitoyl)phenylphosphane oxide (IRGACURE 819)
Gruetzmacher, Hansjoerg,Geier, Jens,Stein, Daniel,Ott, Timo,Schoenberg, Hartmut,Sommerlade, Reinhard H.,Boulmaaz, Souad,Wolf, Jean-Pierre,Murer, Peter,Ulrich, Thomas
, p. 18 - 22 (2008)
A straightforward high-yield synthesis for the photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphane oxide (16, IRGACURE 819) involves: i) the reaction of phenyldichlorophosphane, PhPCl2, with sodium to give [Na2(P2Ph2)(tmeda)]6 (5); ii) protonation of 5 with tert-butanol to give 1,2-diphenyldiphosphane, PhHP-PHPh (12); iii) reduction of 12 by sodium to yield [Na(PHPh)x (13); iv) protonation of 13 with tert-butanol to give phenylphosphane PhPH2 (14) in excellent yields; v) reaction of 14 with 2,4,6-trimethylbenzoylchloride (MesCOCI) in presence of the NaOt-Bu formed in steps ii and iv to give bis(2,4,6-trimethylbenzoyl)phenylphosphane 7; vi) oxygenation of 7 with 30% aqueous hydrogen peroxide to give the final product 16. This reaction can be performed in toluene with about 4 vol-% of tmeda as an activator in a one-pot synthesis without changing the solvent. The structures determined by X-ray diffraction of the unique hexameric aggregate 5 and 16 are reported. Schweizerische Chemische Gesellschaft.
Preparation method of photoinitiator
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Paragraph 0053-0060, (2021/03/24)
The invention provides a preparation method of a photoinitiator phenyl bis(2, 4, 6-trimethylbenzoyl) phosphine oxide, which is characterized by comprising the following steps of (1) reacting water serving as a solvent, phenyl phosphine oxide and 2, 4, 6-trimethylbenzaldehyde serving as raw materials and tert-butyl alcohol salt and pyridinium serving as catalysts to obtain an intermediate compoundshown as a formula I, wherein the equation is as described in the specification, (2) oxidizing the formula I under the action of an oxidizing agent to obtain the target product photoinitiator phenyl bis(2, 4, 6-trimethylbenzoyl) phosphine oxide, wherein the equation is as described in the specification. Tert-butyl alcohol salt and pyridinium are used as catalysts, and the pyridinium has the effectof a phase transfer catalyst, therefore, water can be directly used as a reaction solvent, the use of an organic solvent with toxicity and relatively high price is avoided, and compared with the prior art, the method is more economical and environment-friendly.
Preparation method of bis(2,4,6-trimethylbenzoyl)phenyl phosphine oxide
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Paragraph 0100-0102; 0107-0109; 0115-0117; 0122-0193, (2021/01/11)
The invention provides a preparation method of bis (2,4,6-trimethylbenzoyl)phenyl phosphine oxide, which comprises the following steps: adding a specific ether compound as a complexing agent in the reaction of sodium sand and phenyl phosphine dichloride, and adding the complexing agent to effectively inhibit the formation of phenyl phosphine sodium polyphosphide and promote the generation of phenyl phosphine sodium; a phenyl phosphine hydrogen process is not needed, so that the process cost is reduced, and the safety of the process is improved; besides, the complexing agent is a polar aproticsolvent, is low in dosage, can reduce the content of organic matters in the wastewater compared with a traditional method adopting a protic solvent as an activating agent or a proton source, has certain environmental benefits and saves the cost.
