核磁共振技术分析橡胶制品表面喷霜成分

引用本文: 张文浩, 兰英嘉, 陆成华, 孙子渊, 陆焕钧, 李晓虹, 屠迎锋. 核磁共振技术分析橡胶制品表面喷霜成分[J]. 分析化学, 2023, 51(3): 405-411. doi: 10.19756/j.issn.0253-3820.221376 shu

Citation: ZHANG Wen-Hao, LAN Ying-Jia, LU Cheng-Hua, SUN Zi-Yuan, LU Huan-Jun, LI Xiao-Hong, TU Ying-Feng. Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface[J]. Chinese Journal of Analytical Chemistry, 2023, 51(3): 405-411. doi: 10.19756/j.issn.0253-3820.221376 shu

核磁共振技术分析橡胶制品表面喷霜成分

张文浩 ^1, ,
兰英嘉 ^1, ,
陆成华 ^2, ,
孙子渊 ^2, ,
陆焕钧 ^3, ,
李晓虹 ^{1,
,} ,
屠迎锋 ^{1,
,}

1.
苏州大学材料与化学化工学部, 苏州 215123;
2.
苏州华东橡胶工业有限公司, 苏州 215000;
3.
苏州科技大学物理科学与技术学院, 江苏省微纳热流技术与能源应用重点实验室, 苏州 215009

通讯作者: 李晓虹,Email:lxh83@suda.edu.cn; 屠迎锋,Email:tuyingfeng@suda.edu.cn

基金项目:
国家自然科学基金项目(No.22071167)资助。

摘要: 采用扫描电子显微镜(SEM)与能谱仪(EDS)联用技术、定量核磁共振氢谱(Quantitative ¹H NMR)以及二维核磁共振扩散序谱(DOSY)技术,对橡胶制品表面的喷霜成分进行了分析。EDS测试结果表明,喷霜所含元素为C、O、S和Zn,质量比约为6:1:1:1。¹H NMR结合DOSY证实喷霜析出物为硬脂酸锌、二甲基二硫代氨基甲酸锌(ZDMC)、2-巯基苯并噻唑(MBT)以及橡胶防护蜡,相应各物质的相对质量含量比值为38.9:31.5:14.4:15.2。按照各物质中C、O、S和Zn各元素的含量,得到其比值为5.70:0.44:1.28:1。通过计算得到的各组分含量,可推测出其相应的形成机理。ZnO和硬脂酸生成硬脂酸锌,TMTD和ZnO在硫化阶段生成ZDMC。本研究首次将DOSY与¹H NMR结合用于橡胶制品表面喷霜混合物的成分分析,为混合物组成分析提供了一种新思路。

关键词:

English

Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface

1.
College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou 215123, China;
2.
Su Zhou Hua Dong Rubber Industrial CO., Ltd., Suzhou 215000, China;
3.
Jiangsu Key Laboratory for Micro and Nano Heat Fluid Flow Technology and Energy Application, School of Physical Science and Technology, Suzhou University of Science and Technology, Suzhou 215009, China

Corresponding author: LI Xiao-Hong, ; TU Ying-Feng,

Received Date: 06 July 2022
Revised Date: 09 February 2023
Fund Project:
Supported by the National Natural Science Foundation of China (No. 22071167).

Abstract: Scanning electron microscopy (SEM) coupled with energy spectrometry (EDS), quantitative proton nuclear magnetic resonance (¹H NMR) and two-dimensional diffusion-ordered spectroscopy (DOSY) techniques were applied to analyze the composition of blooming. The EDS results indicated that the elements in the blooming were carbon, oxygen, sulfur and zinc with the mass ratio of 6∶1∶1∶1. Quantitative ¹H NMR combined with DOSY strongly convinced that the main precipitates of the blooming were zinc stearate, zinc dimethyl dithiocarbamate (ZDMC), 2-mercaptobenzothiazole (MBT) and rubber protective wax. Their corresponding mass content ratio was 38.9% : 31.5% : 14.4% : 15.2%, based on which the content ratio of element C, O, S and Zn was estimated as 5.70 ∶0.44 ∶1.28∶1. Then the possible formation mechanism of blooming was proposed. ZnO reacted with S to form ZnS, followed by the reaction of ZnS and stearic acid to generate zinc stearate. Moreover, tetramethyl thiuram disulfide (TMTD) could react with ZnO to produce ZDMC during the vulcanization stage. The DOSY and quantitative ¹H NMR spectroscopy were used together for the first time to analyze the components of blooming mixture on the surface of rubber products, which opened a new avenue to analyze unknown mixtures.

Key words:

Ethylene-propylene-diene rubber
/ Blooming
/ Quantitative proton nuclear magnetic resonance
/ Two-dimensional diffusion-ordered spectroscopy

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

核磁共振技术分析橡胶制品表面喷霜成分

通讯作者: 李晓虹,Email:lxh83@suda.edu.cn; 屠迎锋,Email:tuyingfeng@suda.edu.cn

English

Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface

Corresponding author: LI Xiao-Hong, ; TU Ying-Feng,

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

核磁共振技术分析橡胶制品表面喷霜成分

通讯作者: 李晓虹,Email:lxh83@suda.edu.cn; 屠迎锋,Email:tuyingfeng@suda.edu.cn

English

Application of Nuclear Magnetic Resonance Technology in Component Analysis of Blooming on Rubber Product Surface

Corresponding author: LI Xiao-Hong, ; TU Ying-Feng,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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