以9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)与三聚氰胺(MEL)为原料制备了一种含磷、氮以及苯环的新型阻燃剂(DOPO-MEL)。通过X射线衍射仪、傅立叶红外光谱仪与电喷雾阳离子质谱分析验证了其结构,并将其与聚磷酸铵(APP)复配阻燃聚丙烯(PP)。结果表明:DOPO-MEL与APP具有良好的协同阻燃效应。将30%(质量分数,其中DOPO-MEL∶APP=1∶2)的膨胀型阻燃体系添加于PP时,复合材料的极限氧指数(LOI)为29.4%,且能够通过UL-94测试V0级别。
A novel flame retardant,containing phosphorous,nitrogen and benzene rings,was prepared with 9,10-dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) and melamine (MEL).The X-ray diffraction (XRD),Fourier transform infrared(FT-IR) spectra and the electrospray ionization mass spectrometry (ESI-MS) were introduced to analyze the chemical structure of DOPO-MEL.An intumescent flame-retardant system (IFRs) composed of DOPO-MEL and ammonium polyphosphate (APP) was applied to polypropylene (PP).Results revealed that DOPO-MEL and APP had an excellent synergistic effect.Loaded with 30wt% of IFRs (DOPO-MEL∶APP=1∶2),PP/IFRs composite showed promising flame retardancy,UL-94 test passed V0 rating and LOI value was up to 29.4%.
[1] Li Y T,Li B,Dai J F,et al.Synergistic effects of lanthanum oxide on a novel intumescent flame retardant polypropylene system[J].Polymer Degradation and Stability,2008,93(1):9-16.
[2] Wang D Y,Das A,Costa F R,et al,Synthesis of organo cobalt-aluminum layered double hydroxide via a novel single-step self-assembling method and its use as flame retardant nanofiller in PP[J].Langmuir,2010,26(17):14162-14169.
[3] Chen X C,Ding Y P,Tang T.Synergistic effect of nickel formate on the thermal and flame-retardant properties of polypropylene[J].Polymer International,2005,54(6):904-908.
[4] Li B,Xu M J.Effect of a novel charring-foaming agent on flame retardancy and thermal degradation of intumescent flame retardant polypropylene[J].Polymer Degradation and Stability,2006,91(6):1380-1386.
[5] Peng H Q,Zhou Q,Wang D Y,et al.A novel charring agent containing caged bicyclic phosphate and its application in intumescent flame retardant polypropylene systems[J].Journal of Industrial and Engineering Chemistry,2008,14(5):589-595.
[6] Lin H J,Yan H,Liu B,et al.The influence of KH-550 on properties of ammonium polyphosphate and polypropylene flame retardant composites[J].Polymer Degradation and Stability,2011,96(7):1382-1388.
[7] 张金凯,马丽,葛维娟,等.膨胀型阻燃剂阻燃聚丙烯的研究进展[J].材料导报,2015,29(5):68-72.
[8] 王海军,陈立新,缪桦.氮系阻燃剂的研究及应用概况[J].热固性树脂,2005,20(4):36-41.
[9] 张丽丽,李斌,赵巍,等.新型大分子磷氮阻燃剂的合成及其在阻燃聚碳酸酯中的应用[J].合成化学,2012,20(3):334-336.
[10] Chen L,Wang Y Z.A review on flame retardant technology in China.part 1:development of flame retardants[J].Polymers for Advanced Technologies,2010,21(1):1-26.
[11] 张金凯.DOPO功能化的新型疏水聚磷酸铵的制备及在PP中的应用[D].太原:太原理工大学,2015.
[12] Liao S H,Liu P L,Hsiao M C,et al.One-step reduction and functionalization of graphene oxide with phosphorus-based compound to produce flame-retardant epoxy nanocomposite[J].Industrial & Engineering Chemistry Research,2012,51(12):4573-4581.
[13] Gu L Q,Chen G A,Yao Y W.Two novel phosphorus-nitrogen-containing halogen-free flame retardants of high performance for epoxy resin[J].Polymer Degradation and Stability,2014,108:68-75.
[14] Wu Z J,Li J L,Chen Y P,et al.Synthesis and liquid oxygen compatibility of a phosphorous-containing epoxy resin[J].Polymer Engineering and Science,2015,55(3):651-656.
[15] Veisi H,Hamelian M,Hemmati S.Palladium anchored to SBA-15 functionalized with melamine-pyridine groups as a novel and efficient heterogeneous nanocatalyst for Suzuki-Miyaura coupling reactions[J].Journal of Molecular Catalysis A-Chemical,2014,395:25-33.
[16] Mircescu N E,Oltean M,Chis V,et al.FT-IR,FT-raman,SERS and DFT study on melamine[J].Vibrational Spectroscopy,2012,62(9):165-171.
基金资助
国家青年科学基金(21306124);山西省自然科学基金(2015011035)