發(fā)布時(shí)間：2018-05-25 18:10

  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(xué)》2014年碩士論文

【摘要】：我國(guó)銅冶煉以處理高品位銅礦的火法冶煉技術(shù)為主。經(jīng)過(guò)幾十年的生產(chǎn),我國(guó)很多銅礦已進(jìn)入開(kāi)采后期,富礦、易選礦資源己近枯竭,火法冶煉進(jìn)入了無(wú)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(shù)成為必要。萃取作為濕法冶銅的一個(gè)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(guó)濕法冶銅工業(yè)所用的萃取劑很大程度上依賴進(jìn)口。進(jìn)口銅萃取劑價(jià)格昂貴,因此,研究利用國(guó)產(chǎn)化工原料,大力開(kāi)發(fā)具有自主知識(shí)產(chǎn)權(quán)的銅萃取劑,對(duì)我國(guó)濕法冶銅技術(shù)發(fā)展有著現(xiàn)實(shí)而深遠(yuǎn)意義。本文在芳香族羥酮肟萃取劑的結(jié)構(gòu)基礎(chǔ)上,用特辛基對(duì)其芳環(huán)上的烷基取代基進(jìn)行結(jié)構(gòu)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(duì)銅的萃取條件及萃取效率。以四氯乙烯為溶劑,對(duì)特辛基苯酚、乙酰氯、無(wú)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(duì)特辛基酚在80℃下,與乙酰氯反應(yīng)2.5 h,形成酚酯。接著升高溫度至100℃,在無(wú)水Al Cl3催化條件下,進(jìn)行Frise重排反應(yīng)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(wú)水碳酸鈉作縛酸劑的條件下進(jìn)行肟化反應(yīng),合成了目標(biāo)產(chǎn)物2-羥基-5-特辛基苯乙酮肟。正交試驗(yàn)優(yōu)化反應(yīng)條件后,其平均收率達(dá)到68.4%。對(duì)合成產(chǎn)物進(jìn)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(cè),綜合檢測(cè)表明合成產(chǎn)物為目標(biāo)產(chǎn)物2-羥基-5-特辛基苯乙酮肟。高效液相色譜檢測(cè)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(duì)銅的萃取與反萃性能。實(shí)驗(yàn)結(jié)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(jī)相的體積比(A/O)=1:1.5,振蕩時(shí)間3 min的條件下,銅萃取劑對(duì)銅的單級(jí)萃取率達(dá)到95.45%。在溫度25℃,H2SO4濃度為180 g·L-1,有機(jī)相與水相的相比(A/O)=1:1,反萃時(shí)間5 min的條件下,銅的單級(jí)反萃率達(dá)到94.35%。本文進(jìn)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(duì)銅有較好的萃取效果,可以作為進(jìn)口銅萃取劑的候補(bǔ);有望優(yōu)化羥肟萃取劑的復(fù)配體系;對(duì)提高濕法煉銅生產(chǎn)效率有很好的促進(jìn)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(xué)位授予單位】：江西理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：TF811;TQ421.12

【相似文獻(xiàn)】

相關(guān)期刊論文 前10條

1 劉忻;;2,4二羥基苯乙酮肟快速和選擇性分光光度測(cè)定鋼和合金中的錳[J];上海金屬.有色分冊(cè);1993年04期

2 C.Kesava Rao;許孫曲;許菱;;應(yīng)用2,4-二羥基苯乙酮肟快速、選擇性分光光度法測(cè)定鋼和合金中的錳[J];中國(guó)錳業(yè);1993年06期

3 楊春龍,蔣木庚,倪玨萍,俞幼芬,張湘寧;2,4-二氯苯乙酮肟羧酸酯及其ω-氯代衍生物的合成和生物活性研究[J];南京農(nóng)業(yè)大學(xué)學(xué)報(bào);2003年02期

4 薛偉;宋寶安;汪華;何偉;楊松;金林紅;胡德禹;劉剛;盧平;;2-[5-(3,4,5-三甲氧基苯基)-1,3,4-噻二唑-2-基硫代]-1-(2,3,4-三甲氧基)苯乙酮肟醚合成與抗煙草花葉病毒活性研究[J];有機(jī)化學(xué);2006年05期

5 李效軍;馮成;李春英;陳煒;;萃取劑2-羥基-5-壬基苯乙酮肟的合成[J];天津化工;2007年01期

6 許艷;袁莉萍;曹瑾;倪長(zhǎng)春;沈宙;陳亮;張一賓;;對(duì)氯苯乙酮肟醚衍生物的合成及生物活性[J];農(nóng)藥學(xué)學(xué)報(bào);2007年01期

7 G.V.Ramana Murthy ,游建南;用2-羥苯乙酮肟萃取和同時(shí)分光光度測(cè)定混合物中釩(Ⅳ)和釩(Ⅴ)[J];濕法冶金;1990年02期

8 周強(qiáng),龔大春,羅少華,崔曉玲,趙儒銘;對(duì)羥基苯乙酮肟的合成研究[J];湖北化工;1998年05期

9 楊春龍,蔣木庚,俞幼芬,倪玨萍,張湘寧;2種ω-1H-1,2,4-三氮唑基-2,4-二氯苯乙酮肟羧酸酯的合成及生物活性[J];精細(xì)化工;2003年02期

10 王新宇;閆書(shū)一;;高效萃取劑LIX841的合成及應(yīng)用[J];四川化工;2010年01期

相關(guān)會(huì)議論文 前2條

1 李蕾蕾;李大成;王大奇;竇建民;;2,4-二羥基苯乙酮肟錳金屬配合物的合成與表征[A];中國(guó)化學(xué)會(huì)第28屆學(xué)術(shù)年會(huì)第8分會(huì)場(chǎng)摘要集[C];2012年

2 章永潔;王亞權(quán);劉騰飛;米鎮(zhèn)濤;吳魏;閔恩澤;;鈦硅分子篩催化苯乙酮氨肟化反應(yīng)研究[A];第一屆全國(guó)化學(xué)工程與生物化工年會(huì)論文摘要集(下)[C];2004年

相關(guān)博士學(xué)位論文 前1條

1 馬亞團(tuán);新型苯乙酮衍生物的合成及其生物活性研究[D];西北農(nóng)林科技大學(xué);2012年

相關(guān)碩士學(xué)位論文 前5條

1 賀燕華;2-羥基-5-特辛基苯乙酮肟的合成、表征及其萃取性能的研究[D];江西理工大學(xué);2014年

2 宮項(xiàng)飛;肟生物轉(zhuǎn)化合成手性胺的探討和苯乙酮肟在土壤微生物中的代謝行為研究[D];北京化工大學(xué);2007年

3 趙雙會(huì);5-癸基水楊醛肟和2-羥基-5-癸基苯乙酮肟的合成及萃銅條件研究[D];湘潭大學(xué);2010年

4 馮成;萃取劑2-羥基-5-壬基苯乙酮肟的合成研究及其類似物的設(shè)計(jì)與合成[D];河北工業(yè)大學(xué);2007年

5 王景景;苯乙酮衍生物的合成及抗真菌生物活性研究[D];西北農(nóng)林科技大學(xué);2010年

，

本文編號(hào)：1934170