石油炼制与化工 ›› 2016, Vol. 47 ›› Issue (1): 93-100.

• 分析与评定 • 上一篇    下一篇

运用多谱学分析技术测定高黏聚?烯烃的结构

王京,吴燕珍,王乃鑫,祝馨怡   

  1. 中国石化石油化工科学研究院
  • 收稿日期:2015-07-13 修回日期:2015-08-22 出版日期:2016-01-12 发布日期:2015-12-31
  • 通讯作者: 王京 E-mail:wangjing.ripp@sinopec.com

DETERMINATION OF STRUCTURES OF HIGH VISCOSITY POLY ALPHA OLEFINS BY SEVERAL SPECTROSCOPY ANALYSIS TECHNOLOGIES

  • Received:2015-07-13 Revised:2015-08-22 Online:2016-01-12 Published:2015-12-31
  • Contact: Jing WANG E-mail:wangjing.ripp@sinopec.com

摘要:

为探究典型的高黏聚?烯烃的精细结构,采用飞行时间质谱、核磁共振波谱和红外光谱方法表征了一种高黏度聚?烯烃(PAO)的结构,确定了该PAO样品主要为聚1-癸烯烃类聚合物,及碳数分布、双键类型,以及蒸馏受热后裂解产物的结构信息。质谱结果显示:该PAO聚合度为2~21,其最强峰为五聚1-癸烯;各聚合度PAO几乎都可以检出单烯与链烷烃两类分子。核磁共振氢谱中可见亚乙烯基的同碳偶合烯氢双峰,表明该PAO中存在微量端烯键。经高真空度蒸馏后,蒸馏产物中烯键峰显著增强,表明蒸馏过程产生大量的热裂解产物。红外分析结果表明,PAO样品中的烯键为亚乙烯基双键型,进一步证明了PAO经加氢饱和后残余双键及热解新生成双键皆为端烯类,而非内烯类。

关键词: FD-TOF MS, 质谱, 核磁共振, 红外光谱, 聚?烯烃, 1-癸烯, 基础油

Abstract:

A kind of high viscosity poly alpha-olefin (PAO) as base oil was characterized by time of flight mass spectrometry, and infrared spectrum to investigate the structure of the sample and the fractions after distillation, as well as carbon number distributions and double bond types. The mass spectrometry results show that poly 1-decene with degrees of polymerization of 2-21 is the main component in the PAO sample; the strongest peak is attributed to the pentamer of 1-decene. Both single olefin and alkane can be observed in PAO with different degrees of polymerization. The coupled twin peaks of olefin and hydrogen with the same carbon number as vinylidene are observed by nuclear magnetic resonance 1H spectrum, indicating the existence of trace olefin bond at terminal position. The olefin peaks are much stronger after vacuum distillation, demonstrating the occurrence of thermal cracking. The FT-IR indicates that the olefin bound in PAO sample is the vinylidene double bond type, which proves that the remained double bound and newly produced double bound after hydro-saturation of PAO are terminal position double bound, not the internal olefin.

Key words: FD-TOF MS, mass spectrometry, nuclear magnetic resonance, infrared spectrum, PAO, 1-decene, base oil