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9, 10- dihydro-9- oxa -10- phosphine hetero- phenanthrene -10- oxide compound and its derivant and method of preparing the same

A technology of phosphophenanthrene and oxide, which is applied in the field of preparation of new flame retardants, can solve the problems of CDOP synthesis time, complex production process, and long hydrolysis time, etc., and achieve the effect of simple method, simple product processing and simple method

Inactive Publication Date: 2008-01-23
魏铭杉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0022] The purpose of the present invention is to provide a preparation method for DOPO with high purity and high yield, so as to solve the technical problems of complex production process, long CDOP synthesis time, long hydrolysis time and poor product purity in the prior art;

Method used

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  • 9, 10- dihydro-9- oxa -10- phosphine hetero- phenanthrene -10- oxide compound and its derivant and method of preparing the same
  • 9, 10- dihydro-9- oxa -10- phosphine hetero- phenanthrene -10- oxide compound and its derivant and method of preparing the same
  • 9, 10- dihydro-9- oxa -10- phosphine hetero- phenanthrene -10- oxide compound and its derivant and method of preparing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Add 204Kg OPP, 2Kg ZnCl into the 1500L enamel reaction kettle 2 Heating, when the temperature rises to 50°C, it will start to melt, and when it reaches 80°C, the OPP will completely melt, start stirring, continue to heat up to 180°C, and start adding PCl dropwise 3 197Kg, at this time, HCl is released, 4h is added, and the reaction is continued for 1h. At this time, no HCl is released, stop heating, cool down to about 140°C, add an equal volume of mixed xylenes, and obtain a CDOP xylene mixed solution. Vacuumize (about 0.04mPa) to remove residual PCl 3 , then filtered to remove a small amount of residue. The filtrate is reheated to remove xylene first, and then distilled under a vacuum of 0.05-0.07mpa and 160-165°C to obtain water-like CDOP.

[0056] Then add about 200-300L of xylene into the enamel reaction kettle to dissolve CDOP, add the same amount of water, at this time, HCl is released, and when the temperature is 100°C and no HCl is released, stop the reaction...

Embodiment 2

[0058] According to Example 1, add 204KgOPP and 2Kg ZnCl2 to a 1500L enamel reaction kettle and heat it. When the temperature reaches 50°C, the OPP will start to melt. When the temperature reaches 80°C, the OPP will all melt. Add 197Kg PCl3, at this time, HCl is released, after adding 4h, continue to react for 2h, at this time, no HCl is released, when the temperature is lowered to 140°C, vacuumize, the vacuum degree is 0.04-0.05mpa, to remove residual PCl3, and then add the same amount Mix the xylenes to make a CDOP xylene solution. Cool to room temperature, filter to remove a small amount of solid residue. Then the xylene is evaporated from the solution at 0.04-0.05mpa, the temperature is raised to 160-165°C, 0.17KPa, and the CDOP is evaporated.

[0059] Dissolve CDOP in xylene again, add the same amount of water, at this time, at 80°C, HCl will be released, and at 100°C, no HCl will be released, and then continue to hydrolyze for 2 hours, and the liquid phase temperature i...

Embodiment 3

[0061] In the 1000L enamel reaction kettle, add DOPO411.3Kg, pass N 2 Heating up, at 150°C, add 247.5Kg of itaconic acid, and react for 4 hours to obtain a colorless and transparent resinous product of DOPO-itaconic acid (DDP), add acetone to crystallize, and obtain the white DDP of the DOPO derivative of the present invention. Powder 650.2Kg. Main technical indicators of the product: Yield 99% mp: 187-188°C.

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Abstract

The invention discloses a preparation method of the 9, 10-dihydro-9-oxa-10-phosphahenanthrene-10-oxide and the derivatives DDP, DDP-EG and DOPO-BQ. The invention has three steps to synthesize the DOPO: (1) preparation of CDOP, the O-phenylphenol (OPP) reacts with the Phosphorus trichloride (PCl3) with ZnCl2 as the catalyst. (2) purification of CDOP, vacuum distillation is carried out. (3) DOPO with high purity and yield is gained through the hydrolysis and crystallization. The preparation materials comprises the O-phenylphenol, the Phosphorus trichloride, the toluene, the alcohol, the deionized water, the itaconic acid, the ethylene glycol, the p-benzoquinone and the acetone. The invention simplifies the process conditions, improves the product purity with good production stability and repeatability. The purity of the product reaches over 99.0 per cent, the content of the chloride is below 50ppm, the OPP is about 0.01 per cent, the color is about 10 (10 per cent solution of acetone), the zinc-ion is less than 10ppm. The preparation method of the derivatives DDP, DDP-EG, DOPO-BQ is simple, good in stability and high in yield.

Description

technical field [0001] The invention relates to a preparation method of a novel flame retardant, which belongs to the field of chemical synthesis. Specifically, it relates to a preparation method of organophosphorus compound 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and derivatives thereof. Background technique [0002] At present, the application of new-type halogen-free organophosphorous heterocyclic compounds is researched and explored in various fields at home and abroad, especially a series of studies on the application of flame retardants. Among them, Japan, Germany and China Taiwan region are more in-depth. Our country is also conducting extensive and in-depth research and discussion, and they all provide some effective ways. However, there are still some problems in industrial production and product quality, especially the research on application is still far behind. [0003] The English name of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is 9,10-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
Inventor 吴宝庆果学军魏铭杉
Owner 魏铭杉
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