摘要
以草酸二乙酯、乙醇胺、二氯亚砜等为原料合成了一种能对聚丁二酸丁二醇酯(PBS)增黏,改善其加工性能的新型扩链剂2,2′-双(2-噁唑啉)(BOZ)。探讨了工艺条件对产物合成的影响。结果表明,当乙醇胺与草酸二乙酯的摩尔比为3:1,二氯亚砜与N,N′-二羟乙基草酰胺摩尔比为3:1,NaIH乙醇溶液浓度为2 mol／L,消除反应温度为80℃时所得BOZ产率最高。红外光谱分析表明,在1 621．55 cm-1和1 119．36 cm-1处存在-C=N和C- O-C的伸展振动峰,在918．68 cm-1处存在五元杂环的振动峰,证明合成的产物含噁唑啉环结构。紫外光谱分析表明合成产物中存在-N=C-C=N-共轭双键结构,元素分析进一步证明合成产物为BOZ。通过X-射线衍射和 DSC分析知BOZ为单斜晶系,熔点为210℃。对PBS的扩链研究发现扩链后PBS特性黏度由0．698 dL/g增加到 1．125 dL／g,羧值含量从56 mol／106g降到20 mol／106g,表明该扩链剂对PBS具有良好的扩链效果。
A novel chain extender for poly（butylenes succinate）（PBS）, 2,2＇-bis（2-oxazoline）, was synthesized from diethyl oxalate, ethanolamine, and thionyl chloride, whose composition was confirmed with element analysis. When molar ratio of ethanolamine to diethyl oxalate was 3 ： 1, thionyl chloride to N,N＇-dihydroxyethyl-oxamide was 3：1, the concentration of alcoholic sodium hydroxide solution was 2 mol/L, and the elimination reaction temperature was 80 ℃, a maximum yield was obtained. In the IR spectrum, the absorption peak at 1621.55 cm ^-1 and 1119.36 cm^-1 ensured the existences of --C=N-- and C--O---C respectively, and the band at 918.68 cm^-1 was the vibration of five-membered hetercycles, which confirmed the present of 2,2＇-Bis （2-oxazoline） structure. Furthermore UR spectrum showed the conjugate double bond of --N=C--C=N-- . XRI） and DSC suggested it be- longs to clinorhombic system with a melting point of 210 ℃. When introduced into PBS, the intrinsic viscosity of PBS increased form 0. 698 dL/g to 1. 125 dL/g, the carboxylic acid amount decreased from 56 mol/10^6 g to 20 mol/10^6 g, which proved an effective chain extension.
出处
《中国塑料》
CAS
CSCD
北大核心
2006年第3期94-98,共5页
China Plastics
基金
北京市委组织部优秀人才专项资金项目(20041D0500311)
