聚对苯二甲酸丙二醇酯在超临界甲醇中解聚产物的测定
Determination of solid products from the de-polymerization of poly(trimethylene terephthalate) in supercritical methanol.
作者信息
Zhang Changming, Xu Long, Zhang Haohong, Yang Jianli, Du Junmin, Liu Zhenyu
机构信息
State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, PR China.
出版信息
J Chromatogr A. 2004 Nov 5;1055(1-2):115-21. doi: 10.1016/j.chroma.2004.08.146.
A method based on high-resolution size-exclusion chromatography (SEC) was established to analyze the solid products from the depolymerization of poly(trimethylene terephthalate) (PTT) in supercritical methanol. In the qualitative analysis, four factors (chromatographic retention time, qualitative multi-wavelength ultraviolet spectra, linear internal-insert SEC and qualitative IR spectra) were considered. The main solid products from the process were dimethyl terephthalate (DMT), methyl-(2-hydroxypropyl) terephthalate (MHPT), bis(2-hydroxypropyl) terephthalate (BHPT), methyl-(2-hydroxyethyl) terephthalate (MHET), bis(2-hydroxyethyl) terephthalate (BHET), and hydroxyethyl-(2-hydroxypropyl) terephthalate (HEHPT). It is found that the method is of a high resolution among the solid products and has a fine repeatability. In addition, the solid products from the de-polymerization of poly(ethylene terephthalate) (PET) in similar process were also analyzed by this method. Furthermore, the effects of supercritical conditions on the distribution of the products were also discussed.
建立了一种基于高分辨率尺寸排阻色谱（SEC）的方法，用于分析聚对苯二甲酸丙二醇酯（PTT）在超临界甲醇中解聚得到的固体产物。在定性分析中，考虑了四个因素（色谱保留时间、定性多波长紫外光谱、线性内插SEC和定性红外光谱）。该过程的主要固体产物为对苯二甲酸二甲酯（DMT）、对苯二甲酸单（2-羟丙基）酯（MHPT）、对苯二甲酸双（2-羟丙基）酯（BHPT）、对苯二甲酸单（2-羟乙基）酯（MHET）、对苯二甲酸双（2-羟乙基）酯（BHET）和对苯二甲酸羟乙基-（2-羟丙基）酯（HEHPT）。结果表明，该方法对固体产物具有高分辨率且重复性良好。此外，还用该方法分析了聚对苯二甲酸乙二酯（PET）在类似过程中解聚得到的固体产物。此外，还讨论了超临界条件对产物分布的影响。
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