620596-61-4Relevant academic research and scientific papers
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 0096-0099; 0103-0106; 0111-0114; 0118-0121; 0125, (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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Paragraph 0045-0050, (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.
PRODUCTION METHOD OF ACYL PHOSPHINE
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Paragraph 0041, (2018/12/14)
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
A photo initiator double (2, 4, 6-trimethyl benzoyl) method for preparing phenyl phosphine oxide
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Paragraph 0036, (2017/02/09)
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.
Preparation method of photoinitiator phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide
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Paragraph 0025; 0026; 0027, (2016/12/26)
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.
Preparation method for phenyl bis(2,4,6-trimethylbenzoyl)phosphine oxide
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, (2016/10/09)
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.
