Characterization of Poly(1-methyl-1,4-butanediol-1,4-diyl/2,3,4-trihydro-5-methylfuran-2,5-diyl) Prepared from Natural Rubber through 2D NMR Spectroscopy
Characterization of Poly(1-methyl-1,4-butanediol-1,4-diyl/2,3,4-trihydro-5-methylfuran-2,5-diyl) Prepared from Natural Rubber through 2D NMR Spectroscopy
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通过二维核磁共振波谱表征天然橡胶制备的聚（1-甲基-1,4-丁二醇-1,4-二基/2,3,4-三氢-5-甲基呋喃-2,5-二基）
DOI：
10.1002/app.34446
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发表时间：
2011
期刊：
影响因子：
--
通讯作者：
Y.Ohtake
中科院分区：
文献类型：
--
作者：
T.Saito;Y.Yamamoto;S.Kawahara;Y.Ohtake
以脱蛋白天然橡胶为原料，间氯过苯甲酸为环氧化剂，硫酸为水解剂，合成了聚（1-甲基-1，4-丁二醇-1，4-二基/2，3，4-三氢-5-甲基呋喃-2，5-二基）。通过FT-IR、1H NMR和13 C NMR光谱对所得产物进行表征。所有出现在1H和13 C NMR谱中的信号均通过无畸变增强极化转移（DEPT）、季碳观测（QUAT）、相关光谱（COSY）和异质多量子相关（HMQC）测量进行了归属。在确定了产物的一级结构后，以脱蛋白天然胶乳为原料，过氧乙酸和异丙醇为溶剂，一锅法合成了聚（1-甲基-1，4-丁二醇-1，4-二基/2，3，4-三氢-5-甲基呋喃-2，5-二基）。根据本研究中建立的任务，通过1H NMR光谱对所得产物进行了表征，并测量了其透气性，以作为薄膜进行实际应用。© 2011 Wiley Periodicals，Inc. J Appl Polym Sci，2011.
Poly(1‐methyl‐1,4‐butanediol‐1,4‐diyl/2,3,4‐trihydro‐5‐methylfuran‐2,5‐diyl) was prepared by epoxidation of deproteinized natural rubber withm‐chloroperbenzoic acid followed by hydrolysis with sulfuric acid. Characterization of the resulting product was performed through FT‐IR,1H NMR, and13C NMR spectroscopies. All signals appearing in the1H and13C NMR spectra were assigned by distortionless enhancement by polarization transfer (DEPT), quaternary carbon observation (QUAT), correlation spectroscopy (COSY), and heteronuclear multiple quantum correlation (HMQC) measurements. After proving the primary structure of the product, one pot synthesis of poly(1‐methyl‐1,4‐butanediol‐1,4‐diyl/2,3,4‐trihydro‐5‐methylfuran‐2,5‐diyl) from deproteinized natural rubber latex was carried out with peracetic acid and 2‐propanol. The resulting product was characterized by1H NMR spectroscopy on the basis of the assignments established in this study, and its gas permeability was measured for a practical application as a film. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011.