Synthetic method of 5-nonyl salicylaldoxime

Abstract

The invention discloses a synthetic method of 5-nonyl salicylaldoxime. The method comprises the following steps: a) mixing 4-nonyl phenol and a formaldehyde solution, adding an alkali as a catalyst, and reacting for 2 hours under the thermal insulation condition; b) standing the solution for layering, taking an organic layer and adding chloroform and a Dess-Martin reagent for reaction for 1-3 hours; c) sequentially washing the solution obtained after reaction in the step b) at room temperature by using a saturated sodium carbonate aqueous solution, a sodium thiosulfate aqueous solution and deionized water and standing for layering, then, adding alkali as a catalyst into the organic layer, dropwise adding a hydroxyl amine salt solution, and reacting for 3 hours under the thermal insulation condition; and d) adding sulfuric acid into the solution, standing for layering, washing the organic layer by using deionized water to be neutral, and removing the solvent to obtain 5-nonyl salicylaldoxime. The method provided by the invention is simple in operation step, mild in reaction condition, easy to control and safe, convenient to operate and free of flammable and combustible exhaust gas. Based on 4-nonyl phenol, the yield of products can reach over 98% and the purity can reach over 95%.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for synthesizing copper extractant 5-nonyl salicylaldoxime. Background technique [0002] Copper is an important non-ferrous metal with a wide range of industrial uses. At present, the technology of hydrometallurgy (leaching-extraction-electrodeposition) is mainly used to produce copper at home and abroad. In this process, extraction is to realize the separation of metals in the leachate. The key step, it can be said that the performance of the extractant directly affects the efficiency of copper extraction. Among the copper extractants that have been developed so far, they are mainly divided into oximes (ketoxime, aldoxime), β-diketones, and triamines. Among them, oxime extractants, especially aromatic aldoxime extractants (such as 5-nonyl salicylaldoxime) have the characteristics of large capacity, good extraction performance, and high extraction rate. The most wi...

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Problems solved by technology

[0003] U.S. Patent No. 5,260,487A discloses a preparation method of 5-nonyl salicylaldoxime. The method uses magnesium methoxide as a starting agent, and undergoes three-step synthesis of a salt-forming reaction, a formylation reaction, and an oximation reaction. The reaction process is intense and difficult to control. And there is a large amount of hydrogen generated, which has great safety hazards, and the amount of solvent used is large, recovery is difficult, the reaction time is long, the reaction temperature is high, and there are many side reactions. The yield (calculated by 4-nonylphenol) is only 86%, and the content is only 85%. %; Patent CN101326148A discloses a process of catalyzing the formylation reaction with a new catalyst mixture to obtain a higher yield of 95% (in terms of nonylphenol), and a higher purity of 95%, but the method uses short-distance distillation SPDU The intermediate 5-nonylsalicylaldehyde is distilled out, which requires high equipment, high temperature (160~240°C) and vacuum (1mmHg), high energy consumption, large solvent loss, and high cost. It is unfavorable for large-scale industrial production; patent CN101497576A discloses a kind of preparation method of 5-nonyl salicylaldoxime equally, and this method adopts the technique similar to U.S. Patent US5260487A, has the same shortcoming

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