- Process for preparation of phosphorane and phosphonyl compounds
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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 0028-0030
(2021/06/06)
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- Preparation method of bis(2,4,6-trimethylbenzoyl)phenyl phosphine oxide
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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.
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Paragraph 0096-0099; 0103-0106; 0111-0114; 0118-0121; 0125
(2021/01/11)
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- Preparation method of bis(2, 4, 6-trimethylbenzoyl)phenylphosphine oxide
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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.
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Page/Page column 6-14
(2020/12/30)
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- Preparation method of phenyl bis (2,4,6-trimethylbenzoyl) phosphine oxide
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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.
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- Preparation method of photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide
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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.
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- Double-benzoyl phenyl phosphine oxide and benzoyl diphenyl phosphine oxide of the preparation method
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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 0045-0050
(2019/03/21)
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- PRODUCTION METHOD OF ACYL PHOSPHINE
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PROBLEM TO BE SOLVED: To provide a production method of acyl phosphine and acyl phosphine oxide that has a high production efficiency and safety. SOLUTION: A production method of acyl phosphine represented by formula (1) includes a step for reacting a pho
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Paragraph 0041
(2018/12/14)
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- A photo initiator double (2, 4, 6-trimethyl benzoyl) method for preparing phenyl phosphine oxide
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The invention discloses a preparation method for a photoinitiator bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide. The preparation method comprises the synthesis steps: under the protection of inert gas, carrying out a reaction of aluminium trichloride or tin tetrachloride and trimethylsilane in the temperature range of 0-100 DEG C to obtain aluminium dichloride ions, and rapidly acting with dichlorophenyl phosphine in the reaction system, to obtain a bis(aluminium trichloride or tin tetrachloride)phosphine salt intermediate; then carrying out a reaction of the intermediate and 2,4,6-trimethyl benzoyl chloride, to obtain bis(2,4,6-trimethylbenzoyl)phenyl phosphine; and under the condition of the temperature of 20-50 DEG C, oxidizing by nitrogen dioxide, to obtain the target product. The method avoids use of a dangerous active metal potassium or sodium, and adopts aluminium trichloride or tin tetrachloride with relatively low price and trimethylsilane for on-site generation of the active intermediate to achieve the reaction. The method has the characteristics of low preparation cost, simple and safe operation process, easy control of the reaction process, high product yield, good purity, easy realization of mass production and the like.
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Paragraph 0036
(2017/02/09)
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- Preparation method of photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide
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The invention discloses a preparation method of a photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide, comprising the steps of enabling diethyl benzylphosphonate and an excessive vitride solution to react in argon under the temperature of 60-70 DEG C, so as to generate phenyl phosphine, enabling the phenyl phosphine and 2,4,6-trimethylbenzoyl chloride to react, so as to obtain a methylbenzene solution of diphenyl(2,4,6-trimethylbenzoyl)phosphine, and oxidizing the diphenyl(2,4,6-trimethylbenzoyl)phosphine into 2 phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide by hydrogen peroxide without separating. According to the process, dangerous metal sodium or potassium is not used, the process is advanced, the operation is simple and safe, the product yield is high, the quality is good, and large-scale production is easy.
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Paragraph 0025; 0026; 0027
(2016/12/26)
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- Preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide
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The invention discloses a preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method comprises the following steps: selecting triphenylphosphine as a raw material for reactions with sodium metal and phosphorus halide in the presence of one or more catalysts; carrying out an acyl chloride reaction; carrying out oxidation to prepare phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide. The preparation method has the advantages of being easy in raw material obtaining, low in cost, easy to operate, environmentally friendly, and easy for industrialization.
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- D1479 STABLE LIQUID BAP PHOTOINITIATOR AND ITS USE IN RADIATION CURABLE COMPOSITIONS
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The invention relates to radiation curable compositions comprising a liquid 0/s(acyl)phosphine photo initiators of formula (I): wherein each of Ar1, Ar2 and Ar3 is independently a substituted or unsubstituted aryl group. The invention also relates to stabilized forms of liquid bis(acyl)phosphines of formula (I) and radiation curable composition comprising said stabilized photoinitiators. The radiation curable compositions are selected from the group consisting of an optical fiber coating composition and a coating composition capable of radiation cure on concrete and a coating composition capable of radiation cure on metal.
