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有机金属化合物的机械化学合成:一种大规模制造方法。

Mechanochemical synthesis of an organometallic compound: a high volume manufacturing method.

作者信息

Peters David W, Blair Richard G

机构信息

ATMI, 706 Houston Clinton Dr., Burnet, TX 78611, USA.

出版信息

Faraday Discuss. 2014;170:83-91. doi: 10.1039/c3fd00157a.

Abstract

Chemical vapor deposition (CVD) precursor chemicals are held to some of the highest purity levels in industry. Many metal reagents form stable, unbreakable adducts with the coordinating solvents that are necessary for solvating highly polar reagents. These adducts are undesirable and must be removed prior to usage. Herein we describe a mechanochemical approach to the synthesis of bis(n-propyltetramethylcyclopentadienyl)strontium that eliminates the use of strongly coordinating solvents. This method overcomes the solubility problems of the two reagents without the formation of stable, unbreakable adducts. We utilize a unique reactor geometry that facilitates mechanochemical syntheses while simplifying handling and allowing for "one pot" production. The synthesis was scaled to five hundred gram lot sizes in a six liter reactor. This technique is applicable to many syntheses and is linearly scalable - limited only by reactor size.

摘要

化学气相沉积(CVD)前驱体化学品的纯度在工业中处于极高水平。许多金属试剂会与用于溶解高极性试剂的配位溶剂形成稳定、难以分解的加合物。这些加合物是不理想的,必须在使用前去除。在此,我们描述了一种机械化学方法来合成双(正丙基四甲基环戊二烯基)锶,该方法无需使用强配位溶剂。此方法克服了两种试剂的溶解性问题,且不会形成稳定、难以分解的加合物。我们采用了独特的反应器几何结构,既便于机械化学合成,又简化了操作,并能实现“一锅法”生产。该合成反应在一个6升的反应器中扩大到了500克的批量规模。这项技术适用于许多合成反应,并且具有线性可扩展性——仅受反应器尺寸的限制。

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