Preparation And Application Of Phosphinic Acid/Salt Flame Retardants Containing Amide Group

Halogen-free flame retardants have been fully implemented，coordinatedaction of multielement was widely used in phosphorus flame retardant because ofhigh efficiency. Phosphorus-nitrogen containing flame retardant andalkylphosphinic satls which containing special functional groups have been a hotarea of research in recent years. Those flame retardants not only equipped withhigh-efficiency of multielement, but also improve some special features due tospecial functional group. In order to improved technology, lower costs andsuitable for industrial production. In this study, two new kinds of alkylphosphinicwhich containing special functional group.(Phosphorus-nitrogen containing)---β-（N-phenyl carboxamide)ethyl methyl phosphinic acid (CEMP) and (DDMP)were synthetize by a simple one-step reaction of2-methy-2,5-dioxo-1,2-oxapho--spholane (OP) with aniline or4,4’-Methylenedianiline. And nine new kinds ofalkylphosphinic salt which containing special functional group.(Phosphorus--nitrogen-metal containing)---β（-N-phenyl carboxamide)ethyl methyl phosphinicsatls X(CEMP)[X select：Al、Zn、Mg、Ca、Fe]、β-（N-cyclohexylcarboxamide)ethyl methyl phosphinic satls Y(HEMP)[Y select：Al、Ca]、aluminumβ-（N-butyl carboxamide)ethyl methyl phosphinate Al(NEMP) weresynthesize by three-step reaction of OP; aniline、cyclohexylamine or butyl amine;sodium hydroxide and inorganic metal salt. The structure of these syntheticproducts were characterized with FTIR、1H-NMP and XRF. Use TG and DSCdetermining the nature of synthetic products. The research result shows that metalions can enhance thermostability and the alkyl carbon structure can affect thermalproperties. Various performance of these flame retardants filled epoxy resin (EP)or polybutylene terephthalate (PBT) were studied. Results of EP system show that:(1) These flame retardants can reacts with EP. Also, flame retardants/EP systemand DDM/EP system reinforcing each other, metal ions and alkyl carbon structureinfluenced the curing process of EP.(2) CEMP、Al(CEMP) and DDMP wereefficient flame-retardant, such as:20wt.%CEMP/DDM/EP can reach the LOIvalue of29.4and UL-94V-0.(3) Metal ions and types of cross linker could change various properties and process of thermolysis of epoxy resins compositematerials. Results of PBT system show that:(1) Al(CEMP)、Al(HEMP)、Al(NEMP) were efficient flame-retardant;20wt.%Al(CEMP)/PBT can reach theLOI value of39.5and UL-94V-0，20wt.%Al (CEMP)/GFPBT can reach the LOIvalue of32and UL-94V-0.it was superior to aluminum methylcyclohexyl--phosphinate Al (MHP)[industrial products] and OP930[products of Clariantcompany].(2) CEMP and other kinds of alkylphosphinic satls lose fire resistance.(3) Metal ions and types of cross linker also affect various properties and processof thermolysis of PBT composite materials. Compare EP and PBT system, CEMPmore specifically suited to EP materials and Al (CEMP) more appropriate for useof PBT materials.