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:

1. [1]
  Shirayama, K., Okada, T. and Kita, S.I., J. Polym. Sci., Part B: Polym. Phys., 1965, 3(3): 907
2. [2]
  Desreux, V. and Spiegels, M.C., Bull. Soc. Chim. Belg., 1950, 59(7-8): 476
3. [3]
  Wild, L., Adv. Polym. Sci., 1991, 98: 1
4. [4]
  Anantawaraskul, S., Soares, J.B.P. and Wood-Adams, P.M., Adv. Polym. Sci., 2005, 182: 1
5. [5]
  Wild, L., Ryle, T.R., Knobeloch, D.C. and Peat, I.R., J. Polym. Sci., Part B: Polym. Phys., 1982, 20(3): 441
6. [6]
  Xu, J.T., Xu, X.R., Feng, L.X., Chen, L.S. and Chen, W., Macromol. Chem. Phys., 2001, 202(9): 1524
7. [7]
  Liu, Y.G. and Bo, S.Q., Int. J. Polym. Anal. Charact., 2003, 8(4): 225
8. [8]
  Kong, J., Fan, X.D., Xie, Y.C. and Qiao, W.Q., J. Appl. Polym. Sci., 2004, 94(4): 1710
9. [9]
  Xu, J.T. and Feng, L.X., Eur. Polym. J., 2000, 36(5): 867
10. [10]
  Zhang, B., Dong, Q., Fu, Z.S. and Fan, Z.Q., Polymer, 2014, 55(19): 4865
11. [11]
  Lu, X.Y., Yi. J.J., Chen, S.T., Zu, F.H. and Li, R.B., Chinese J. Polym. Sci., 2012, 30(1): 122
12. [12]
  Kang, J., Yang, F., Wu, T., Li, H.L., Cao, Y. and Xiang, M., Eur. Polym. J., 2012, 48(2): 425
13. [13]
  Liu, W.F., Wang, W.J., Fan, H., Yu, L.Q., Li, B.G. and Zhu, S.P., Eur. Polym. J., 2014, 54: 160
14. [14]
  Zhang, M.Q., Lynch, D.T. and Wanke, S.E., J. Appl. Polym. Sci., 2000, 75(7): 960
15. [15]
  Yau, W.W. and Gillespie, D., Polymer, 2001, 42(21): 8947
16. [16]
  Ortin, A., Monrabal, B. and Sancho, T.J., Macromol. Symp., 2007, 257: 13
17. [17]
  Yau, W.W., Macromol. Symp., 2007, 257: 29
18. [18]
  Mahdavi, H. and Enayati, N.M., J. Appl. Polym. Sci., 2008, 109(6): 3492
19. [19]
  Ko, Y.S., Jeon, J.K., Yim, J.H. and Park, Y.K., Macromol. Res., 2009, 17(5): 296
20. [20]
  Xue, Y.H., Fan, Y.D., Bo, S.Q. and Ji, X.L., Eur. Polym. J., 2011, 47(8): 1646
21. [21]
  Cheruthazhekatt, S., Pijpers, T.F.J., Harding, G.W., Mathot, V.B.F. and Pasch, H., Macromolecules, 2012, 45(15): 5866
22. [22]
  Lu, X.Y., Yi, J.J., Chen, S.T., Zu, F.H. and Li, R.B., Chinese J. Polym. Sci., 2012, 30(1): 122
23. [23]
  Xu, J.T, Xu, X.R. and Feng, L.X., Eur. Polym. J., 2000, 36(4): 685
24. [24]
  Fu, Q., Chiu, F.C., He, T.B, Liu, J.P. and Hsieh, E.T., Macromol. Chem. Phys., 2001, 202(6): 927
25. [25]
  Xue, Y.H., Wang, Y.H., Fan, Y.D., Yang, H.R., Tang, T., Bo, S.Q. and Ji, X.L., Chinese J. Polym. Sci., 2014, 32(6): 751
26. [26]
  Tackx, P. and Tacx, J., Polymer, 1998, 39(14): 3109
27. [27]
  Fu, Q., Du, R.N., Chiu, F.C. and He, T.B., Acta Polymerica Sinica (in Chinese), 2000, (2): 142
28. [28]
  Song, S.J., Feng, J.C., Wu, P.Y., Yang, Y.L. and Qiao, J.L., Polym. Bull., 2008, (3): 15
29. [29]
  Sun, X., Shen, G.H., Shen, H.W., Xie, B.H., Yang, W. and Yang, M.B., J. Polym. Sci., Part B: Polym. Phys., 2013, 52(10): 1372
30. [30]
  Chen, S.T., Huang, Q., Wu, L.M., Wang, Y.F. and Lou, L.J., Polym. Bull., 2012, (4): 97
31. [31]
  Galland, G.B., Mauler, R.S., DaSilva, L.P., Liberman, S., DaSilva, A.A. and Quijada, R., J. Appl. Polym. Sci., 2002, 84(1): 155
32. [32]
  Aust, N., Gahleitner, M., Reichelt, K. and Raninger, B., Polym. Test., 2006, 25(7): 896
33. [33]
  Mller, A.J. and Arnal, M.L., Prog. Polym. Sci., 2005, 30(5): 559
34. [34]
  Mller, A.J., Hernndez, Z.H., Arnal, M.L. and Snchez, J.J., Polym. Bull., 1997, 39(4): 465
35. [35]
  Zhang, M.Q. and Wanke, S.E., Polym. Eng. Sci., 2003, 43(12): 1878
36. [36]
  Fillon, B., Wittmann, J.C., Lotz, B. and Thierry, A., J. Polym. Sci., Part B: Polym. Phys., 1993, 31(10): 1383
37. [37]
  Mirabella, F.M. and Bafna, A., J. Polym. Sci., Part B: Polym. Phys., 2002, 40(15): 1637
38. [38]
  Pooter, M.De., Smith, P.B., Dohrer, K.K., Bennett, K.F., Meadows, M.D., Smith, C.G., Schouwenaars, H.P. and Geerards, R.A., J. Appl. Polym. Sci., 1991, 42(2): 399
39. [39]
  Soares, J.B.P. and Hamielec, A.E., Polymer, 1995, 36(8): 1639

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 929
HTML全文浏览量: 50

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs