Preparation and characterization of high softening point and homogeneous isotropic pitches produced from distilled ethylene tar by a novel bromination method
Homogeneous isotropic pitches with high softening points were prepared from vacuum-distilled heavy residue ethylene tar (ET-HR) by a two-step method of bromination and subsequent dehydrobromination/polycondensation. The ET-HR was first brominated at 30 or 200 oC, and then heat-treated at 350 oC to e...
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| Published in | New carbon materials Vol. 33; no. 1; pp. 71 - 81 |
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| Main Authors | , , , , , |
| Format | Journal Article |
| Language | English |
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Elsevier Ltd
01.02.2018
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| Abstract | Homogeneous isotropic pitches with high softening points were prepared from vacuum-distilled heavy residue ethylene tar (ET-HR) by a two-step method of bromination and subsequent dehydrobromination/polycondensation. The ET-HR was first brominated at 30 or 200 oC, and then heat-treated at 350 oC to enable the dehydrobromination/polycondensation reactions. GC/MS and LDI TOF/MS spectra indicated that the ET-HR was mainly composed of compounds containing 3- to 6-ring aromatic species with a considerable aliphatic chain content. Compared with thermal condensation alone, such a two-step method increased the softening point of the pitches from 152 to 264 oC with a yield in the range of 62 wt. %−67 wt.% and a coking value in the range of 57 wt. %−77 wt.%, depending on the bromination temperature and the bromine content. Structural characterization of the as-prepared pitches by elemental analysis, 1H NMR, FT-IR and LDI-TOF/MS showed increased aromatization and polymerization of the precursor during the dehydrobromination/polycondensation. All the homogeneous isotropic pitches showed an ability to transform into an anisotropic texture after coking at 800 °C. |
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| AbstractList | Homogeneous isotropic pitches with high softening points were prepared from vacuum-distilled heavy residue ethylene tar (ET-HR) by a two-step method of bromination and subsequent dehydrobromination/polycondensation. The ET-HR was first brominated at 30 or 200 oC, and then heat-treated at 350 oC to enable the dehydrobromination/polycondensation reactions. GC/MS and LDI TOF/MS spectra indicated that the ET-HR was mainly composed of compounds containing 3- to 6-ring aromatic species with a considerable aliphatic chain content. Compared with thermal condensation alone, such a two-step method increased the softening point of the pitches from 152 to 264 oC with a yield in the range of 62 wt. %−67 wt.% and a coking value in the range of 57 wt. %−77 wt.%, depending on the bromination temperature and the bromine content. Structural characterization of the as-prepared pitches by elemental analysis, 1H NMR, FT-IR and LDI-TOF/MS showed increased aromatization and polymerization of the precursor during the dehydrobromination/polycondensation. All the homogeneous isotropic pitches showed an ability to transform into an anisotropic texture after coking at 800 °C. |
| Author | Qiao, Wen-ming Ling, Li-cheng Long, Dong-hui Yang, Hai-xiao Sun, Zhen-long Ge, Chuan-zhang |
| Author_xml | – sequence: 1 givenname: Chuan-zhang surname: Ge fullname: Ge, Chuan-zhang organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China – sequence: 2 givenname: Zhen-long surname: Sun fullname: Sun, Zhen-long organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China – sequence: 3 givenname: Hai-xiao surname: Yang fullname: Yang, Hai-xiao organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China – sequence: 4 givenname: Dong-hui surname: Long fullname: Long, Dong-hui email: longdh@mail.ecust.edu.cn organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China – sequence: 5 givenname: Wen-ming surname: Qiao fullname: Qiao, Wen-ming organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China – sequence: 6 givenname: Li-cheng surname: Ling fullname: Ling, Li-cheng email: lchling@ecust.edu.cn organization: State Key Laboratory of Chemical Engineering, East China University of Science and Technology, Shanghai 200237, China |
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| Keywords | Distillation Ethylene tar Properties Bromination Dehydrobromination |
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| Snippet | Homogeneous isotropic pitches with high softening points were prepared from vacuum-distilled heavy residue ethylene tar (ET-HR) by a two-step method of... |
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| SubjectTerms | Bromination Dehydrobromination Distillation Ethylene tar Properties |
| Title | Preparation and characterization of high softening point and homogeneous isotropic pitches produced from distilled ethylene tar by a novel bromination method |
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