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.
Co-production preparation of monoacylphosphine and bisacylphosphine and oxides thereof
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Paragraph 0058-0060, (2021/11/19)
The invention relates to the field of photocuring functional new material chemicals, discloses co-production preparation of a series of monoacylphosphine and diacylphosphine, and oxides thereof, namely monoacylphosphine oxide and diacylphosphine oxide for the first time, wherein one-pot preparation of the compounds in the same flow process and the same reactor is achieved for the first time. The process technology has the characteristics of outstanding low-cost economic competitiveness and environmental friendliness. The compounds are important olefinic bond (C=C)-containing unsaturated photoinitiator for a radiation polymerization system.
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.
Process for preparation of phosphorane and phosphonyl compounds
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, (2021/06/06)
The invention relates to the field of new materials of fine chemicals, in particular to a new safe, convenient, mild, efficient, environment-friendly and economical preparation process technology of phosphorane and phosphonyl compounds.
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.
Preparation method of bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide
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Page/Page column 6-14, (2020/12/30)
The invention provides a preparation method of bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide, which comprises the following steps of (1) mixing sodium sand, phenylphosphine dichloride and urotropine in a non-polar solvent to react to obtain a reactant, and (2) adding mesitylene formyl chloride into the reactant obtained in the step (1), reacting, and oxidizing to obtain bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide. According to the method, urotropine is used as an activating agent, sodium phenylphosphine can be effectively prevented from being agglomerated to form sodium phenylphosphine polyphosphide, generation of sodium phenylphosphine is promoted, the hydrogen phenylphosphine process is not needed, and the reaction safety is greatly improved; and the preparation process can be realized by only needing a small amount of activating agent, so that the economical efficiency of industrial production is facilitated, the content of organic matters in the wastewater can be reduced, certain environmental benefits are achieved, and the cost is saved.
Preparation method of photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide
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, (2019/10/29)
The invention belongs to the technical field of photoinitiator preparation synthesis, particularly relates to a preparation method of organophosphorus photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide, and provides a preparation method of the phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide. The preparation method is characterized by comprising the steps: phenyl phosphine metallide and CO2 are directly constructed to form phosphenyl phthalate, then carboxyl of the phosphenyl phthalate is subjected to in-situ activation through N,O-dimethylhydroxylamine hydrochloride (DMHA) toprepare Weinreb amide, then a Grignard reagent or an organic lithium reagent of trimethylphenyl is used for attacking, an addition reaction is conducted to obtain a main skeleton, and finally throughoxidation, the phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide is obtained. A process technology route is novel, the raw materials are cheap and easy to obtain, the cost is economical, environmental friendliness is achieved, and compared with an existing process, significant advantages are achieved.
Preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide
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, (2019/10/01)
The invention provides a preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide. The preparation method comprises the following steps: using phenyl phosphorus dichloride as an initial raw material, under the protection of nitrogen, adopting a catalyst (the catalyst is a mixture of potassium tert-butoxide and serine) to replace chlorine with powdery metal sodium, carrying out reduction under a weak alkaline condition, and carrying out condensation and oxidation reaction with 2,4,6-trimethylbenzoyl chloride to prepare a phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide product. The preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide has better catalytic effect and higher yield; and the metal sodium is prepared into powder in a toluene solvent, and all reaction processes are carried out under the protection of nitrogen, so that the safety is high.
Double-benzoyl phenyl phosphine oxide and benzoyl diphenyl phosphine oxide of the preparation method
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, (2019/03/21)
The invention relates to a preparation method of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide used in the technical field of radiation polymerization curing new materials, hydrogen phosphide as a raw material is reacted with chlorobenzene or bromobenzene and 2,4,6-trimethylbenzoyl chloride, and an acyl oxygen phosphonic compound is obtained by oxidizing with an oxidant. By adjusting the feed ratio, the di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and the (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide are respectively obtained, and the purpose for simultaneously producing the two target products of di (2,4,6-trimethylbenzoyl) phenyl phosphine oxide and the (2,4,6-trimethylbenzoyl) diphenyl phosphine oxide can be achieved by use of same material and device, and compared with known technology paths reported in literatures, the preparation method has the significant advantages of novelty of the chemical reaction technology, cost economic competitiveness and environmental friendliness.
( benzoin phosphine oxygen radical ) (are three a phenyl) methanone and ( benzene phosphine oxygen radical ) double (are three a phenyl methanone) method for the preparation of
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Paragraph 0016; 0025; 0026, (2017/04/07)
The invention relates to the technical field of optical radiation free-radical polymerized new materials, especially to a novel synthesis technological process of commercial photoinitiator compounds of (diphenylphosphine oxide)(mesitylene)ketone and (phenylphosphine oxide)bis(mesitylene ketone). According to the invention, 1,3,5-trimethyl-2-(trichloromethyl)-benzene is used as a key raw material and is respectively subjected to a condensation reaction with corresponding organic phosphine precursors so as to prepare the target compounds. In comparison with a known technological route, the technology disclosed in the application has significant advantages such as novelty of the chemical reaction process, economical cost, competitiveness and environmental friendliness.
