Study On The Condensed Phosphates RDP & BDP And Their Analog's Design And Synthesis

The polymeric materials are widely used nowadays and their safety is much more concerned. At the same time the need of flame retarded materials and flame retardant grows rapidly. This paper reviewed the phylogeny of flame retardant, the mechanisms of flame retardant and related research and development. A kind of low contaminative condensed phosphate which was excellent as flame retardant was studied. Besides this, this paper designed and synthesized 4 novel phosphates, adding the new number to the family of flame retardant.The condensed phosphates which were studied in this paper were oligomeric resorcinol bis(diphenyl phosphate)(RDP for short) and oligomeric bisphenyl A bis(diphenyl phosphate) (BDP for short). The optimized reaction conditions were obtained through the single factor experiment. The results were as follows:(1)RDP: In presence of aluminium chloride as catalyst, the molar ratio of phosphorus oxytrichloride, resorcinol and phenol was 6.7:1:4.04. The appropriate calefactive time to the refluence temperature(~113℃) was about 0.5h and the reaction time was 3h in the condensation reaction. The reaction temperature was 150℃ and the reaction time was 4h in the end capping reaction. The proper temperature of adding phenol was 40~60℃. Upon the above proper condition, the yield of the target product was 90.2% based on resorcinol.(2)BDP: In presence of aluminium chloride as catalysis, the molar ratio of phosphorus oxytrichloride, bisphenol A and phenol was 5.5:1:4.04. The appropriate calefactive time to the reaction temperature (105~118℃) was about 0.5h and the reaction time was 3.5~4h in the condensation reaction. The reaction temperature is 150℃ and the reaction time was 5h in the end capping reaction. In this condition, the yield was 85.7% based on bisphenol A.This paper designed one type (two kinds) of phosphorous and chloro-containing compound based on the conclusion that cooperating phosphorus with halogen can improve the effect of flame retardant, they were resorcinol bis(bis(1-chloro-2-propyl) phosphate) and bisphenyl A bis(bis(1-chloro-2-propyl) phosphate). This paper designed another type (two kinds) of cyclic phosphate based on the conclusion that the kind of phosphate having high molecule mass and symmetrical structure and high content of phosphors are excellent as flame retardant, they were 1,3-bis(2-oxo-5,5-dimethyl-1,3,2-dioxaphos-phorinanyl-2-oxy)benzene and 2,2'-(4-(5,5-dimethyl-1,3,2-dioxaphos-phorinanyl-2-oxy)phenyl)propane. The structures of the target compounds were confirmed by IR, 'H-NMR, 13C-NMR, UV and MS. The results showed that the structures of the synthesized compounds were identical with the expected ones. The reaction conditions of two compounds were studied and optimized. They were as follows:(l)Resorcinol bis(bis(l-chloro-2-propyl) phosphate): The molar ratio of resorcinol phsphorochloride and 1,2-epoxypropane was 1:6, reaction temperature was 65 °C, reaction time was 4h, and the manner of adding 1,2-epoxypropane was drop by drop, aluminium chloride as catalyst, the yield was 89.9% based on resorcinol.(2)l,3-Bis(2-oxo-5,5-dimethyl-l,3,2-dioxaphos-phorinanyl-2-oxy)benzene: The molar ratio of neopentyl glycol phosphorous chloride, resorcin and triethylamine was 2:1:4, chloroform as solvent and refluence for 4h(the reaction temperature was 64 *C), the yield of the product was 66.2% based on resorcinol.