氟硅酸處理含鉀頁巖中硅鋁鐵的高效分離技術(shù)研究
發(fā)布時(shí)間:2018-05-03 07:49
本文選題:含鉀頁巖 + 鐵鋁分離; 參考:《貴州大學(xué)》2015年碩士論文
【摘要】:含鉀頁巖是一種難溶性的含鉀礦物,富含K2O在9%左右,儲(chǔ)量豐富,品質(zhì)優(yōu)良,且分布廣泛,我國從20世紀(jì)50年代,就開始研究和開發(fā)利用不溶性鉀礦制備鉀肥。貴州省就有近百個(gè)含鉀巖石的礦點(diǎn),礦產(chǎn)儲(chǔ)存量很大,僅銅仁礦帶的儲(chǔ)量就超過50億噸。本文所述含鉀頁巖是以貴州銅仁市萬山特區(qū)的鉀頁巖為研究對象,采用化學(xué)分析和XRD分析,得到其主要化學(xué)成分為K2O、SiO2、Al2O3,三者含量之和大于85%。本文主要研究的是氟硅酸分解含鉀頁巖后的固體(以下稱為固體溶樣),探討了其中硅鋁鐵的提取和分離方法。本實(shí)驗(yàn)選用濃硫酸將固體溶樣中的氟和硅揮發(fā)掉,將鐵鋁轉(zhuǎn)變?yōu)榭扇苄缘柠}。原礦粉質(zhì)量(g):硫酸用量(ml)為1:0.6時(shí),中間體鋁的提取率可達(dá)95.3%,鐵的提取率可達(dá)到86.8%。當(dāng)溶解用水的體積(ml)和洗水的體積(ml)分別為礦粉質(zhì)量(g)的4倍和1倍時(shí),能夠?qū)⒖扇苄缘牧蛩徼F和硫酸鋁完全溶解。本實(shí)驗(yàn)采用三級有機(jī)絡(luò)合沉淀分離鐵鋁,單因素實(shí)驗(yàn)確定最佳工藝條件為:一級分離過程:鐵與DDTC的質(zhì)量比為1:8,溶液pH為1.8,反應(yīng)溫度35℃,反應(yīng)時(shí)間為10min,溶液中鐵的分離率為74.6%。二、三級分離過程:鐵與DDTC的質(zhì)量比為1:10,溶液pH為1.8,反應(yīng)溫度25℃,反應(yīng)時(shí)間為5min,溶液中鐵的分離率為99%。經(jīng)過三級分離溶液中鐵的分離率可以達(dá)到99%。鐵的絡(luò)合物可以與堿反應(yīng)制備氫氧化鐵,經(jīng)過煅燒后得到氧化鐵。通過單因素實(shí)驗(yàn)確定最佳工藝條件為:Fe-DDTC與KOH的固液比為1:50,反應(yīng)溫度60℃,反應(yīng)時(shí)間2h,聚乙二醇加入量為3ml時(shí),制備的氧化鐵的純度為91.2%。氧化鋁制備過程,通過單因素實(shí)驗(yàn)確定的最佳反應(yīng)工藝條件是,反應(yīng)溫度60℃,反應(yīng)時(shí)間0.5h,反應(yīng)體系的pH為8,氨水的質(zhì)量分?jǐn)?shù)為15%時(shí),制備的氧化鋁的純度為92.3%。
[Abstract]:Potash shale is an insoluble mineral containing potassium, rich in about 9% of K 2O, rich in reserves, excellent quality and widely distributed. In China, insoluble potassium ore has been studied and utilized to produce potassium fertilizer since 1950s. Guizhou province has nearly 100 K-bearing rock ore sites, the mineral reserves are very large, Tongren ore belt alone reserves more than 5 billion tons. In this paper, the potassium shale in Wanshan Special Zone of Tongren City, Guizhou Province is taken as the research object. By chemical analysis and XRD analysis, the main chemical composition of the shale is K _ 2O _ 2O _ 2 Sio _ 2 and Al _ 2O _ 3, and the sum of the three contents is more than 85%. In this paper, the method of extraction and separation of silicon-aluminum-ferric acid from the solid after the decomposition of potassium shale by fluorosilicic acid (hereinafter referred to as solid dissolved sample) is studied. In this experiment, concentrated sulfuric acid was used to volatilize the fluorine and silicon in the solid sample, and to transform iron and aluminum into soluble salt. When the mass of raw ore powder is 1: 0.6, the extraction rate of aluminum and iron can reach 95.3and 86.8 respectively. When the volume of dissolved water (ml) and the volume of washing water (ml) are 4 times and 1 times of the mass of mineral powder, the soluble ferric sulfate and aluminum sulfate can be dissolved completely. In this experiment, the three-stage organic complexation precipitation was used to separate iron and aluminum. The optimum technological conditions were determined as follows: the mass ratio of iron to DDTC was 1: 8, the pH of solution was 1.8, the reaction temperature was 35 鈩,
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