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Chemistry
分离硫酸选择性结晶用双 - iminoguanidinium配体
分离硫酸选择性结晶用双 -  iminoguanidinium配体
JoVE Journal
Chemistry
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JoVE Journal Chemistry
Sulfate Separation by Selective Crystallization with a Bis-iminoguanidinium Ligand

分离硫酸选择性结晶用双 - iminoguanidinium配体

Full Text
8,813 Views
08:01 min
September 8, 2016

DOI: 10.3791/54411-v

Charles A. Seipp1,2, Neil J. Williams1,3, Radu Custelcean1

1Chemical Sciences Division,Oak Ridge National Laboratory, 2Department of Chemistry,The University of Texas at Austin, 3Department of Chemistry,The University of Tennessee

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Please note that some of the translations on this page are AI generated. Click here for the English version.

一种在双(iminoguanidinium)配位体及其在硫酸盐的选择性分离利用原位水性合成协议提出。

该程序的总体目标是通过使用从简单前驱体一步合成的双胍配体进行选择性结晶,将硫酸根阴离子从竞争性水溶液中分离出来。由于这种阴离子具有很强的亲水性,因此从竞争性水溶液中分离硫酸盐具有挑战性,并且通常需要难以合成和纯化的复杂受体。该技术的主要优点是它将原位配体合成和阴离子分离结合为一个步骤。要开始原位程序,将 10 毫升去离子水加入配备有磁力搅拌棒的圆底烧瓶中。然后加入 067 克对苯二甲醛和 2.2 毫升 0.5 摩尔的氨基胍氯化物水溶液。在 20 摄氏度下搅拌溶液 4 小时,这将产生略带黄色的大氯化物溶液。搅拌完成后,加入 0.5 毫升一摩尔的硫酸钠水溶液。这将沉淀出 1,4 苯双氨基硫酸胍为结晶白色固体。接下来,利用真空过滤回收 BIG 硫酸盐。用 5 毫升等分试样的水在滤纸上洗涤回收的固体 5 次,得到纯硫酸盐。使用粉末 X 射线折射,检查结晶 BIG 硫酸盐的相纯度,如前所述。对于非原位合成,首先设置一个带有搅拌棒和热板的 50 毫升圆底闪蒸。加入 20 毫升乙醇。接下来,加入 4 克对苯甲醛和 7.26 克氨基胍氯化物。将溶液加热至 60 摄氏度并搅拌 2 小时。然后将溶液冷却至 20 摄氏度,静置 3 小时。使用配备滤纸的 B

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