cas 75980-60-8, Diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide

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Effective Catalyst for Oxidation Synthesis of 2,4,6-Trimethylbenzoyldipenylphosphine Oxide: V/MCM-41
Abstract: 2,4,6-Trimethylbenzoyldipenylphosphine oxide (TPO) is an important photoinitiator, nevertheless some drawbacks exist in its synthesis. So V/MCM-41 catalysts were designed. Compared with commonly used VO(acac)2, V/MCM-41 catalysts exhi
Wang, Tingting,Wang, Zhiming,Zhao, Junjing,Yu, Qing,Wang, Zhongwei
p. 953 - 957
(2018)
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High performance liquid phase continuous automatic production and co-production technology of organic phosphine compound
The invention relates to the field of photocuring functional new material chemicals, and discloses a high performance liquid phase streamline type continuous automatic production technology of an acylphosphine oxide organic phosphine compound for the first time, which not only can produce a single specific target product, but also can co-produce a product mixture of two or more than two of the products of the type. The process technology has outstanding low-cost economic competitiveness and environment-friendly characteristics for large-scale manufacturing of target products. The target product comprises sym-trimethylbenzoyl diphenyl phosphine oxide (also known as 2, 4, 6-trimethylbenzoyl diphenyl phosphine oxide, trade name TPO), sym-trimethylbenzoyl phenyl ethyl phosphonate (trade name TPO-L) and structural analogues thereof, and a mixture of the sym-trimethylbenzoyl diphenyl phosphine oxide and the sym-trimethylbenzoyl phenyl ethyl phosphonate. The organic phosphine compound is an olefinic bond-containing (C=C) unsaturated radiation polymerization system photoinitiator and/or flame retardant and the like with wide application.
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(2021/05/12)

Palladium-catalyzed C–P bond activation of aroyl phosphine oxides without the adjacent “anchoring atom”
A novel palladium-catalyzed decarbonylation of aroyl phosphine oxides to prepare phosphine oxides from carboxylic acids is developed. Without the adjacent “anchoring atom”, the challenging C–P bond activation is achieved in high selectivity. The disclosure of this reaction provides a new example of C–P bond activation and helps to extend the understanding of the property of C–P bond.
Chen, Xingyu,Liu, Xiaoyan,Zhu, Hong,Wang, Zhiqian
(2021/01/14)

Preparation method of methyl substituted benzaldehyde
The invention relates to a preparation method of methyl substituted benzaldehyde, in particular to a method for preparing alkyl aromatic aldehyde through a carbonylation reaction by adopting methyl substituted aromatic hydrocarbon as raw materials. According to the method, ionic liquid with the high catalytic activity is adopted, and methyl substituted benzene is used for preparing the methyl substituted benzaldehyde under the alleviated condition with high conversion rate; meanwhile, the reaction time is shortened, waste water, gas and industrial residues are reduced, and no auxiliaries withhigh corrosivity are adopted.
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Paragraph 0064-0066

(2021/03/06)

Process for preparation of phosphorane and phosphonyl compounds
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.
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Paragraph 0031-0033

(2021/06/06)

Method for catalytically synthesizing benzoyl phosphine oxide compound
The invention discloses a method for catalytically synthesizing a benzoyl phosphine oxide compound, and belongs to the technical field of chemical engineering. According to the method, trimethylchlorosilane is taken as a catalyst, a halogen-containing compound is taken as a cocatalyst, reaction of a phosphine oxide compound and 2, 4, 6-trimethylbenzoyl chloride is realized in a proper solvent at a certain temperature, and the benzoyl phosphine oxide compound (represented by 2, 4, 6-trimethylbenzoyl diphenyl phosphine oxide (TPO for short) is prepared with high selectivity. The process has the characteristics of mild reaction conditions and high quality of the prepared product. The method does not involve a violent oxidation process, does not generate toxic waste gas, is simple and convenient to operate in the whole process, is environment-friendly and is particularly suitable for industrial mass production.
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Paragraph 0039-0040; 0043-0050

(2021/06/12)

Co-production preparation of monoacylphosphine and bisacylphosphine and oxides thereof
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.
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Paragraph 0056; 0057

