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再次,我還要感謝魏小磊同學(xué),在試驗(yàn)中得到他的協(xié)助和支持,有時(shí)我們共同探討,在此過(guò)程中,讓我學(xué)到了許多知識(shí),在此表示感謝!另外,感謝本論文所引用的所有參考文獻(xiàn)的作者,感謝他們?yōu)楸菊撐牡膶懽魈峁┱鎸?shí)可靠的科學(xué)知識(shí)。其次,我要感謝張邦文教授、李解老師、趙瑞超老師,他們?cè)谖业膶?shí)驗(yàn)過(guò)程中也給予我很大的幫助和鼓勵(lì)。試驗(yàn)后他又耐心的指導(dǎo)我書寫論文。試驗(yàn)前,我在他的指導(dǎo)下搜集了很多和本論文有關(guān)的專業(yè)方面的資料。本論文所研究的內(nèi)容和書寫是在許多老師以及同學(xué)們的幫助下才得以順利進(jìn)行的,在此,我要衷心的感謝他們!首先,我要感謝我的指導(dǎo)老師布林朝克老師。因此,用合成的TQ從埃及礦的硫酸鹽浸出液中提取分離鈮時(shí)可行的。%。實(shí)驗(yàn)室提取試驗(yàn)結(jié)果表明:%,鈮的提取達(dá)到84%。當(dāng)4%%的鐵被提取時(shí),%的鉭也被提取。 TQ對(duì)干涉元素的萃取從硫酸鹽溶液中TQ提取的主要元素為鈰和銥,提取率分別為63%%。所得濾渣洗滌過(guò)濾,然后加熱到900℃干燥。表4的結(jié)果表明。%TQ以體積比3/1,%。 TQ的載荷能力TQ的載荷能力決定于所接觸的目的溶液。當(dāng)TQ濃度再增加時(shí)浸出率沒(méi)有明顯的變化。 TQ濃度的影響研究這個(gè)因素,別的條件如A/O定為1/1,接觸時(shí)間15分鐘,%%變化。 A/O的影響,在不同油水度(從1/4—3/1)下振蕩15分鐘。有可能存在下列反應(yīng)關(guān)系式:Nb2O5+6H2SO4+5/2O2——2NbO2(SO4)3+6H2O (2) 接觸時(shí)間的影響,從一分鐘到三十分鐘。值得提的是高度解離的礦對(duì)試驗(yàn)時(shí)有好處的。 硫酸濃度的影響、%提取劑TQ后振蕩15分鐘,隨著硫酸濃度的減小,%%。本次試驗(yàn)將檢驗(yàn)1,3環(huán)己酮對(duì)提鈮的效果,其浸出率不超過(guò)5%。然后用紫外—可見(jiàn)雙射束檢測(cè)分析。最后得到的產(chǎn)物用SEM分析其中的化學(xué)組成和純度。由蒸餾水、進(jìn)行萃取鈮試驗(yàn)。 鈮的回收率,所得懸浮液在150℃下攪拌兩個(gè)小時(shí),不溶殘?jiān)^(guò)濾,所得濾液的化學(xué)成分在表2中給出。用電子顯微鏡進(jìn)行礦樣元素分析。 礦石性質(zhì)本實(shí)驗(yàn)所用礦樣為埃及東部Kadabora礦山得來(lái),此礦山的礦為典型的復(fù)雜氧化礦。接下來(lái),在酒精中有氨基三唑的情況下反應(yīng)六小時(shí),隨后加入結(jié)晶態(tài)的pipredine。1,3雜環(huán)二酮的懸浮液在有DMF、DMA的情況下加熱三小時(shí)。為了這個(gè)目的,本實(shí)驗(yàn)就是利用咪唑啉酮化合物從埃及礦硫酸浸出液中提取鈮。唑類化合物作為重要的環(huán)狀系因?yàn)樗麄兊纳镄阅艿亩鄻佣艿街匾?。這些對(duì)提鈮效果顯著地藥劑可以分為兩大類:一類是中性氧化萃取劑,如酮類、TBP、TOPO和亞砜;另一類為含長(zhǎng)鏈脂肪族或芳香族的胺類化合物,如TOA、TBA等。鈮一般來(lái)源于自然鈮礦物、進(jìn)口或者錫渣。鈮應(yīng)用于很多的工業(yè)行業(yè),而且需求很高并且還在增長(zhǎng)。 and it was mainly contaminated with sulfur, calcium and yttrium ().Table 4 Stripping of niobium from loaded extractant % TQ at O/A ratio of 1/1 for 15 minStripping agentH2O mol/L HF mol/L HFStripping efficiency/% Elemental position of precipitate formed from stripsolution as analyzed by scanning electron microscope Interfering elements extracted by TQThe major elements extracted by TQ from the sulfate leach liquor were cerium and yttrium with efficiency of 63% and %, respectively. Both elements were stripped with 20% sodium hydroxide. The extraction process was also interfered by % calcium, which was detected in the final product. Only % tantalum was transferred to the extractant while 4% uranium and % iron were extracted but none of the mentioned elements were stripped with mol/L HF.4 ConclusionsThis study demonstrated the potentiality of TQ in the extraction of niobium from sulfate leach liquor of Egyptian ore sample. The results of the bench scale extraction experiments showed that 84% of niobium was extracted by shaking equal volumes of % TQ in methylene chloride with leach liquor of [NbO2(SO4)3]3 in the organic phase. The mol/L HF was used to strip % niobium, which was precipitated by ammonium hydroxide with efficiency of %. The purity of the final product reached %.Thus, it is possible to utilize the synthesized TQ as an extractant in hydrometallurgical processes for separating niobium from sulfate liquor of Egyptian ore sample.