Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques

Satu terbitan siklik ditiokarbonat yang terdiri daripada getah asli terepoksida (ENR-50) dan tiga jenis hibrid ENR-50/titania (TiO2), ENR-50/zirkonia (ZrO2) dan kompleks ENR-50/stanum (Sn) telah disediakan. Teknik FTIR, 1D NMR; 1H-, 13C-, 119Sn-NMR, 2D NMR; HMQC, HMBC, COSY, TGA, DSC, TEM, SEM-EDX d...

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Main Author: Hamzah, Rosniza
Format: Thesis
Language:English
Published: 2015
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Online Access:http://eprints.usm.my/32036/1/Rosniza_Bt_Hamzah.pdf
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spelling my-usm-ep.320362019-04-12T05:25:43Z Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques 2015-06 Hamzah, Rosniza QD1-999 Chemistry Satu terbitan siklik ditiokarbonat yang terdiri daripada getah asli terepoksida (ENR-50) dan tiga jenis hibrid ENR-50/titania (TiO2), ENR-50/zirkonia (ZrO2) dan kompleks ENR-50/stanum (Sn) telah disediakan. Teknik FTIR, 1D NMR; 1H-, 13C-, 119Sn-NMR, 2D NMR; HMQC, HMBC, COSY, TGA, DSC, TEM, SEM-EDX dan XRD telah digunakan untuk mencirikan terbitan dan hibrid ENR. Suatu susunan triad ENR-50 berjaya ditandakan menggunakan teknik NMR dan gabungan terbitan siklik ditiokarbonat ENR-50. Suatu terbitan siklik ditiokarbonat ENR-50 telah disintesis daripada tindak balas ENR-50 dan karbon disulfide (CS2) dengan kehadiran mangkin 4-dimetilaminopridina (DMAP) pada suhu refluks (47 °C) selama 3 jam. Kedua-dua hibrid ENR/TiO2 dan ENR/ZrO2 telah disediakan daripada tindak balas pembukaan gelang epoksida ENR-50 pada keadaan berasid lembut (ENR-50 terawat asid) dan berbes (ENR-50 terawat bes) yang seterusnya ditindak balaskan dengan pemula masing-masing melalui teknik sol-gel pada suhu refluks (60 °C) selama 24 jam. Sumber pemula TiO2 dan ZrO2 masing-masing adalah Ti(OCH2CH2CH3)4 dan Zr(OCH2CH2CH3)4. A cyclic dithiocarbonate derivatives of epoxidized natural rubber (ENR-50) and three types of hybrids comprising ENR-50/titania (TiO2), ENR-50/zirconia (ZrO2) and ENR-50/tin (Sn) complex were prepared. FTIR, 1D NMR; 1H-, 13C-, 119Sn-NMR, 2D NMR; HMQC, HMBC, COSY, TGA, DSC, TEM, SEM-EDX and XRD techniques were used to characterize the ENR derivative and hybrids. A triad sequence of ENR-50 was successfully assigned using NMR techniques consolidated by the cyclic dithiocarbonate derivative of ENR-50. A cyclic dithiocarbonate derivative of ENR-50 was synthesized from the reaction of purified ENR-50 with carbon disulfide (CS2), in the presence of 4-dimethylaminopyridine (DMAP) as catalyst at reflux temperature (47 °C) for 3 hours. Both ENR/TiO2 and ENR/ZrO2 hybrids were prepared from epoxide ring opening reaction of ENR-50 at mild acidic (acid treated ENR-50) and basic (base treated ENR-50) conditions which later reacted with the respective precursors via sol-gel technique at reflux temperature (60 °C) for 24 hours. The respective source of TiO2 and ZrO2 precursors used were Ti(OCH2CH2CH3)4 and Zr(OCH2CH2CH3)4. 2015-06 Thesis http://eprints.usm.my/32036/ http://eprints.usm.my/32036/1/Rosniza_Bt_Hamzah.pdf application/pdf en public phd doctoral Universiti Sains Malaysia Pusat Pengajian Sains Kimia
institution Universiti Sains Malaysia
collection USM Institutional Repository
language English