(2021/11/19)

Conversion of α‐hydroxy(2,4,6‐trimethylbenzyl)diphenylphosphine oxide to TPO: oxidation vs decomposition
This study details the oxidation of α-hydroxy(2,4,6-trimethylbenzyl)diphenylphosphine oxide (α-HDPO) to diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO) by choosing the proper MnO2 as oxidant. In addition, the equilibrium of α-HDPO and 2,4
Zhang, Jian-Qiu,Zhao, Jingzhuo,Li, Chunya,Ye, Jingjing,Han, Li-Biao
p. 207 - 210
(2020/12/15)

Condensation of s-trimethyltrihalomethyl benzene and diphenylphosphine oxide for preparation of organic phosphine compound
The invention relates to the field of photocuring functional new material chemicals. A 'one-pot' direct condensation reaction between s-trimethyltrihalomethyl benzene (also known as '2, 4, 6-trimethyl-1-trihalomethyl-benzene') and diphenylphosphine oxide is disclosed for the first time, and s-trimethylbenzoyl diphenyl phosphine oxide (also known as '2, 4, 6-trimethylbenzoyl diphenyl phosphine oxide') is efficiently prepared by using the reaction process technology. The process technology has the characteristics of outstanding low-cost economic competitiveness and environmental friendliness. The compound is an olefinic bond (C = C)-containing unsaturated radiation polymerizable system photoinitiator with wide application.
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Paragraph 0026-0027; 0032-0033

(2020/05/14)

Chlorosilane-Catalyzed Coupling of Hydrogen Phosphine Oxides with Acyl Chlorides Generating Acylphosphine Oxides
We report a new method for the synthesis of acylphosphine oxides by the direct coupling of hydrogen phosphine oxides and acyl chlorides mediated by chlorosilanes. This new protocol is greener and safer, because it precludes the generation of volatile haloalkanes and the use of oxidants employed in the conventional methods. Moreover, moisture-unstable acylphosphine oxides that are difficult to prepare via the conventional methods can be generated using this new method.
Zhang, Jian-Qiu,Han, Li-Biao
supporting information
p. 4633 - 4637
(2020/06/23)

Method for preparing photoinitiator, namely TPO and simultaneously preparing byproduct, namely benzyl chloride
The invention provides a method for preparing a photoinitiator, namely TPO and simultaneously preparing a byproduct, namely benzyl chloride. The method provided by the invention avoids the problem ofrecovery of a large amount of organic waste gas, namely chloroethane and the like in production of the TPO, and also avoids the problem of serious pollution caused by a large amount of the byproduct,namely chlorine in production of the benzyl chloride. The benzyl chloride is an important chemical raw material for preparing a photoinitiator 369, so the method disclosed by the invention greatly reduces the production cost. Meanwhile, the whole process is low in preparation cost, simple in operation process, safe and easily-controllable in reaction process and easy to realize large-scale production.
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Paragraph 0021-0027

(2020/06/02)

New preparation method of first-class phenyl phosphine oxide initiator
The invention provides a new preparation method of a first-class phenyl phosphine oxide initiator. The method comprises the steps that (1) benzene and aluminum trichloride are added into a reaction vessel and stirred uniformly, then phosphorus trichloride is added, the temperature is slowly increased, and after a complete reaction, the temperature is reduced to room temperature; (2) a reaction mixture obtained in the step (1) is slowly added dropwise into a solvent containing a decomplexing agent, and the temperature is controlled for decomplexing; (3) a decomplexing product obtained in the step (2) is filtered to separate solids, and filtrate is subjected to pressure reduction distillation to obtain phenyl dialkoxy phosphine or diphenyl alkoxy phosphine; (4) a product obtained in the step(3) is dissolved in a benzene or methylbenzene solvent, and a trichloromethyl acetyl compound is added dropwise for a reaction; and (5) a solution obtained after the complete reaction in the step (4)is subjected to low-pressure desolvation, and light-yellow liquid or solid, namely the phenyl phosphine oxide initiator, is obtained through crystallization, suction filtering and drying. The methodhas the advantages that raw materials are easy to obtain, cost is low, operation is easy to perform, and mass production can be realized.
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(2020/03/05)