用咪唑啉酮化合物從埃及礦硫酸浸出液中提取鈮1 緒論自然界中,鈮和鉭總是以復(fù)雜的氧化物共存,脈石礦物主要為結(jié)晶花崗巖。L1)Da Effect of TQ concentrationTo study this factor, the TQ concentration in methylene chloride was varied from % up to % while the other extraction conditions were fixed at an A/O ratio of 1/1, contact time 15 min and using the leach liquor of mol/L sulfuric acid. The extraction efficiency increased from % till it reached 84% at the extractant concentration of % and no further extraction occurred by using an excess TQ (%). The logarithmic plot of niobium distribution ratio versus TQ concentration given in yielded a molar ratio of 3/1. Logarithmic plot of Nb distribution ratio lg D vs lg[TQ] Loading capacity of TQThe loading capacity of TQ was determined by contacting the feed solution and % TQ in methylene chloride at an A/O ratio of 1/1 for 15 min. Regarding the molar ratio, the maximum loading capacity was found to be g/L. It is worth to mention that contacting three volumes of the feed solution with one volume of % TQ yielded g/L (Table 3), which is % of the maximum loading capacity. Stripping and precipitation experimentsThe loaded organic phase assaying g/L niobium was shaken with the same volume of the following stripping agents: distilled water, mol/L HF and mol/L HF. The results given in Table 4 showed that mol/L HF stripped % of the loaded niobium. Two volumes of ammonia solution (33%) were mixed with one volume of mol/L HF strip solution to yield % precipitation efficiency. The solid product was filtered and thoroughly washed。L1)Recovery/%69,83 Results and discussion Extraction experimentsCyclohexone was previously used for extracting 70% niobium from sulfate leach liquor in presence of ammonium nitrate. In the present study, 1,3 cyclohexane dione was examined for extracting niobium. Its extraction efficiency did not exceed 5% by shaking equal volumes of the organic phase and sulfate leach liquor ( mol/L H2SO4) containing g/L Nb for 15 min. Thisβdiketone was used as start for synthesizing TQ. The latter was prepared as % in methylene chloride and was used to study the influence of different extraction conditions in improving niobium extraction efficiency from the sulfate leach liquor. Effect of sulfuric acid concentrationFour leach liquors were prepared by digesting the ground ore sample with sulfuric acid of , , and mol/L. Equal volumes of these solutions were shaken for 15 min with the extractant % TQ. The extraction efficiency of niobium increased from % to % by decreasing the acid concentration, which may be due to the ability of TQ to extract sulfuric acid. The maximum distribution coefficient was at shows the plot of lg D versus lg [H2SO4],which is found to be linear with slope of about . It is probable that the following reaction may occur:Nb2O5+6H2SO4+5/2O2——2NbO2(SO4)3+6H2O (2) Logarithmic plot of Nb distribution ratio lg D vslg[H2SO4] Effect of contact timeThe aqueous leach liquor of mol/L sulfuric acid and the extractant % TQ were shaken at A/O