Study On The Synthesis And Flame Retardant Property Of Tris(2,4,6-tribromophenoxy)-Triazine

Tris?2,4,6-tribromophenoxy?-triazine?TTBPC?is a kind of additive brominated flame retardant with synergistic effect of nitrogen and bromine in molecule,which is applied to acrylonitrile-butadiene-styrene copolymer?ABS?and HIPS and other plastics due to its characteristics of high temperature resistance,good light and heat stability,good compatibility with resin and good processing performance.However,there are few reports on the synthesis and application of TTBPC in China,so it is significant to carry out the synthesis and application research.In this paper,TTBPC is synthesized through bromination and condensation,which taked 2,4,6-tribromophenol?TBP?,Br₂,H₂O₂ and cyanuric chloride as raw materials.The results showed that the optimum condition of the synthesis of TBP was as follows:the temperature of adding Br₂ being 20?,n?TBP?:n?Br₂?:n?H₂O₂?=1:1.53:1.60,the reaction temperature being 40?and the reaction time being 4 h.Under above conditions,the yield of TBP was 98%and the mass fraction of TBP was 99.8%;the optimum condition of the synthesis of TTBPC was as follows:the catalyst being N?CH₂CH₃?₃?TBN?,the temperature of adding cyanuric chloride being 20?,the stirring rate being 350 r/min,n?TBP?:n?NaOH?:n?TCT?:n?DCM?=3:3:0.95:28.6,m?DCM?:m?H₂O?=4:1,m?TCT?:m?TBN?=25.8:1,the reaction temperature being40?and the reaction time being 2.5 h.On this condition,the total yield of TTBPC was 94.5%and the mass fraction of TTBPC was 98.5%,the melting point was 228.5²32.2?.The results of TGA and DSC revealed that synthesized TTBPC had excellent thermal stability,T_1wt%,T_2wt%,T_5wt%were 355.24?,362?and 373?,respectively,and the temperature of maximum weight loss rate was 412.63?.Test results show that the differential scanning calorimeter,the glass transition temperature was228.29²33.63?.The flame retardancy of TTBPC in ABS and HIPS was researched by limiting oxygen index?LOI?measurement,vertical burning test and cone calorimetry test.The results indicated that TTBPC/Sb₂O₃ had good flame retardancy in ABS and HIPS.When the addtion amount of TTBPC/Sb₂O₃ is 15wt.%based on the total weight of material and m?TTBPC?:m?/Sb₂O₃?=4:1,LOI of flame retardant ABS and HIPS reached up to 29.7%and 25.0%respectively,vertical burning level all pass V-0.Compared with pure ABS,total heat release?THR?,peak heat release rate?PHRR?,mean heat release rate?MHRR?,average effective combustion heat?MEHC?and mean mass loss rate?MMLR?of flame retardant ABS were reduced by 58.6%,55.9%,55%,47.3%and 18.3%,respectively;Compared with pure HIPS,THR,PHRR,MHRR,MEHC and MMLR of flame retardant HIPS were reduced respectively by 50%,62.6%,52%,19.6%and 50%.