Condensation reaction of homotrimethoxy benzoyl halides and diphenylphosphines and preparation of organic phosphine compounds
The present invention relates to the field of organic phosphine functional new material chemicals, and a "one-pot" direct condensation reaction of trimethylbenzoyl halide and an equivalent thereof and diphenylphosphine oxide is disclosed for the first time. By using this reaction process technology, two organic phosphine compounds are prepared simultaneously or one of them is selectively prepared, that is, trimethylbenzoyldiphenylphosphine oxide and trimethylbenzyl alcohol diphenylphosphine oxide diphenylphosphonate. The process technology has outstanding low-cost economic competitiveness and environmentally friendly characteristics.
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Paragraph 0068-0069

(2020/03/17)

Efficient preparation method of 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide
The invention discloses an efficient preparation method of 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide, which comprises the following steps: reacting 2, 4, 6-trimethylbenzaldehyde and diphenyl phosphine oxide in ethanol at room temperature for 24 hours to obtain a 2, 4, 6-trimethylphenyl diphenyl phosphine oxide-based methanol raw material; by adopting a catalyst, a solvent and an oxidant, reacting a separated and purified 2, 4, 6-trimethylphenyl diphenyl phosphine oxide-based methanol raw material at room temperature for 12 hours; evaporating to remove the acetic acid solvent, and recrystallizing with ethyl acetate and n-hexane to obtain pure 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide (TPO) crystals. According to the technical scheme, the use amount of the oxidation catalystis small, conditions are mild, operation is convenient and rapid, decomposition of the 2, 4, 6-trimethylphenyl diphenyl phosphine oxide-based methanol raw material or deterioration of the 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide product is avoided, and the 2, 4, 6-trimethylbenzoyl-diphenyl phosphine oxide target product is obtained with high yield and high purity.
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Paragraph 0030; 0034-0035

(2020/09/12)

Preparation of compound 2,4,6-trimethylbenzoyl diphenyl phosphine oxide
The invention relates to the field of photocuring functional new material chemicals, and discloses a novel one-pot synthesis process of a compound 2,4,6-trimethylbenzoyl diphenyl phosphine oxide for the first time; the process has the characteristics of outstanding low-cost economic competitiveness and environmental friendliness. The compound is an important ethylenic bond-containing unsaturated radiable polymerizable system photosensitive initiator.
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Paragraph 0021-0029; 0033-0034

(2020/02/14)

Method for preparing arylphosphine oxide derivatives
The invention discloses a method for preparing aryl phosphine oxide derivatives. According to the invention, potassium (hetero) arylmethyl trifluoroborate is used as a starting material, the raw material is easy to obtain and various in types, the material is solid, and storage and use are convenient; the products obtained by the method have various types and wide applications; the derivatives canbe conveniently converted into acylphosphine acylates, and the compounds can be widely used in the production of polymer materials, coatings, adhesives, adhesive tapes and the like as photoinitiators. In addition, the method has mild reaction conditions, high yield of the target product, little pollution, simple reaction operation and post-treatment process, and is suitable for industrial production.
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(2019/10/15)

Continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide compound
The invention discloses a continuous preparation method of trimethylbenzoyl-diphenylphosphine oxide (TPO) and its derivatives. The preparation method comprises: in a tubular reactor, benzaldehyde or its derivative reacts with chlorodiphenyl phosphine or its derivative; and then a catalytic oxidation reaction is directly carried out without separation, and the reaction solution is desolvated and re-crystallized to obtain a TPO product. The conversion rate of the product TPO is 98% and above, and the finished product content reaches 99.5% and above.
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(2019/10/07)

Double-benzoyl phenyl phosphine oxide and benzoyl diphenyl phosphine oxide of the preparation method
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.
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Paragraph 0051-0056

(2019/03/21)

