Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

Citation: Yan-hu Xue, Shu-qin Bo, Xiang-ling Ji. Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation[J]. Chinese Journal of Polymer Science, 2015, 33(7): 1000-1008. doi: 10.1007/s10118-015-1648-5 shu

Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

1.
1. State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
2.
2. University of Chinese Academy of Sciences, Beijing 100049, China
3.
4.
State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
基金项目:
This work was financially supported by the National Natural Science Foundation of China (Nos. 20734006 and 50921062).

摘要: 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.

关键词:

English

Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

1.
1. State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
2.
2. University of Chinese Academy of Sciences, Beijing 100049, China
3.
4.
State Key Laboratory of Polymer Physics and Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Sciences, Changchun 130022, China
Received Date: 30 October 2014
Revised Date: 05 January 2015
Available Online: 05 July 2015
Fund Project:
This work was financially supported by the National Natural Science Foundation of China (Nos. 20734006 and 50921062).

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.

Key words:

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Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

English

Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

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Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

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Calibration Curve Establishment and Fractionation Temperature Selection of Polyethylene for Preparative Temperature Rising Elution Fractionation

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