Comprehensive Application of Various Instrumental Analytical Methods for the Analysis of a Polyurethane Product
摘 要
综合运用多种仪器分析方法剖析了一种聚氨酯产品。热重分析的结果显示: 此产品主要由挥发性组分、高分子聚合物和无机填料三部分组成,其中无机物的相对含量达19.5%。傅里叶变换红外光谱分析结果证明了此无机物为碳酸钙,而且还提示此产品中主要含有异氰酸酯和大分子多元醇反应所生成的预聚体以及大量增塑剂。根据凝胶渗透色谱图可知,此产品所含聚合物只有一种,其相对分子质量分布较宽,又根据顶空-气相色谱-质谱法(GC-MS)分析所得图谱可知,样品中的挥发性组分为乙苯、二甲苯、三甲苯和其它脂肪烷烃是作为稀释剂加入的;用13C核磁共振和DEPT-135谱以及裂解-GC-MS分析,样品中含有硅烷偶联剂KH-560、防霉剂和抗菌剂对甲苯磺酰胺(Ritcizer-8)和增塑剂邻苯二甲酸二癸酯(DDP);综合分析以上方法的结果,得知聚氨酯预聚体是甲苯二异氰酸酯(TDI)、聚丙二醇(PPG)的反应产物且由异氰酸根封端。
Abstract
Analysis of a polyurethane product of unknown composition was performed by comprehensive application of various instrumental analytical methods. It was found that: ① as shown by results of TGA, volatile substances, polymer, and inorganic filler are the 3 main components in the sample; ② as demonstrated in the FT-IR spectrum, the inorganic substance is CaCO3, and besides, pre-polymer formed by reaction between isocyanate and macro-molecular polyol alcohol and large amounts of plasticizer are also present; ③ as observed from the chromatogram of GPC, only one kind of polymer with widely distributed molecular mass is found in the sample; ④ as shown in the spectrum of HS-GC-MS, the volatile components are found to be ethylbenzene, xylene, trimethyl benzene and some other alkanes; which are added as diluents; ⑤ based on comprehensive study on the results of 13C NMR and DEPT-135 NMR spectrometry and Py-GC-MS analysis, a silane coupling agent KH-560, antifungal and anti-bacterial-Ritcizer-8 and a plasticizer DDP are present in the sample, and the pre-polymer of polyurethane is the product of reaction between TDI and PPG, with -N=C=O as its ending group.
中图分类号 O657
所属栏目 工作简报
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收稿日期 2013/9/11
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备注朱雪荣(1972-),男,浙江义乌人,博士,主要从事运用各种现代分析仪器综合剖析未知物。
引用该论文: ZHU Xue-rong. Comprehensive Application of Various Instrumental Analytical Methods for the Analysis of a Polyurethane Product[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2014, 50(10): 1268~1273
朱雪荣. 综合运用当代多种仪器分析技术剖析一种聚氨酯产品[J]. 理化检验-化学分册, 2014, 50(10): 1268~1273
被引情况:
【1】南洋,王振华, "气相色谱-质谱法测定复合食品包装材料中的2,4-二氨基甲苯",理化检验-化学分册 52, 211-213(2016)
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【3】周风山.一种商品蒸汽驱油用高温发泡剂组分剖析[J].分析化学, 2000,28(4): 452-453.
【4】陈和生,邵景昌,孙振亚.一种抗氧剂的剖析[J].理化检验-化学分册, 2012,48(4): 432-434.
【5】钟山.裂解毛细管柱气相色谱-傅里叶变换红外光谱的剖析应用[J].色谱, 1995,13(4): 274-276.
【6】吴励行.红外光谱在聚氨酯研究和生产中的应用[J].聚氨酯工业, 2000,15(1): 48-52.
【7】黄志萍,芦明.高效液相色谱分析及其在聚氨酯中的应用[J].聚氨酯工业, 1998,13(4): 46-48.
【8】柘植新,大古肇.高分辨裂解色谱原理与高分子裂解谱图集[M].金熹高,罗远芳,译.北京: 中国科学技术出版社, 1993: 312-319.
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【11】BOLGAR M, HUBBALL J, GROEGER J, et al. Handbook for the Chemical analysis of plastic and polymer additives[M]. Boca Raton: CRC Press, 2008: 19-27.
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