Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparat

来源 :Chinese Journal of Polymer Science | 被引量 : 0次 | 上传用户:zguohui69
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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), 13 C 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. 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) , 13 C 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. Furthermore, the standard calibration curve (ethylene / 1-hexene) of P-TREF is established, which relates to the degree of short-chain branching of the fractions. 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 A multiple of 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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