Synthesis,Characterization And Extractive Behaviors Of 2-hydroxy-5-octyl Phenyl Ethyl Ketoxime

Copper smelting was focused on treating high grade copper by pyrometallurgy in our country. After decades of development, many copper mines of our country enter the later exploiting period of copper. With the depletion of bonanza and easy dressing ores mineral resources, pyrometallurgy is trapped by raw materials, which make paying great attention to develop copper hydrometallurgy on treating low grade copper mine become necessary. As a significant process of copper hydrometallurgy, the study of extraction has very important significance, among which the selection of extractants plays crucial role on it. Extractant which is applied in industrial copper hydrometallurgy relies on imports to a large extent. For the expensive imported copper extractants, it has great realistic meaning and profound significance to research domestic raw materials to develop independent knowledge property copper extractant.In this paper, 2-hydroxy-5-octyl phenyl ethyl ketoxime were designed and synthesized based on the structure of aromatic hydroxyl ketone oxime extractants by modifying the alkyl substituents on the aromatic ring using p-(tert-octyl) phenol. The optimal synthetic processes and copper extraction condition and efficiency in acidic medium were studied.2-hydroxy-5-octyl phenyl ethyl ketoxime was prepared by three-step method using tetrachloroethylene as solvent, p-(tert-octyl)phenol, acetyl chloride, anhydrous aluminum chloride and hydroxylamine hydrochloride as raw material. At 80 ℃, p-(tert-octyl) phenol was reacted with acetyl chloride for 2.5 h to form phenolic ester. When the temperature was up to 100 ℃, it went on Frise rearrangement reaction for 3.5 h catalyzed by anhydrous Al Cl3 to get 2- hydroxyl-5- octyl hypnone. In order to obtain target product 2-hydroxy-5-octyl phenyl ethyl ketoxime, midbody would be reacted with hydroxylamine hydrochloride by oximation reaction with anhydrous Na2CO3 as acid-binding agent. The average yield achieved 68.4% after orthogonal optimization of the reaction conditions. The product was detected by fourier transform infrared spectroscopy, ultraviolet spectroscopy, nuclear magnetic resonance spectroscopy and high performance liquid chromatography. These detections showed that the product was 2-hydroxy-5-octyl phenyl ethyl ketoxime,and its purity was above 99% confirmed by the high performance liquid chromatography.The performance of extraction and stripping copper by 2-hydroxyl-5-octyl phenyl ethyl ketoxime in acid solution were studied. The results showed that when the temperature was 25 ℃, the aqueous initial p H was 4, Cu2+ concentration was 4 g·L-1, the concentration of 2-hydroxyl-5-octyl phenyl ethyl ketoxime copper extractant in diluents was 10%, the volume ratio of aqueous phase and organic phases(A/O) was 1:1.5, and the shaking time was 3 min, the copper extraction rate can reach 95.45% by one-stage extraction. And when the temperature was 25 ℃, H2SO4 concentration was 180 g·L-1, the volume ratio of aqueous phase and organic phases(A/O) was 1:1 and the shaking time was 3 min, the copper stripping rate can reach 94.35% by one-stage stripping.In this paper, the theoretical study on extraction copper with hydroxamic extractants is further improved. Because of the high copper extraction efficiency, the synthetic extractant can be a candidate for the imported copper extractants, optimizes the complex system of the hydroxamic extractants, and has an active effect on improving the production efficiency of the copper hydrometallurgy.