摘要
分别运用离子液体[Bmim]BF_4和氯化镁两种不同的催化剂催化一步法合成环状磷酸酯阻燃剂,并进行红外、气相色谱和质谱等表征,探究合成效果最好的催化剂种类。结果发现,以离子液体为催化剂的一组相比于以氯化镁催化剂的一组,不仅反应快,而且合成的环状磷酸酯的产率很高。
Two different catalysts, ionic liquid [Bmim]BF_4 and magnesium chloride, were used to synthesize cyclic phosphate flame retardants by one-step method. The products were characterized by IR and gas chromatography-mass spectrometry to find out the type of catalyst with the best effect. The results show that ionic liquid [Bmim]BF_4 is a better catalyst for the synthesis of cyclic phosphate flame retardant. Not only the reaction is quick, but also the yield of synthetic cyclic phosphate is high.
引文
[1]SHEN G H,HONG J H.Recent advances in the synthesis of cyclic 5′-nornucleoside phosphonate analogues [J].Carbohydrate Research,2018,463:47-106.
[2]FANG W,SIYU P,PEIKUN Z ,et al.Synthesis and application of phosphorus-containing flame retardant plasticizer for polyvinyl chloride [J].Fibers and Polymers,2018,19(5):1057-1063.
[3]WANG S,DU Z,CHENG X ,et al.Synthesis of a phosphorus-and nitrogen-containing flame retardant and evaluation of its application in waterborne polyurethane [J].Journal of Applied Polymer Science,2018,135(6):46093.
[4]JANUSZEWSKI R,DUTKIEWICZ M,MACIEJEWSKI H,et al.Synthesis and characterization of phosphorus-containing,silicone rubber based flame retardant coatings [J].Reactive and Functional Polymers,2018,123:1-9.
[5]孙志松.环状磷酸酯无卤阻燃剂的合成与表征 [D].广州:华南理工大学,2013.
[6]马作广,倪忠斌,东为富,等.一种环状磷酸酯的合成及其阻燃性能测定 [J].精细化工,2018,35(2):320-325.
[7]ANDERSON J J,CAMACHO V G,KINNEY R E.Cyclic phosphonate esters and their preparation [P].US:3789091 A,1971-12-15.
[8]HOANG D Q,KIM J,JANG B N.Synthesis and performance of cyclic phosphorus-containing flame retardants [J].Polymer Degradation & Stability,2008,93(11):2042-2047.
[9]董春梅,孙才英,展召顺,等.离子液体[Bmim]BF4催化合成环状膦酸酯Antiblaze [J].精细化工,2011,28(6):581-584.
[10]BRADLEY A E,HARDACRE C,HOLBREY J D ,et al.Small-angle X-ray scattering studies of liquid crystalline 1-alkyl-3-methylimidazolium salts[J].Chemistry of Materials,2002,14(2):629-635.
[11]徐辉,桂奇飞,谌志华,等.碱性离子液体催化的一锅法合成4-氨基苯乙烯衍生物 [J].有机化学,2015,35(9):1910-1916.
[12]STEINRüCK H-P,WASSERSCHEID P.Ionic liquids in catalysis [J].Catalysis Letters,2015,145(1):380-397.