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Process for the recovery of cobalt catalysts from the products formed during the oxo reaction

机译:从羰基合成反应生成的产物中回收钴催化剂的方法

摘要

Cobalt is recovered from the degassed liquid product of a cobalt-catalysed oxo reaction by heating the product at a temperature of 100-190 DEG F. and at an absolute pressure of 10-25 p.s.i. with steam, separating from the resulting mixture an aqueous phase substantially free of cobalt, and removing cobalt from the remainder of the mixture. In one embodiment of the invention the steam is provided at atmospheric pressure or slightly above, and the mixture separates into three phases-a clear top organic phase, a clear aqueous phase and at the interface between the layers a thick black suspension containing the cobalt and referred to as the cobalt "interfacial rag". The liquid layers can be separated leaving the interfacial rag which can be recovered as a cobalt soap and recycled to the oxo reactor. In another modification the cobalt is converted into a form which passes into the organic layer by passing an oxygen-containing gas into the mixture either at the same time as or subsequently to passing in the steam. The organic layer is then separated and distilled to give a bottoms fraction containing cobalt which can be recycled to the oxo reactor. The oxygen-containing gas may be commercial oxygen, air, air diluted with inert gas. The interfacial rag may be converted to a form suitable for use as catalyst in the oxo reaction by treating it with sulphuric acid to form the sulphate, treating the sulphate with an alkali metal hydroxide and then adding an acid such as oleic acid, linoleic acid, stearic acid or tall oil acid. Alternatively the interfacial rag may be treated direct with the organic acid while passing oxygen into the mixture. Specification 682,177 is referred to.
机译:通过在100-190°F的温度和10-25p.s.i。的绝对压力下加热产物,从钴催化的羰基合成反应的脱气液体产物中回收钴。用蒸汽从所得混合物中分离出基本上不含钴的水相,并从混合物的其余部分中除去钴。在本发明的一个实施方案中,在大气压或稍高于常压下提供蒸汽,并且混合物分离成三个相:澄清的顶部有机相,澄清的水相以及在层之间的界面处的厚的黑色悬浮液,其包含钴和水。称为钴“界面碎布”。可以分离液体层,留下界面抹布,该界面抹布可以作为钴皂回收并循环到氧代反应器中。在另一种改型中,通过使含氧气体在与蒸汽同时或之后通过,使钴转化成通过有机层而进入有机层的形式。然后分离有机层并蒸馏,得到含有钴的塔底馏分,该塔底馏分可再循环至氧代反应器中。含氧气体可以是商业氧气,空气,用惰性气体稀释的空气。界面抹布可以通过用硫酸处理以形成硫酸盐,用碱金属氢氧化物处理硫酸盐,然后添加酸(例如油酸,亚油酸),硬脂酸或妥尔油酸。或者,可以在将氧气通入混合物的同时,用有机酸直接处理界面抹布。参考规格682,177。

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