堿性溶液中砷萃取分離研究
本文關(guān)鍵詞:堿性溶液中砷萃取分離研究 出處:《江西理工大學》2015年碩士論文 論文類型:學位論文
【摘要】:就高砷煉銅煙灰資源綜合利用,此前的研究工作提出了堿浸脫砷預處理工藝,該工藝能實現(xiàn)良好的堿浸脫砷效果,并能從堿浸渣中高效回收銅、鉛、鋅等有價金屬。針對堿浸液中砷(III)的分離與富集問題,本文研究采用了CO32-型三辛基甲基氯化銨(Tri-n-octylmethyl-ammonium chloride,TOMAC)有機相萃取硫代亞砷酸的新工藝,可以實現(xiàn)由高砷煙灰堿浸液中直接提取砷。新工藝為高砷煙灰短流程資源化及砷無害化奠定了基礎。本文的研究內(nèi)容如下:基于熱力學計算,研究了水溶液中砷溶解行為。基于此,對砷萃取劑進行了篩選。為提高砷萃取能力,對所選的TOMAC,將Cl-型有機相轉(zhuǎn)型為CO32-型。研究制定了TOMAC有機相轉(zhuǎn)型的較優(yōu)工藝;诩t外光譜,對轉(zhuǎn)型前后TOMAC有機相結(jié)構(gòu)進行分析比較;赥OMAC有機相CO32-轉(zhuǎn)型實驗,通過熱力學計算,分析了AsIII-S-H2O體系中砷賦存的離子形態(tài),探討了其與溶液p H值之間的關(guān)系。結(jié)果發(fā)現(xiàn),在高堿條件下,HAs OS22-可能是As III硫化反應的最主要的產(chǎn)物;趬A浸模擬溶液實驗,測定了CO32-型TOMAC有機相(30%TOMAC+15%仲辛醇+磺化煤油)自含As III 9.69×10-2 mol/L、Na OH 0.5 mol/L的水相料液中萃取硫代亞砷酸的飽和容量。萃取劑與硫代亞砷酸可能按摩爾比2:1締合。基于堿浸模擬溶液實驗,研究確定了CO32-型TOMAC有機相萃取硫代亞砷酸的較優(yōu)工藝條件:有機相組成,30%TOMAC+15%仲辛醇+磺化煤油;水相料液組成,0.5 mol/L Na OH+9.69×10-2 mol/L As III;萃取溫度,室溫;萃取相比,O/A=1/l。在上述條件下,AsIII單級萃取率為85.3%。經(jīng)4級逆流萃取,萃余液中As III濃度可降至1.34×10-3 mol/L以下,萃取率可達98.5%以上,初步達到堿性溶液有效脫砷目的。負載有機相經(jīng)1.0 mol/L Na Cl+2.0 mol/L Na OH混合溶液以相比O/A=1/l反萃,單級反萃率可達89.8%。當反萃相比選擇2/1,經(jīng)6級逆流反萃,理論反萃率可達98%以上。進一步基于紅外光譜,分析比較了有機相經(jīng)“轉(zhuǎn)型-萃取-反萃”后結(jié)構(gòu)變化。
[Abstract]:Comprehensive utilization of high arsenic copper smelting dust resource, research work had made alkaline leaching pretreatment for arsenic removal process, the process can achieve good effect of removing arsenic alkali leaching, and efficient recovery of copper from slag, alkali leaching of lead, zinc and other valuable metals. The alkaline leaching solution of arsenic (III) and enrichment the problem of separation, this paper uses CO32- type three octyl dimethyl ammonium chloride (Tri-n-octylmethyl-ammonium chloride TOMAC) new technology of organic phase extraction thioarsenous acid, can be achieved by the high arsenic ash alkaline leaching solution of direct extraction of arsenic. Laid the foundation for the new technology of high arsenic ash short process resources and harmless. The contents of arsenic this paper is as follows: Based on the thermodynamic calculation of arsenic dissolution behavior in aqueous solution. Based on this, the arsenic extraction agent were screened. In order to improve the extraction ability of arsenic, selected TOMAC, Cl- type organic phase transition to CO32-. To study the development of TOMAC The organic phase transition of the optimal process. Based on the infrared spectra of TOMAC before and after transformation of organic phase structure analysis. TOMAC CO32- organic phase transition experiments based on thermodynamic calculation of the ion forms of arsenic occurrence in AsIII-S-H2O system, and discusses the relationship between P and solution H value. The results showed that in high alkali under the condition of HAs OS22- As III may be the main product of the vulcanization reaction. The alkali leaching solution of simulated experiments based on the determination of CO32- type TOMAC organic phase (30%TOMAC+15% octanol + kerosene) from As containing III 9.69 * 10-2 mol/L, the saturated capacity of aqueous feed solution OH 0.5 Na mol/L extraction thioarsenous acid.. extractant and thioarsenous acid may molar of 2:1 Association. Simulation experiment based on alkali leaching solution, studied CO32- type TOMAC organic phase extraction thioarsenous acid the optimum conditions: organic phase composition, 30% TOMAC+15% 1-METHYLHEPTYL Alcohol + kerosene; aqueous feed solution composed of 0.5 mol/L Na OH+9.69 * 10-2 mol/L As III; extraction temperature, extraction at room temperature; compared to O/A=1/l. under the above conditions, AsIII single stage extraction rate of 85.3%. by the 4 stage countercurrent extraction raffinate As III concentration can be reduced to 1.34 * 10-3 mol/L, extraction the rate is over 98.5%, achieved the effective removal of arsenic alkaline solution. The loaded organic phase by 1 mol/L Na Cl+2.0 mol/L Na OH O/A=1/l mixed solution compared to single-stage stripping, stripping rate 89.8%. when stripping compared to 2/1, the 6 stage countercurrent stripping, the theory of the stripping rate can reach more than 98%. Further based on the infrared spectroscopy, analysis and comparison of the organic phase change structure transformation and counter extraction ".
【學位授予單位】:江西理工大學
【學位級別】:碩士
【學位授予年份】:2015
【分類號】:X758
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