聚乙烯醇产品醇解度测定的核磁共振方法分析  

Investigation of nuclear magnetic resonance method for determining the alcoholysis degree of polyvinyl alcohol products

作　　者：邓东浩 张姝 张育红 王洪学 王建强 刘巍 Deng Donghao;Zhang Shu;Zhang Yuhong;Wang James H;Wang Jianqiang;Liu Wei(SINOPEC Shanghai Research Institute of Petrochemical Technology Co.,Ltd.,Shanghai 201208,China)

机构地区：[1]中石化(上海)石油化工研究院有限公司,上海201208

出　　处：《合成技术及应用》2023年第3期45-49,共5页Synthetic Technology & Application

摘　　要：聚乙烯醇(PVA)产品醇解度是影响产品品质和下游应用的一项重要指标,通常采用化学滴定法测定,但耗时耗力。目前文献报道的核磁共振波谱测定醇解度的方法虽然大大简化了实验流程,提高了测定速度,但大多存在谱峰指认不清导致测定结果误差较大的问题。本文优化了样品制备和测试条件,如溶剂、温度等,在此基础上通过一系列二维核磁实验对不同谱峰进行了准确的归属,并通过定量核磁实验进行了定性、定量分析。结果表明,3种^(1)H谱计算方法和^(13)C谱计算方法结果高度一致,并与滴定结果十分吻合。与定量^(13)C谱相比,定量^(1)H谱实验方法在10 min以内即可得到结果,是一种快速准确的聚乙烯醇产品醇解度测定方法。The alcoholysis degree of polyvinyl alcohol(PVA)is an important composition parameter affecting the properties and applications of PVA products.It is usually determined by a chemical titration method which is time-consuming and labor-intensive.Although a method of measuring alcoholysis degree by nuclear magnetic resonance(NMR)spectroscopy was reported in the literature which has significantly simplified the experimental process and improved the measurement efficiency,but it had the issue of large calculation errors caused by inaccurate peak identifications.In this paper,the sample preparation conditions and test conditions,such as solvent and dissolution temperature,were optimized.On this basis,different spectral peaks were accurately assigned through a series of two-dimensional NMR experiments,and the qualitative and quantitative analysis were carried out by quantitative NMR experiments.The results of three types of calculation methods based on^(1)H NMR spectrum and one type of calculation method based on^(13)C NMR spectrum were highly consistent and consistent with the titration method.By comparing the results,quantitative^(1)H NMR experiments method can get results within ten minutes,which is a fast and accurate method for determining the alcoholysis degree of PVA products.

关 键 词：聚乙烯醇 醇解度 核磁共振 定量方法 

分 类 号：TQ322[化学工程—合成树脂塑料工业]