羧基苯氧基酞菁钴的合成及其脱硫醇性能 |
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引用本文: | 崔娜 宋兆阳 朱丽君 夏道宏. 羧基苯氧基酞菁钴的合成及其脱硫醇性能[J]. 石油炼制与化工, 2016, 47(2): 60-64 |
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作者姓名: | 崔娜 宋兆阳 朱丽君 夏道宏 |
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作者单位: | 中国石油大学(华东)重质油国家重点实验室 |
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基金项目: | 中央高校基本科研业务费专项资金 |
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摘 要: | 以4-硝基邻苯二甲腈和5-羟基间苯二甲酸为原料,合成中间体4-(3,5-二羧基)苯氧基-邻苯二甲腈;在1,8-二氮杂二环十一碳-7-烯液相催化条件下,合成新型四-β-(间二羧基苯氧基)酞菁钴化合物;通过柱色谱分离方法对中间体进行提纯,利用红外光谱、1H-NMR以及MADLI-TOF-MS对中间体及最终产物进行表征。在液化气脱硫醇模拟体系中,对四-β-(间二羧基苯氧基)酞菁钴的催化性能进行评定。结果表明,所合成的新型酞菁钴类催化剂对丙硫醇和正丁硫醇转化率达到98.0%左右,对叔丁硫醇转化率达到68.2%,其脱硫醇性能优于工业应用催化剂。
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关 键 词: | 酞菁金属 合成 柱色谱分离 脱硫醇 |
收稿时间: | 2015-06-30 |
修稿时间: | 2015-07-25 |
SYNTHESIS OF DISCARBOXYL PHENOXY PHTHALOCYANINE COBALT AND APPLICATION IN OXIDATION DESULFURIZATION OF MERCAPTAN COMPOUNDS |
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Abstract: | The 4-(3,5-dicarboxy) phenoxyphthalonitrile as an intermediate was synthesized with 4-Nitrophthalonitrile and 5-hydroxy isophthalic acid as raw materials, followed by the purification by column chromatography. Afterwards, a new tetra -2(3), 9(10), 16(17), 23(24) - (3,5-discarboxylphenoxy) phthalocyanine cobalt was obtained from the intermediate under the catalytic action of 1,8-diazabicyclo undec-7-ene (DBU). The intermediate and the final product were characterized by mass spectrum, Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance (1H-NMR) and MADLI-TOF-MS techniques. The sweetening performance of the synthesized phthalocyanine cobalt was evaluated using mercaptan compounds and compared with the industrial catalysts. The sulfur conversions of n-propyl mercaptan and n-butyl mercaptan of the synthesized phthalocyanine cobalt are both around 98.0%, and for t-butyl mercaptan the conversion is 68.2%. The results show that the sweetening performance of the synthesized phthalocyanine cobalt is better than the industrial catalysts. |
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Keywords: | metallophthalocyanine synthesis column chromatography sweetening |
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