Preparation method of 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide
The invention relates to a preparation method of 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide and particularly relates to a method, which comprises that phosphorus trichloride, benzene and aluminumtrichloride as raw materials undergo a reaction, the reaction product undergoes a hydrolysis reaction to produce diphenylphosphine oxide, diphenylphosphine oxide and 2, 4, 6-trimethylbenzoyl chloridedirectly undergo a reaction to produce 2, 4, 6-trimethylbenzoyldiphenylphosphine oxide. The preparation method of TPO solves the problems that the raw materials are difficult to prepare, the cost ishigh, the reaction steps are many, and the yield is low. The preparation method is an eco-friendly preparation process.
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(2019/02/13)

New synthesis method of photoinitiator 2,4,6-teimethyl benzoyl-diphenyl phosphine oxide
The invention discloses a new synthesis method of photoinitiator 2,4,6-teimethyl benzoyl-diphenyl phosphine oxide, and belongs to the technical field of the synthesis of the photoinitiator. The methodcomprises the following steps: adding diphenylethoxy phosphine and 2,4,6-trimethyl benzoyl in a reaction vessel at a vacuum condition of -0.098MPa, beginning reaction by controlling temperature at 40DEG C, rising temperature for 10 DEG C at the interval of 20min in the reaction process until the temperature is raised to 90 DEG C, and then reacting at constant temperature of 90 DEG C for 4-8h, and adding 50% ethanol crystal after the reaction is finished, namely obtaining a target product. The method disclosed by the invention is simple in synthesis and post-treatment step, the solvent is unnecessary to use in the synthesis process, and the purity and yield of the synthesized product are high.
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Paragraph 0020-0029

(2019/02/27)

Novel synthesis method of clean and safe photoinitiator (2,4,6-trimethylbenzoyldiphenyl-diphenylphosphine oxide)
The invention relates to the technical field of synthesis of photoinitiators, in particular to a novel synthesis method of a clean and safe photoinitiator (2,4,6-trimethylbenzoyldiphenyl-diphenylphosphine oxide). The method includes the steps of evenly mixing anhydrous alcohol with N-methylimidazole at the room temperature, raising the temperature to 30-50%, controlling the temperature, dropwise adding diphenylphosphine oxide, raising the temperature to 50-100 DEG C, conducting the constant-temperature reaction for 2-3 h, conducting standing and layering to take supernatant liquid for decompressing and distilling to obtain diphenyl alkoxylphosphine, making the diphenyl alkoxylphosphine start to react with 2,4,6-trimethylbenzoyldiphenyl chloride at the controlled temperature of 50 DEG C under the vacuum condition of -0.098 Mpa, raising the temperature by 10 DEG C every 20 minutes until the temperature is raised to 90 DEG C, conducting the constant-temperature reaction for 4-8 h, and adding 50% ethyl alcohol crystals to obtain a target product. The produced byproduct is subjected to vacuum removal and then enters a tail gas recovery system to be recovered through two stages of condensation. The synthesis method is simple in step, safe, clean, low in running cost and high in byproduct recovery rate.
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Paragraph 0041; 0043-0044

(2019/06/12)

Preparation method of 2,4,6-trimethyl benzoyl dibenzyl phosphine oxide
The invention relates to preparation technology of 2,4,6-trimethyl benzoyl dibenzyl phosphine oxide, specifically to a method which comprises taking phosphorus trichloride, benzene and aluminium trichloride as raw materials, performing a reaction, synthesizing dibenzyl phosphine oxide through a one-step reaction of decomplexing and hydrolysis, carrying out an addition reaction between dibenzyl phosphine oxide and 2,4,6-trimethylbenzaldehyde, and performing oxidation to prepare 2,4,6-trimethyl benzoyl dibenzyl phosphine oxide. The provided TPO preparation method solves the problem that raw materials are hard to prepare and the cost is high. The preparation method is available in raw materials, low in cost, easy to operate, and friendly to the environment and is not restricted in productionamount.
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Paragraph 0017-0022

(2018/04/01)

