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Synthesis Of 5-decylsalicylaldoxime And 2-hydroxy-5-decylacetophenone Oxime And Research On The Extract Condition Of Copper(Ⅱ)

Posted on:2011-01-17Degree:MasterType:Thesis
Country:ChinaCandidate:S H ZhaoFull Text:PDF
GTID:2121330332964158Subject:Organic Chemistry
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There is abundant resource of copper deposit in our country. However, most of deposits of copper are associated minerals of low quality. An efficient technique of smelting the copper ore is using the process:"Leaching-Solvent Extraction-Electro winning". At a key step, an extractant plays a vital role at solvent-extract technology. At present, most of available copper extractants are imported and their cost is high, so the imported extractants hardly be applied by a lot of companies for our copper minerals of low quality. Therefore, the ultimate resolution is to exploit rather cheap copper extractants of ours.In the paper, two copper extractants 5-decylsalicylaldoxime and 2-hydroxy-5-decylacetophenone oxime were synthesized with the mixture of decene, cheap and industrial by-product from Sinopec Company, as raw material. Their synthetic technological conditions and copper-extract condition were investigated to obtain innovative resuts as follows:1. In a reagent a mixture of decene, 4-decylphenol was synthesized by Friedel-Crafts alkylation of phenol as raw material, successive formylation with paraformaldehyde to obtain 5-decylsalicyaldehyde, and condensation with hydroxylamine hydrochloride to achieve 5-decylsalicylaldoxime, the yield is 75.3% with 99.0% purity. In the formylation technology, material ratio, reaction time, reaction temperature and so on were discussed, and optimal condition has been obtained as follows: n (decylphenol): n (magnesium): n (paraformaldehyde) = 1:0.67:2.8, reaction time 5 h; reaction temperature 105°C. In oximation reaction of 5-decylsalicylaldehyde, material ratio and reaction time were discussed, and optimal condition has been found as follows: n (decylphenol): n (hydroxylamine hydrochloride) = 1:1, reaction time 1 h. The structure of all products and middle products were charactered by MS, NMR and element analysis. Its extraction performance was measured to show as follows: degree of saturation of copper is 6.36 g/L, fractionation factor of copper over ironβ[Cu/Fe] = 1340, the extracting and stripping balance time is as short as 4 min, the extracting rate is more than 98 % and the stripping extracting rate is more than 90 % through only one stage.The results have been shown that the extractant has higher copper-extract capability.2. The intermediate 4-decylphenol was reacted with acetyl chloride to get phenol ester, successive hot rearrangement at the catalysis of Lewis acid to obtain 2-hydroxy-5-decylacetophenone, and condensation with hydroxylamine hydrochloride to achieve target compound 2-hydroxy-5-decylacetophenone oxime. The mixture of 5-decylsalicylaldoxime and 2-hydroxy-5-decylacetophenone oxime in mass ratio of 1:1 was applied to extract copper to get the results as follows: The stripping extracting rate is more than 95.0% through only one stage. The fractionation factor of copper over ironβ[Cu/Fe] comes up to 1760. The data is shown that the mixture performance is superior to each component, their concerted effect has been reached.
Keywords/Search Tags:5-decylsalicylaldoxime, 2-hydroxy-5-decylacetophenone oxime, synthesis, extraction
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