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Preparation and characterization of cycloolefin polymer based on dicyclopentadiene (DCPD) and dimethanooctahydronaphthalene (DMON)

机译:基于二环戊二烯(DCPD)和二甲基辛基八氢萘(DMON)的环烯烃聚合物的制备与表征

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摘要

Ring-opening metathesis polymerization (ROMP) and subsequent hydrogenation of the mixture of dicyclopentadiene (DCPD) and 1,4,5,8-dimethano-1,2,3,4,4a,5,8, 8a-octahydronaphthalene (DMON) were conducted. ROMP was successfully performed at room temperature using WCl_6/iBu_3Al/2-BuOH (1/0.7/1.2) catalyst system when the DCPD/DMON molar ratio was 1. Depending on the DCPD/DMON molar ratio, the catalyst component ratio for the polymerization changed. The double bond in the prepared ROMP polymer could be completely hydrogenated using Ni(acac)_2/iBu_3Al at molar ratio of the Ni/double bond in polymer = 0.2 mol% and Al/Ni = 4 when the reaction was conducted at 80 C for 3 h. After hydrogenation, the glass transition temperature (T_g) of all ROMP polymers was decreased by 40 C. Depending on the DCPD and DMON molar ratio, the T_g of the ROMP polymer and hydrogenated ROMP polymer changed. The hydrogenated DCPD-DMON ROMP copolymer was characterized by using 2D ~1H-~1H COSY and 2D ~1H-~(13)C HSQC NMR spectroscopy. Thermal stability and light transmittance for the ROMP polymer and the hydrogenated ROMP polymer were compared by using TGA and UV.
机译:开环易位聚合(ROMP)和随后的双环戊二烯(DCPD)和1,4,5,8-二甲氧基-1,2,3,4,4a,5,8,8a-八氢萘(DMON)的混合物的氢化进行了。当DCPD / DMON摩尔比为1时,使用WCl_6 / iBu_3Al / 2-BuOH(1 / 0.7 / 1.2)催化剂体系在室温下成功进行ROMP。取决于DCPD / DMON摩尔比,用于聚合的催化剂组分比改变了。当在80°C下进行反应时,使用Ni(acac)_2 / iBu_3Al可以使聚合物中Ni /双键的摩尔比= 0.2 mol%和Al / Ni = 4完全氢化所制备的ROMP聚合物中的双键。 3小时氢化后,所有ROMP聚合物的玻璃化转变温度(T_g)降低40°C。根据DCPD和DMON摩尔比,ROMP聚合物和氢化的ROMP聚合物的T_g发生变化。通过使用2D〜1H-〜1H COZY和2D〜1H-〜(13)C HSQC NMR光谱对氢化的DCPD-DMON ROMP共聚物进行表征。通过使用TGA和UV比较ROMP聚合物和氢化ROMP聚合物的热稳定性和透光率。

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