Pan Zhi-quan
2013
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Journal
Chemistry & Bioengineering
Abstract
Phosphorus-nitrogen-bromine containing intumescent flame retardant bis(2,4,6-tribromophenyl) phosphoric dimelamine salt was synthesized from phenol,bromine,hydrogen peroxide,phosphorous oxychloride and melamine through the three-step method.The suitable synthetic conditions were obtained as follows:in the step one,the molar ratio 1∶1.55∶1.78 of phenol,bromine and hydrogen peroxide was used with ethanol as solvent,the yield of intermediate I reached 98.2%,in the step two,the molar ratio of intermediateⅠto phosphorous oxychloride was 2.3∶1 using phenol as solvent,pyridine as HCl acceptor,the yield of intermediate Ⅱ reached 89.1%,in the step three,DMSO was selected as solvent,the reaction temperature was 130 ℃,and the yield of target product Ⅲreached 95.8%.The structures of the intermediates and the target product were confirmed by FTIR and MS.