CAJ | 학술논문

采用复式催化剂/缚酸剂体系,合成了六氯环三磷腈。研究了反应溶剂、投料比例、催化剂、反应时间和原料粒径对六氯环三磷腈产率的影响,优化了合成条件和纯化方法,并确定了最佳反应条件。采用熔点测试、元素分析、红外光谱、X射线衍射、核磁共振等测试手段对产物进行了表征。结果表明,所得产物为目标化合物。产率可稳定在75%～80%之间,产物纯度达到98%。在聚合反应前,需要用重结晶结合升华的方法对六氯环三磷腈单体进行精制,以使聚合反应顺利进行。
채용복식최화제/박산제체계,합성료륙록배삼린정。연구료반응용제、투료비례、최화제、반응시간화원료립경대륙록배삼린정산솔적영향,우화료합성조건화순화방법,병학정료최가반응조건。채용용점측시、원소분석、홍외광보、X사선연사、핵자공진등측시수단대산물진행료표정。결과표명,소득산물위목표화합물。산솔가은정재75%～80%지간,산물순도체도98%。재취합반응전,수요용중결정결합승화적방법대륙록배삼린정단체진행정제,이사취합반응순리진행。
Hexachlorocyclotriphosphazene was synthesized by adopting mixed catalyst/acid binding agent synthesis system.The influences of reaction solvent,ratio of reactants,catalysts,reaction time,reactant particle size on the yield were investigated.Synthetic conditions and purification method were optimized and the best reaction condition was determined.The product was characterized by melting point determination,elemental ana-lysis,infrared spectrometer（IR）,XRD and nuclear magnetic resonance（NMR）.The result showed that the pro-duct obtained is just the target compound.It turned out that the yield of the product was maintained at a level between 75% and 80%,and the purity of the product was increased to 98%.Before polymerization reaction,HCCP needs to be purified by recrystallization and sublimation for the polymerization reaction to be done smoothly.