A 2, 4, 6 - trimethyl benzoyl diphenyl phosphine oxide - green environmental protection preparation method (by machine translation)
The invention discloses a 2, 4, 6 - trimethyl benzoyl diphenyl phosphine oxide - green environmental protection preparation method, comprises the following steps: a will be 2, 4, 6 - trimethyl benzaldehyde and diphenyl phosphine oxygen added to the equipped with dichloromethane three-opening in the bottle, the stirring reaction at room temperature, to obtain the intermediate TPO; b will be three-opening bottle into a low-temperature water bath cooled to 8 - 10 °C, then to the three-mouth bottle is sequentially added in the vanadium catalyst and oxidizing agent hydrogen peroxide, stirring reaction 0.5 hours, then the three mouth bottle is to continue stirring at room temperature 3 - 5 hours; c to the three-mouth bottle adding sodium thiosulfate aqueous solution in removing unreacted oxide, get the reaction solution, then the reaction solution is purified by separation, TPO products obtained. The present invention is the use of clean environmental protection of H2 O2 As the oxidizing agent, with the vanadium catalyst to form the green environmental protection oxidation system, and reduces the production cost, and improves product yield, friendly to the environment, is favorable to realize commercial production. (by machine translation)
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Paragraph 0030; 0031; 0032; 0033; 0034

(2017/07/19)

Method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'
The invention aims to provide a method for compounding 2,4,6-trimethylbenzoyl-diphenylphosphine oxide through 'one-pot process'. According to the preparation method, a sodium, ethanol, chlorodiphenylphosphine and 2,4,6-trifluoromethyl benzoyl chloride 'one-pot process' is firstly adopted for replacing the original diphenyl oxethyl phosphine and acyl chloride process for preparing 2,4,6-trimethylbenzoyl-diphenylphosphine oxide, so that the method can greatly reduce the preparation steps and processes, has the characteristics of low cost, simplicity in operation and high yield and can more effectively meet the increasing market requirements at present.
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Paragraph 0006; 0016-0023

(2017/11/16)

Phosphono-replaced methyl alcohol derivative, and preparation method and application thereof
The invention discloses a phosphono-replaced methyl alcohol derivative, and a preparation method and application thereof. The phosphono-replaced methyl alcohol derivative has the advantages that a (hetero) aryl methyl alcohol derivate serves as an initiator, and raw materials are easy to get and have great varieties; products obtained according to the preparation method have various types and wide application ranges, and serve as ligands which coordinate with rhodium to obtain various aldehydes through catalyzed synthesis; the phosphono-replaced (hetero) aryl methyl alcohol can be transformed into phosphonic compounds conveniently; the phosphonic compounds serving as photoinitiators can be widely applied to production of high polymer materials, paint, binders, adhesive tapes and the like. The preparation method has the advantages that reactions are achieved in the air, reaction conditions are mild, yield of target products is high, pollution is small, reaction operations and post-treatment processes are simple, and the preparation method is suitable for industrial production.
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Paragraph 0023

(2017/08/28)

Method for efficiently and recyclably synthesizing 2,4,6-trimethylbenzoyldiphenyl phosphine oxide
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.
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Paragraph 0028; 0030; 0032; 0033; 0036; 0040; 0044; 0048; 00

(2017/07/21)

The preparation method of compound acyl method
The invention relates to the technical field of radiation polymerization curing novel materials, and especially relates to a chemical preparation novel process of an acyl phosphine (oxide) compound represented by the general formula (I). A core characteristic of the method is that: a Grignard reagent of an aromatic compound substituted by an appropriate trichloromethyl group is subjected to condensation with related (substituted) phosphorus halide, such that a critical phosphorus-carbon bond is obtained. The innovativeness, cost economic competitiveness, and environment-friendliness of the process and chemical reaction technology provided by the invention are substantially advantaged than those of literatures and existing process routes.
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Paragraph 0024-0026

(2017/03/08)

( 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
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.
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(2017/04/07)

PHOSPHINE COMPOUND HAVING PERFLUORO GROUP, AND COMPLEX BETWEEN METAL AND PHOSPHINE HAVING PERFLUORO GROUP
PROBLEM TO BE SOLVED: To provide a perfluoroalkylphosphine compound, and a complex between a metal and the perfluoroalkylphosphine. SOLUTION: A perfluoroalkylphosphine compound is a phosphine compound represented by the general formula Rf-PR1R2. In the formula, R1 and R2 are each independently a substituted or unsubstituted hydrocarbon group; Rf is a perfluorinated hydrocarbon group. Also provided is a complex between the perfluoroalkylphosphine and a phosphine coordination metal. SELECTED DRAWING: None COPYRIGHT: (C)2016,JPOandINPIT
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Paragraph 0169; 0290-0292

