低聚GAP中引发剂残基的结构鉴定及其残余氯分析

为确定部分结构未知的工业级聚叠氮缩水甘油醚(GAP)中的残余氯含量,通过工业级低聚GAP(GAP-R)充分叠氮化制备了无氯低聚GAP(GAP-P)。采用电喷雾四级杆飞行时间质谱(ESI-Q-TOF-MS)、核磁共振定量碳谱(13C NMR)、傅里叶变换红外光谱(FT-IR)对GAP-R和GAP-P进行了精细的结构分析。确定了GAP-R中引发剂残基、残余氯含量、氯原子位置、平均聚合度和数均分子质量的分析方法。结果表明,GAP-R中引发剂残基为丙撑基,残留氯原子存在于GAP中间的结构单元上,氯含量为3.39%,平均聚合度为3.70,数均分子质量为439.57g/mol。

Structure Identification of Residual Group of the Initiator of GAP with Low Polymerization Degree and Its Residual Chlorine Analysis

To determine the residual chlorine content in the industrial grade glycidyl azide polymer (GAP) with unknown part structure ,the GAP without chlorine(GAP‐P) was prepared by sufficient azido reaction of industrial GAP with low pol‐ymerization degree(GAP‐R) .The fine structural analyses of GAP‐R and GAP‐P were performed by electrospray ionization‐quadrupole‐time of flight mass spectra (ESI‐Q‐TOF‐MS) ,quantitative 13 C nuclear magnetic resonance spectra (quantitative 13 C NMR) and Fourier transform infrared spectra (FT‐IR) .The analytical methods of the residual group of the initiator , the residual chlorine content ,chlorine atom position ,the average polymerization degree and the number average molecular weight of GAP‐R were determined .The results show that the residual groups of the initiators of GAP‐R are the propylidene groups ,and the residual chlorine atoms are on the internal structural units ,the chlorine content is 3 .39% ,the average de‐gree of polymerization is 3 .70 and the number average molecular weight is 439 .57 g/mol .