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Method for preparing 10-(2,5-hydroxyphenyl)-10-H-9-oxa-10-phosphaphenanthrene-10-oxide

A technology of dihydroxyphenyl and phosphaphenanthrene is applied in the field of preparation of phosphorus-containing reactive flame retardant intermediates, which can solve the problems of easy decomposition and poor stability in the application process, and achieve simple and easy-to-control operation, low equipment investment, Wide range of effects

Active Publication Date: 2013-07-24
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide an efficient synthetic route for preparing 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, namely DOPO-HQ, To overcome the poor stability of the products obtained in the prior art, and the problems of easy decomposition during application

Method used

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  • Method for preparing 10-(2,5-hydroxyphenyl)-10-H-9-oxa-10-phosphaphenanthrene-10-oxide

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Experimental program
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Effect test

Embodiment 1

[0030]Add 31.4g of BQ and 0.78g of activated carbon into 55.9g of tetrahydrofuran, raise the temperature to 50°C, dissolve BQ in the solvent tetrahydrofuran under stirring, and filter while it is hot to obtain feed liquid A; (2) While preparing feed liquid A, Add 59.4g DOPO into 54.1g tetrahydrofuran, raise the temperature to 50°C, and dissolve DOPO into tetrahydrofuran under stirring to obtain feed liquid B; add feed liquid A dropwise to feed liquid B while it is hot, and add dropwise for 30 minutes while stirring After the dropwise addition is completed, the reaction system formed by the feed liquid A and the feed liquid B is first carried out a 30-minute preliminary reaction at a temperature of 60° C. and under agitation, and then 0.59 g of zinc stearate is added to the reaction system. The reaction system continued to carry out the post-reaction for 3 hours at 65°C under stirring conditions. After the reaction was completed, the reaction system was cooled until the solid pr...

Embodiment 2

[0032] Add 29.7g of BQ and 1.19g of diatomaceous earth into 56.4g of toluene, raise the temperature to 70°C, dissolve BQ in the solvent toluene under stirring, and filter while it is hot to obtain feed liquid A; (2) Preparation of feed liquid A At the same time, add 59.4g DOPO into 59.4g toluene, raise the temperature to 70°C, dissolve DOPO into toluene under stirring, and obtain material liquid B; After 40 minutes, after the dropwise addition is completed, the reaction system formed by the feed liquid A and the feed liquid B is firstly reacted for 40 minutes at a temperature of 90° C. and stirred, and then 0.89 g of magnesium stearate is added to the reaction system. Under the condition of stirring at a temperature of 105°C, the reaction system continued to carry out the post-reaction for 4 hours. After the reaction was completed, the reaction system was cooled until the solid product was fully separated, and 92.56 g of the solid product obtained by filtering the reaction syst...

Embodiment 3

[0034] Add 32.67g of BQ and 1.96g of activated carbon into 71.9g of chlorobenzene, raise the temperature to 90°C, dissolve BQ in the solvent chlorobenzene under stirring, and filter while it is hot to obtain feed liquid A; (2) Prepare feed liquid A At the same time, add 59.4g DOPO into 83.2g chlorobenzene, raise the temperature to 90°C, and dissolve DOPO into chlorobenzene under stirring to obtain feed liquid B; while hot, add feed liquid A dropwise into feed liquid B, and stir under Add dropwise for 50 minutes. After the dropwise addition is completed, make the reaction system formed by feed liquid A and feed liquid B under stirring conditions at a temperature of 110°C for 50 minutes of preliminary reaction, and then add 1.19 g of stearic acid into the reaction system Lead, under the temperature of 125 ℃ and stirring conditions, make the reaction system continue to carry out the post-reaction for 5 hours. After the reaction is completed, cool the reaction system until the soli...

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Abstract

The invention discloses a method for preparing 10-(2,5-hydroxyphenyl)-10-H-9-oxa-10-phosphaphenanthrene-10-oxide. The method comprises the following steps of: (1) dissolving p-benzoquinone in a solvent and adding active carbon or diatomite for absorption treatment, and then performing solid-liquid separation to obtain feed liquid A; (2) dissolving DOPO (9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) in the same solvent of the step (1) according to a mass ratio of DOPO to p-benzoquinone of 1:(0.5-0.6), thereby obtaining feed liquid B; (3) adding the feed liquid A to the feed liquid B for earlier-stage reaction, and then adding a stabilizer for continuous late-stage reaction, and after the reaction is completed, cooling the reaction system until a solid product is thoroughly separated out; and finally, performing solid-liquid separation to obtain the solid product, namely the target product. The product provided by the method is stable in quality and good in process repeatability; the product can not be decomposed in the process of application; as a result, the application range of the product is expanded and the product is popular with users; and the process is simple to operate and easy for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a phosphorus-containing reactive flame retardant intermediate, specifically a compound 10-(2,5-dihydroxyphenyl)-10-hydrogen-9-oxa-10-phosphorus Preparation method of heterophenanthrene-10-oxide. Background technique [0002] As an important material to protect people's lives and properties, flame retardants have attracted much attention, and their consumption is increasing day by day. Various flame retardants and flame retardant materials have been widely used in various fields such as construction, medicine, and transportation. Traditional halogen-based flame retardants will generate hydrogen halide gas, dioxin and other toxic substances during use, causing many environmental problems. Therefore, under the pressure of environmental protection, the development of halogen-free flame retardant additives is unstoppable. Among them, phosphorus-based flame retardants are the most complex and well-studied cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 闫晓红赵庭栋李善清杨海燕钟世强孙树青尹展翔
Owner SHANDONG TIANYI CHEM
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