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Paragraph 0192; 0193
(2013/09/26)
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- A simple straightforward synthesis of phenylphosphane and the photoinitiator bis(mesitoyl)phenylphosphane oxide (IRGACURE 819)
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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.
- Grützmacher, Hansj?rg,Geier, Jens,Stein, Daniel,Ott, Timo,Sch?nberg, Hartmut,Sommerlade, Reinhard H.,Boulmaaz, Souad,Wolf, Jean-Pierre,Murer, Peter,Ulrich, Thomas
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- PROCESS FOR PREPARING ACYLPHOSPHANES AND DERIVATIVES THEREOF
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The invention relates to a process for the preparation of (bis)acylphosphanes of formula I, wherein n and m are each independently of the other 1 or 2; R1 if n = 1 , is e.g. unsubstituted or substituted C1-C18alkyl or C2-C18alkenyl, or phenyl, R1 if n = 2, is e.g. a divalent radical of the monovalent radical defined above; R2 is e.g. C1-C18alkyl, C3-C12cycloalkyl, C2-C18alkenyl, mesityl, phenyl, naphthyl; R3 is one of the radicals defined under R1; the process comprises the steps a) contacting e.g. elemental phosphorous [P]∞, P(Hal)3 with a reducing metal optionally in the presence of a catalyst or an activator in a solvent to obtain metal phosphides Me3P or Me'3P2, wherein Me is an alkali metal and Me' is an earth alkali metal or to obtain metal polyphosphides b) optionally adding a proton source, optionally in the presence of a catalyst or an activator to obtain metal dihydrogen phosphides MePH2; c) subsequent acylation reaction with m acid halides of formula III or m carboxylic acid esters of formula IV or, in case that in formula I m = 1, with one carboxylic ester of formula IV followed by one acid halide of formula III or vice versa, wherein R is the residue of an alcohol and R2 is as defined above; d) alkylation reaction subsequent reaction with an electrophilic agent R1Hal or other electrophilic agents to obtain the compounds of formula I. An oxidation step may follow to obtain mono- and bisacylphosphane oxides or mono- and bisacylphosphane sulfides, which are used as photoinitiators.
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Page/Page column 45
(2010/11/08)
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- A PROCESS FOR THE PREPARATION OF ACYLPHOSPHINES
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A process for the preparation of acylphosphines of formula (I) wherein m is 1 or 2; R1, R2, and R3 are organic residues derived from aliphatic or aromatic hydrocarbons; by (1) reacting organic phosphorus halides of formula (II) wherein Y is Br or Cl,with an alkali metal in a solvent in the presence of an activator, wherein the alkali metal is present in the form of a dispersion of alkali metal particles having a mean particle size of ≤ 500 μm in the solvent, (2) subsequent reaction with acid halides of formula (III) which process is carried out without isolation of the intermediates. Preferably, R1, R2 and R3 are independently from each other phenyl, naphthyl and bi-phenyl, being unsubstituted or substituted by one to five halogen, C1-C8 alky and/or C1-C8 alkoxy. Most preferably, R1 and R3 are phenyl and R2 is 2,4,6-trimethylphenyl. The alkali metal is preferably sodium, the activator is preferably chlorobenzene and/or n-butanol.
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Page/Page column 9-10
(2010/02/10)
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- PROCESS FOR PREPARING ACYLPHOSPHANES AND DERIVATIVES THEREOF
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The present invention relates to a new, selective process for the preparation of mono- and bisacylphosphanes of formula (I) n and m are each independently of the other 1 or 2; R1, if n = 1, is e.g. phenyl R1, if n = 2, is e.g. C1-C18alkylene or phenylene; R2 is e. g. C1-C18alkyl, phenyl or substituted phenyl; R3 is e. g. C1-C18alkyl, by (1) reacting a phosphorous halide of formula Ila or a phosphorous halide oxide of formula (Ilb) or a phosphorous halide sulfide of formula (IIc) with an alkali metal in a solvent in the presence of a proton source; (2) subsequent reaction with m acid halides of formula (III) An oxidation step may follow to obtain mono- and bisacylphosphane oxides or mono-and bisacylphosphane sulfides.
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Page/Page column 39-40
(2010/02/10)
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