本文選題：2-羥基-5-特辛基苯乙酮肟 + 合成優(yōu)化��； 參考：《江西理工大學》2014年碩士論文

【摘要】：我國銅冶煉以處理高品位銅礦的火法冶煉技術為主。經(jīng)過幾十年的生產(chǎn),我國很多銅礦已進入開采后期,富礦、易選礦資源己近枯竭,火法冶煉進入了無原料生產(chǎn)的困境,這使大力發(fā)展適宜處理低品位銅礦的濕法冶銅技術成為必要。萃取作為濕法冶銅的一個重要組成部分,有著十分重要的研究意義。其中,萃取劑的選取起著決定性的作用。目前,我國濕法冶銅工業(yè)所用的萃取劑很大程度上依賴進口。進口銅萃取劑價格昂貴,因此,研究利用國產(chǎn)化工原料,大力開發(fā)具有自主知識產(chǎn)權的銅萃取劑,對我國濕法冶銅技術發(fā)展有著現(xiàn)實而深遠意義。本文在芳香族羥酮肟萃取劑的結構基礎上,用特辛基對其芳環(huán)上的烷基取代基進行結構修飾,合成了2-羥基-5-特辛基苯乙酮肟。探討了其合成最佳工藝條件及其在酸性溶液中對銅的萃取條件及萃取效率。以四氯乙烯為溶劑,對特辛基苯酚、乙酰氯、無水Al Cl3和鹽酸羥胺為主要原料,采用分步合成法合成了2-羥基-5-特辛基苯乙酮肟。對特辛基酚在80℃下,與乙酰氯反應2.5 h,形成酚酯。接著升高溫度至100℃,在無水Al Cl3催化條件下,進行Frise重排反應3.5 h,得到了2-羥基-5-特辛基苯乙酮。后者與鹽酸羥胺在無水碳酸鈉作縛酸劑的條件下進行肟化反應,合成了目標產(chǎn)物2-羥基-5-特辛基苯乙酮肟。正交試驗優(yōu)化反應條件后,其平均收率達到68.4%。對合成產(chǎn)物進行傅里葉紅外光譜、紫外光譜、核磁共振和高效液相色譜檢測,綜合檢測表明合成產(chǎn)物為目標產(chǎn)物2-羥基-5-特辛基苯乙酮肟。高效液相色譜檢測表明產(chǎn)物純度大于99%。研究了2-羥基-5-特辛基苯乙酮肟在酸性溶液對銅的萃取與反萃性能。實驗結果表明:在溫度25℃,初始水相p H值=4,Cu2+濃度為4 g·L-1,2-羥基-5-特辛基苯乙酮肟銅萃取劑在稀釋劑中濃度為10%,水相和有機相的體積比(A/O)=1:1.5,振蕩時間3 min的條件下,銅萃取劑對銅的單級萃取率達到95.45%。在溫度25℃,H2SO4濃度為180 g·L-1,有機相與水相的相比(A/O)=1:1,反萃時間5 min的條件下,銅的單級反萃率達到94.35%。本文進一步完善了羥肟類萃取劑萃取銅的理論研究。所合成的萃取劑對銅有較好的萃取效果,可以作為進口銅萃取劑的候補;有望優(yōu)化羥肟萃取劑的復配體系;對提高濕法煉銅生產(chǎn)效率有很好的促進作用。
[Abstract]:After several decades of production, many copper mines in our country have entered the later period of mining, rich ore, easy mineral resources have been exhausted, and fire smelting has entered the difficult situation of raw material production, which makes it necessary to develop wet metallurgy technology suitable for treating low grade copper mines. As an important part of the wet metallurgy copper, it has a very important research significance. Among them, the selection of extractants plays a decisive role. At present, the extractant used in the wet metallurgy industry in China is largely dependent on the import. The imported copper extractant is very expensive. Therefore, the research and utilization of domestic chemical raw materials have been developed with great efforts. The copper extraction agent of the main intellectual property has a realistic and profound significance to the development of wet metallurgy of copper in China. On the basis of the structure of the aromatic hydroxyketoxime extractant, the structure modification of the alkyl substituents on the aromatic ring of the aromatic hydroxyketoxime was constructed and the 2- hydroxy -5- terocyl acetophenone oxime was synthesized, and the optimum synthesis conditions and its application were discussed. The extraction conditions and efficiency of copper in acid solution. Using four chloroethylene as the solvent, 2- hydroxyl -5- terocinyl acetophenone oxime was synthesized by step synthesis by step synthesis, with teocylphenol, acetyl chloride, anhydrous Al Cl3 and hydroxylamine hydrochloride as the main raw materials. The reaction of teocylphenol to acetyl chloride was 2.5 h, and the phenol ester was formed at 80 C. Then the temperature was raised to 10. At 0 C, under the condition of water free Al Cl3, Frise rearrangement reaction was 3.5 h, and 2- hydroxy -5- teoctyl acetophenone was obtained. The latter was oximed with hydroxylamine hydrochloride under the condition of anhydrous sodium carbonate as an acid binding agent. The target product 2- hydroxy -5- teroctyl acetophenone oxime was synthesized. The average yield of the product was 68.4 after the orthogonal test. The synthetic products were detected by Fourier transform infrared spectroscopy, ultraviolet spectroscopy, nuclear magnetic resonance and high performance liquid chromatography, and the synthetic products were detected as the target product 2- hydroxy -5- teoctyl acetophenone oxime. High performance liquid chromatography showed that the purity of the product was greater than 99%. and the extraction of 2- hydroxy -5- tertyl Acetophenone oxime in acid solution to copper The experimental results show that at 25 C, the initial water phase P H value =4, Cu2+ concentration is 4 g. L-1,2- hydroxyl -5- acetophenone oxime oxime copper extractant in the diluent concentration is 10%, the volume ratio of the water and organic phase (A/O) =1:1.5, oscillation time 3 min, copper extraction agent to copper single stage extraction rate to 95.45%. in the temperature 25 The concentration of H2SO4 is 180 G. L-1, the organic phase is compared with the water phase (A/O) =1:1, and the stripping time is 5 min. The single stage stripping rate of copper reaches 94.35%.. This paper further perfects the theoretical study on the extraction of copper by hydroxamic acid extractant. The synthesized extractant can be used as a candidate for copper extractant. The complex system of hydroxyl oxime extractant can improve the production efficiency of copper hydrometallurgy.
【學位授予單位】：江西理工大學
【學位級別】：碩士
【學位授予年份】：2014
【分類號】：TF811;TQ421.12

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