Method for preparing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide

A phosphaphenanthrene and oxide technology is applied in the field of preparation of phosphorus-containing reactive flame retardant intermediates, which can solve the problems of poor product purity, complicated production process, and excessively long synthesis time, and achieves high product yield and high product quality. High-purity, easy-to-use results

Inactive Publication Date: 2011-08-10
SHANDONG TIANYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a friendly synthetic route for the preparation of DOPO to overcome the problems of complex production process, long synthesis time and poor product purity in the prior art, while avoiding the use of high-vacuum equipment and facilitating industrial production

Method used

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  • Method for preparing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide

Examples

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Embodiment 1

[0029] Add 170g of OPP and 1.7g of anhydrous zinc chloride to a 1000ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel, stir and raise the temperature to 140°C to melt the OPP, and continue to raise the temperature to 160°C , Began to add 164.4g of phosphorus trichloride dropwise, after 8 hours of dropping, keep the reaction at 160-165°C for 2 hours; after the reaction is completed, distill out excess phosphorus trichloride at a temperature of 120°C to prepare intermediate The product 6-chloro-(6hydro)-diphenyl[C,E][1,2]-phosphaphenanthrene (CDOP); under stirring and reaction conditions of 50℃, drop the obtained CDOP into a concentration of 25% In the sodium hydroxide solution containing 80g of sodium hydroxide, drip in 1 hour and maintain the reaction for 2 hours to obtain the sodium salt solution of CDOP; let the sodium salt solution of CDOP stand for 30 minutes, and then filter the sodium salt solu...

Embodiment 2

[0031] Add 170g of OPP and 3.4g of FeCl to a 1000ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel 3 , Stir and raise the temperature to 140°C to melt the OPP, continue heating to 165°C, start adding 219.2g of phosphorus trichloride dropwise, the addition is completed in 10 hours, and keep the reaction at 165~170°C for 4 hours; after the reaction is completed, the temperature Excess phosphorus trichloride was distilled out at 130℃ to obtain the intermediate product 6-chloro-(6hydro)-diphenyl[C,E][1,2]-phosphaphenanthrene (CDOP); Under the reaction conditions of ℃, drop the obtained CDOP into a 30% concentration of sodium hydroxide 100g sodium hydroxide solution, drop in 1.5 hours, maintain the reaction for 3 hours, obtain the sodium salt solution of CDOP; leave the CDOP to stand still The sodium salt solution of CDOP is filtered for 40 minutes, and then the catalyst iron and impurities in the sodium ...

Embodiment 3

[0033] Add 170g of OPP and 5.1g of TiCl to a 1000ml four-necked flask equipped with a thermometer, a magnetic stirrer, a reflux condenser, and a constant pressure dropping funnel 4 , Stir and raise the temperature to 140℃ to melt the OPP, continue heating to 170℃, start to add 274g phosphorus trichloride dropwise, 12 hours to complete the dropwise addition, 170~175℃ to continue to react for 4 hours; after the reaction is completed, the temperature is 140 Excess phosphorus trichloride was distilled out at ℃ to obtain the intermediate product 6-chloro-(6hydro)-diphenyl[C,E][1,2]-phosphaphenanthrene (CDOP); under stirring and 95℃ Under the reaction conditions, the obtained CDOP was dropped into a 10% concentration of sodium hydroxide 120g sodium hydroxide solution, after 2 hours of dripping, after maintaining the reaction for 4 hours, the sodium salt solution of CDOP was obtained; Sodium salt solution for 60 minutes, and then filter the catalyst titanium and impurities in the CDOP ...

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Abstract

The invention discloses a method for preparing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. The method comprises the following steps: using phosphorus trichloride and o-phenylphenol to react and prepare an intermediate product 6-chloro-(6-hydro)-diphenyl[C,E][1,2]phosphaphenanthrene; (2) performing alkaline hydrolysis on the intermediate product to obtain a saline solution of the intermediate product, and filtering the saline solution to obtain filtrate; (3) acidizing the filtrate to obtain a crystal-solution mixture, filtering the crystal-solution mixture to obtain 2-hydroxybiphenyl-2-hypophosphorous acid crystal powder; and (4) heating the crystal powder to dewater, and then stirring and cooling to crystallize, thus obtaining a block material which is the target product. The method disclosed by the invention has the advantages of simplified technological conditions, low equipment investment, good production stability and suitability for industrialized production; and the prepared product has higher purity and yield.

Description

Technical field [0001] The invention relates to a preparation method of a phosphorus-containing reactive flame retardant intermediate, specifically a compound 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) The preparation method. Background technique [0002] Halogen flame retardants have shortcomings such as excessive smoke, release of toxic and corrosive hydrogen halide gas when used, and potential secondary hazards. In particular, recent studies have found that high polymers flame-retarded with polybrominated diphenyl ethers will produce toxic carcinogens polybrominated dibenzoxanes (PBDDs) and polybrominated dibenzofurans (PBDFs) when burned. Therefore, in recent years, countries in the world have begun to actively seek alternatives to halogen-containing flame retardants. Compared with halogen-based flame retardants, organophosphorus flame retardants have better flame retardancy, low smoke and low toxicity, good compatibility with polymers, conform to the develop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 孟烨闫晓红赵庭栋刘兆明李善清邢晓华钟世强王善华
Owner SHANDONG TIANYI CHEM
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