Synthesis And Study On Condensation Type Phosphate Ester Flame Retardants PAPTE&BDP

Organic phosphorus flame retardants,as a halogen-free system,has the advantages of high flame retardant efficiency,low toxicity,low corrosion and good compatibility with polymer materials,etc.Much attention has been paid to the research of condensation type phosphate ester flame retardant because of its high phosphorus content,large molecular chain and structure symmetry,it has become the trend of the future.The main contents of this paper are summarized as follows:The P,P'-1,4-phenylene P,P,P',P'-tetraphenyl ester(PAPTE)was prepared by hydroquinone,phosphorus oxychloride and phenol.The intermediate of hydroquinone chloride phosphate has been discussed in detail.The bisphenol-A Bis(dipenyl phosphate)(BDP)was synthesized by diphenyl chlorophosphate and bisphenol-A.Low temperature crystallization method is used to convert BDP in powder.In order to find the optimal process,a series of factors such as solvent type,crystallization solvent content,crystallization time on product yield have been discussed.The structures of compounds were characterized and confirmed by IR spectra,~1H NMR spectra.Their thermal stability were studied by thermogravimetric analysis(TGA).The solubility of hydroquinone pairs of phosphorus oxychloride and BDP in the select solvents were measured by static analytical method.Hydroquinone pairs of phosphorus oxychloride in toluene,1,2-dichloroethane and chloroform,BDP in ethyl acetate,acetonitrile and acetone were measured respectively.The solubility against the temperature was investigated and the experimental data was associated by parameter equations.It provides a fundamental thermodynamic property data for the industrial synthesis and purification.