核磁共振法测定氟硅油的分子量和氟硅橡胶中乙烯基含量

波谱学杂志 ›› 1984, Vol. 1 ›› Issue (5): 429-436.

核磁共振法测定氟硅油的分子量和氟硅橡胶中乙烯基含量

俞槐根, 宓菊华

上海市有机氟材料研究所

收稿日期:1984-05-05 出版日期:1984-09-05 发布日期:2018-01-25

THE DETERMINATION OF MOLECULAR WEIGHT OF FLUORO SILICONS OIL AND VINYL GROUP IN FLUORO SILICONE RUBBER BY NMR

Yu Huaigen, Mi Juhua

Shanghai Institute of Organo-Fluorine Materials

Received:1984-05-05 Online:1984-09-05 Published:2018-01-25

摘要/Abstract

摘要： 用一系模型化合物归属了氟硅油和氟硅橡胶(聚甲基,r.r.r.三氟丙基硅氧烷,的¹H NMR谱,提出了一测定氟硅油分子量的方法。此法是基于端基的测量。对于甲基封端的氟硅油,
x=6S_CH₃(b)/S_CH₃(a),M=156x+162对于羟基封端的氟硅油,
x=((SCH₃(b))/SCH₃(a)+1)×2,M=156x+18
S_CH₃(a)和S_CH₃(b)分别为端甲基和其余的甲基的峰面积,x和M分别为聚合度和分子量。
使用高灵敏度的¹H NMR谱测定了氟硅橡胶中乙烯基含量和一系列共聚物的组成。
乙烯基 mole%=(S_-CH-CH₂)/S_-CH₂×(2)/3
S_-CH-CH₂和S_-CH₂分别是乙烯基和-CH₂基的峰面积。

Abstract: Proton NMR spectra of fluoro silicone oil and rubber (polymethyl r,r,r-trifluoropropyl siloxanes, have been assigned by using a series of modle compounds. A method was developed for the determination of molecular weight of oil. It was based on the measurment of end group.For oil ended bymethyl group,

For oil ended by hydroxy group,

S_{CH₃ (a)} and S_CH₃(b) are peak areas of end methyl group and remaining methyl group, respectively. X and M is polymerization degree and molecular weight, respectively.
High sensitive proton NMR spectra were used for the determination of vinyl group in rubber and composition in a series of copolymers,
vinyl mole%=(S_-CH-CH₂)/S_-CH₂×(2)/3
S_-CH=CH₂ and S_-CH₂, are peak areas of vinyl group and -CH₂, group, respectively.

俞槐根, 宓菊华. 核磁共振法测定氟硅油的分子量和氟硅橡胶中乙烯基含量[J]. 波谱学杂志, 1984, 1(5): 429-436.

Yu Huaigen, Mi Juhua. THE DETERMINATION OF MOLECULAR WEIGHT OF FLUORO SILICONS OIL AND VINYL GROUP IN FLUORO SILICONE RUBBER BY NMR[J]. Chinese Journal of Magnetic Resonance, 1984, 1(5): 429-436.