Abstract
A series of copolymers of ethylene with 1-hexene synthesized using a metallocene catalyst are selected and mixed. The blend is fractionated via preparative temperature rising elution fractionation (P-TREF). All fractions are characterized via high-temperature gel permeation chromatography (GPC), 13C nuclear magnetic resonance spectroscopy (13C-NMR), and differential scanning calorimetry (DSC). The changes in the DSC melting peak temperatures of the fractions from P-TREF as a function of elution temperature are almost linear, thereby providing a reference through which the elution temperature of TREF experiments could be selected. Moreover, the standard calibration curve (ethylene/1-hexene) of P-TREF is established, which relates to the degree of short-chain branching of the fractions. The standard calibration curve of P-TREF is beneficial to study on the complicated branching structure of polyethylene. A convenient method for selecting the fractionation temperature for TREF experiments is elaborated. The polyethylene sample is fractionated via successive self-nucleation and annealing (SSA) thermal fractionation. A multiple-melting endotherm is obtained through the final DSC heating scan for the sample after SSA thermal fractionation. A series of fractionation temperatures are then selected through the relationship between the DSC melting peak temperature and TREF elution temperature.
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This work was financially supported by the National Natural Science Foundation of China (Nos. 20734006 and 50921062).
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Xue, Yh., Bo, Sq. & Ji, Xl. Calibration curve establishment and fractionation temperature selection of polyethylene for preparative temperature rising elution fractionation. Chin J Polym Sci 33, 1000–1008 (2015). https://doi.org/10.1007/s10118-015-1648-5
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DOI: https://doi.org/10.1007/s10118-015-1648-5