(2018/10/16)

METHODS OF PRODUCING PHOSPHINE COMPOUND HAVING PERFLUORO GROUP AND COMPLEX BETWEEN METAL AND PHOSPHINE HAVING PERFLUORO GROUP
PROBLEM TO BE SOLVED: To provide methods of producing a perfluoroalkylphosphine compound improved in a phosphorus element yield and a chemical yield. SOLUTION: A method of producing a perfluoroalkylphosphine compound comprises either reacting a perfluoroalkyl iodide with, e.g., 2,4,6-trimethylbenzoyldiphenylphosphine oxide (TMDPO) or a triarylphosphine such as triphenylphosphine, which are easily available, in the presence of a radical generator such as azobis(isobutyronitrile) or light irradiation, or reacting TMDPO or the like with perfluoroalkyl iodide in the presence of diphenylphosphine, diethylphosphine, dicyclohexylphosphine or the like. SELECTED DRAWING: None COPYRIGHT: (C)2016,JPOandINPIT
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Paragraph 0243-0244

(2018/10/19)

Method for producing acylphosphine oxide solids
The present invention relates to a process for the preparation of solid acylphosphine oxides by converting an acylphosphine oxide which is in the form of a melt or in dispersed form into the solid state of aggregation with mechanical stress, shearing/internal agitation of the melt.
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(2008/06/13)

METHOD FOR PRODUCING ACYLPHOSPHINE OXIDE SOLIDS
The invention relates to a method for producing acylphosphine oxide solids consisting in transforming a molten or dispersed acylphosphine oxide into the solid aggregated state thereof by means of mechanical stress, shear force or the internal motion of the melt.
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Page/Page column 12-14

(2008/06/13)

Photo-curable reparative material for dental use
A photocurable dental restorative comprising (i) 100 parts by weight of a polymerizable monomer, (ii) 0.01 to 5 parts by weight of a photopolymerization initiator of acylphosphine oxide, and (iii) 200 to 1900 parts by weight of an inorganic filler, wherein the inorganic filler (iii) is a mixed filler of: (A) irregular-shaped inorganic particles having an average particle size of not smaller than 0.1 μm but smaller than 1 μm; (B) spherical inorganic particles having an average primary particle size of not smaller than 0.1 μm but not larger than 5 μm; and (C) fine inorganic particles having an average primary particle size of not larger than 0.1 μm; which are so blended as to satisfy the following mass ratios {circle over (1)} to {circle over (3)}: mA/(mB+mC)=0.2 to 3??{circle over (1)} mB/(mB+mC)=0.5 to 0.99??{circle over (2)} mC/(mB+mC)=0.01 to 0.5??{circle over (3)} where mA, mB and mC are masses of the inorganic particles (A) to (C). The restorative features excellent handling property, and makes it possible to obtain a cured product having a high fracture toughness and excellently glossy surface.
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(2008/06/13)

PROCESS FOR PREPARING ACYLPHOSPHINES AND DERIVATIVES
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(2008/06/13)

Molecular complex compounds of acylphosphine oxide and α-hydroxy ketones as photoinitiators
Molecular complex compounds comprising a mono-, bis- or trisacylphosphine oxide compound with an α-hydroxy ketone compound are suitable as photoinitiators for the photopolymerization of free-radically polymerizable compounds.
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(2008/06/13)

Preparation of α-carbonylphosphine oxides
The preparation of α-carbonylphosphine oxides by oxidizing an α-hydroxyalkyl phosphine oxide with an organic hydroperoxide or of an organic peroxy acid in the presence of a compound of a Group IV to Group VIII metal in the periodic table, and novel α-hydroxybenzyl phosphine oxides. α-Carbonylphosphine oxides are used as photoinitiators for polymerizable compositions.
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(2008/06/13)