Study On The Synthesis And Application Of Methyl Octabromo Ether In Water Phase

Due to the safety problems caused by the inflammability of polymer materials,people pay close attention to the flame-retardant polymer materials.With the wide use of polyurethane,polystyrene,polypropylene and other general plastics,it is particularly important to choose suitable flame retardants according to the properties of the material.For PS/PP materials,brominated flame retardants have the best effect,among which 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromopropoxy?benzene??BDDP??5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?has a good compatibility with the substrate,and has little impact on the properties of the materials.At present,the method of 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?with organic solvent is difficult to meet the requirements of environmental protection due to its high energy consumption,difficult discharge and high toxicity.In order to solve these problems,a synthetic method using water as solvent was developed.On the basis of the synthesis of 4,4'-?propane-2,2-diyl?bis??allyloxy?benzene?,the process of BDDP was further optimized,the optimum conditions for the synthesis of flame retardants of 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-??2-methylallyl?oxy?benzene?and 5,5'-?propane-2,2-diyl?bis?1,3-dibromo2-?2,3-dibromo-2-methylpropoxy?benzene?and the application of 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?in materials were explored.The synthesis of 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?by water instead of organic solvent was in line with the green synthesis of flame retardants.The by-product hydrogen bromide was converted into sodium bromide by adding sodium carbonate,which was conducive to increasing the solubility of liquid bromine in water and speeding up the reaction rate.The synthetic5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?was added to the building insulation material instead of hexabromocyclododecane,and its flame retardant performance was tested.The results showed that the flame retardant effect of methyl octabromoether was good.?1?In the aqueous phase,4,4'-?propane-2,2-diyl?bis??allyloxy?benzene?was synthesized from chloropropylene and bisphenol A,and A white solid was obtained.The influence of reaction temperature,material ratio and drip time on product yield was investigated.Etrabromoether was synthesized from chloropropylene and tetrabromobisphenol A in the aqueous phase by further optimizing the process.The reaction time was shortened from 7 h to 5 h,and the purity and yield reached 98%.In the synthetic tetrabromoether system,the octabromoether was synthesized by directly dropping bromine into liquid bromine,and the factors such as temperature,material ratio,time and different kinds of surfactant were studied,which solved the problem of low purity of raw material insoluble in aquatic products.The structure of the product was characterized by FTIR,¹H-NMR,¹³C-NMR,and the performance was analyzed by TGA.?2?Tetrabromobisphenol A-bis?2-methyl?allyl ether was synthesized in aqueous phase.The effects of material quantity,water dosage and raw material mass ratio,reaction temperature,drop time and other factors on product yield were investigated.FTIR,¹H-NMR,¹³C-NMR,MS were used to characterize the structure of the product.?3?Using the synthesized Tetrabromobisphenol A-bis?2-methyl?allyl ether as raw material and water as solvent,the white 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?was obtained with a purity of 88.2%and a yield of 98%.The admixture reaction of alkene and liquid bromine in aqueous phase was realized,and the problem of Tetrabromobisphenol A-bis?2-methyl?allyl ether insoluble in water and easy to agglomerate was solved by changing the temperature,dropping acceleration of liquid bromine and changing the type of surfactant.The side reaction product HBr and the addition of sodium carbonate to generate sodium bromide,conducive to the solution of liquid bromide,no exhaust gas,in line with the environmental protection requirements.?4?The process amplification experiment of Tetrabromobisphenol A-bis?2-methyl?allyl ether was carried out in a 2.5 L container,and the products obtained were compared with those on the market,which all met the market requirements.?5?The synthesized 5,5'-?propane-2,2-diyl?bis?1,3-dibromo-2-?2,3-dibromo-2-methylpropoxy?benzene?was combined with polypropylene and Sb₂O₃ to make flame retardant polypropylene masterbatch,and its flame retardant and mechanical properties were tested,with good results.