topic QD1-999 Chemistry
spellingShingle QD1-999 Chemistry
Hamzah, Rosniza
Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
description Satu terbitan siklik ditiokarbonat yang terdiri daripada getah asli terepoksida (ENR-50) dan tiga jenis hibrid ENR-50/titania (TiO2), ENR-50/zirkonia (ZrO2) dan kompleks ENR-50/stanum (Sn) telah disediakan. Teknik FTIR, 1D NMR; 1H-, 13C-, 119Sn-NMR, 2D NMR; HMQC, HMBC, COSY, TGA, DSC, TEM, SEM-EDX dan XRD telah digunakan untuk mencirikan terbitan dan hibrid ENR. Suatu susunan triad ENR-50 berjaya ditandakan menggunakan teknik NMR dan gabungan terbitan siklik ditiokarbonat ENR-50. Suatu terbitan siklik ditiokarbonat ENR-50 telah disintesis daripada tindak balas ENR-50 dan karbon disulfide (CS2) dengan kehadiran mangkin 4-dimetilaminopridina (DMAP) pada suhu refluks (47 °C) selama 3 jam. Kedua-dua hibrid ENR/TiO2 dan ENR/ZrO2 telah disediakan daripada tindak balas pembukaan gelang epoksida ENR-50 pada keadaan berasid lembut (ENR-50 terawat asid) dan berbes (ENR-50 terawat bes) yang seterusnya ditindak balaskan dengan pemula masing-masing melalui teknik sol-gel pada suhu refluks (60 °C) selama 24 jam. Sumber pemula TiO2 dan ZrO2 masing-masing adalah Ti(OCH2CH2CH3)4 dan Zr(OCH2CH2CH3)4. A cyclic dithiocarbonate derivatives of epoxidized natural rubber (ENR-50) and three types of hybrids comprising ENR-50/titania (TiO2), ENR-50/zirconia (ZrO2) and ENR-50/tin (Sn) complex were prepared. FTIR, 1D NMR; 1H-, 13C-, 119Sn-NMR, 2D NMR; HMQC, HMBC, COSY, TGA, DSC, TEM, SEM-EDX and XRD techniques were used to characterize the ENR derivative and hybrids. A triad sequence of ENR-50 was successfully assigned using NMR techniques consolidated by the cyclic dithiocarbonate derivative of ENR-50. A cyclic dithiocarbonate derivative of ENR-50 was synthesized from the reaction of purified ENR-50 with carbon disulfide (CS2), in the presence of 4-dimethylaminopyridine (DMAP) as catalyst at reflux temperature (47 °C) for 3 hours. Both ENR/TiO2 and ENR/ZrO2 hybrids were prepared from epoxide ring opening reaction of ENR-50 at mild acidic (acid treated ENR-50) and basic (base treated ENR-50) conditions which later reacted with the respective precursors via sol-gel technique at reflux temperature (60 °C) for 24 hours. The respective source of TiO2 and ZrO2 precursors used were Ti(OCH2CH2CH3)4 and Zr(OCH2CH2CH3)4.
format Thesis
qualification_name Doctor of Philosophy (PhD.)
qualification_level Doctorate
author Hamzah, Rosniza
author_facet Hamzah, Rosniza
author_sort Hamzah, Rosniza
title Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
title_short Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
title_full Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
title_fullStr Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
title_full_unstemmed Structural Study Of Epoxidized Natural Rubber (Enr-50) And Its Derivatives Synthesized Via Epoxide Ring-Opening Reactions Using Nmr Techniques
title_sort structural study of epoxidized natural rubber (enr-50) and its derivatives synthesized via epoxide ring-opening reactions using nmr techniques
granting_institution Universiti Sains Malaysia
granting_department Pusat Pengajian Sains Kimia
publishDate 2015
url http://eprints.usm.my/32036/1/Rosniza_Bt_Hamzah.pdf
_version_ 1747820519104708608