电炉钛渣磷酸化焙烧-浸出脱除镁、钙杂质（英文）
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摘要
提出一种利用磷酸化焙烧-盐酸浸出从电炉钛渣(含3.12%MgO和0.86%CaO)中有效脱除镁、钙杂质的方法。利用XRF、XRD和SEM对钛渣样品的化学成分、物相成分和显微组织进行表征。研究钛渣的磷酸氧化焙烧热力学、氧化焙烧过程中钛渣物相的转变、显微组织和元素分布的变化以及浸出除杂过程。热力学分析结果表明,焙烧过程中加入磷酸能有效促进MgTi_2O_5和CaSiO_3的分解。研究结果表明,在焙烧过程中磷酸能有效促进渣中含钛矿物转变为金红石,并促使M_xTi_(3-x)O_5中杂质元素富集在磷酸盐中,进而通过酸浸除去。在所研究的实验条件下,钛渣中镁和钙的脱除率可分别达到94.68%和87.19%。最终酸浸渣中MgO和CaO含量可分别降低至0.19%和0.13%(质量分数)。
H_3PO_4 oxidation roasting followed by HCl acid leaching was proposed to remove magnesium and calcium from electric furnace titanium slag containing 3.12% MgO and 0.86% CaO. XRF, XRD and SEM techniques were used to characterize the composition, mineral phase component and microstructure of the titanium slag. The H_3PO_4 oxidation thermodynamic, mineral phase transformation, microstructure, element distribution in titanium slag during H_3PO_4 oxidation process and leaching process were investigated. The thermodynamic analysis indicated that H_3PO_4 could promote the decomposition of MgTi_2O_5 and CaSiO_3. The results indicated that H_3PO_4 could effectively promote the transformation of titanium-bearing mineral to rutile and enrich the impurities in M_xTi_(3-x)O_5 into phosphate which could be removed by acid leaching process. Under the studied conditions, the leaching rates of magnesium and calcium reached 94.68% and 87.19%, respectively. The acid leached slag containing 0.19% MgO and 0.13% CaO(mass fraction) was obtained.
H_3PO_4 oxidation roasting followed by HCl acid leaching was proposed to remove magnesium and calcium from electric furnace titanium slag containing 3.12% MgO and 0.86% CaO. XRF, XRD and SEM techniques were used to characterize the composition, mineral phase component and microstructure of the titanium slag. The H_3PO_4 oxidation thermodynamic, mineral phase transformation, microstructure, element distribution in titanium slag during H_3PO_4 oxidation process and leaching process were investigated. The thermodynamic analysis indicated that H_3PO_4 could promote the decomposition of MgTi_2O_5 and CaSiO_3. The results indicated that H_3PO_4 could effectively promote the transformation of titanium-bearing mineral to rutile and enrich the impurities in M_xTi_(3-x)O_5 into phosphate which could be removed by acid leaching process. Under the studied conditions, the leaching rates of magnesium and calcium reached 94.68% and 87.19%, respectively. The acid leached slag containing 0.19% MgO and 0.13% CaO(mass fraction) was obtained.
引文
[1]QIAO Li-ying,XIE Feng-yu,XIE Ming-hui,GONG Cai-hua,WANG Wei-lang,GAO Jia-cheng.Characterization and photoelectrochemical performance of Zn-doped Ti O2 films by sol–gel method[J].Transactions of Nonferrous Metals Society of China,2016,26(8):2109-2116.
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[14]SUI Li-li,ZHAI Yu-chun.Reaction kinetics of roasting high-titanium slag with concentrated sulfuric acid[J].Transactions of Nonferrous Metals Society of China,2014,24(3):848-853.
[15]CHEN Guo,CHEN Jin,PENG Jin-hui,WAN Run-dong.Green evaluation of microwave-assisted leaching process of high titanium slag on life cycle assessment[J].Transactions of Nonferrous Metals Society of China,2010,20(S1):s198-s204.
[16]GUéGUIN M,CARDARELLI F.Chemistry and mineralogy of titania-rich slags.Part 1:Hemo-ilmenite,sulphate,and upgraded titania slags[J].Mineral Processing and Extractive Metallurgy Review,2007,28(1):1-58.
[17]LEDDY J J,SCHECHTER D L.Pressure leaching of titaniferous material:US patent,3060002A[P].1962-05-20.
[18]ELGER G W,HOLMES R A.Purifying titanium-bearing slag by promoted sulfation:US patent,4362557[P].1982-12-07.
[19]WANG Dong,CHU Jing-long,LI Jie,QI Tao,WANG Wei-jing.Anti-caking in the production of titanium dioxide using low-grade titanium slag via the Na OH molten salt method[J].Powder Technology,2012,232:99-105.
[20]LASHEEN T A.Soda ash roasting of titania slag product from Rosetta ilmenite[J].Hydrometallurgy,2008,93(3-4):124-128.
[21]DONG Hai-gang,JIANG Tao,GUO Yu-feng,CHEN Jia-lin,FAN Xing-xiang.Upgrading a Ti-slag by a roast-leach process[J].Hydrometallurgy,2012,113-114:119-121.
[22]SUI Li-li,ZHAI Yu-chun.Extraction of Ti O2 from high titanium slag through roasting by ammonium bisulfate[J].The Chinese Journal of Nonferrous Metals,2014,24(3):826-830.(in Chinese)
[23]ZHANG Jian-bo,LIAO Jun-hui,CHENG Xiao-zhe,YE Si-dong.Contrastive study on processes of redox modification-acid leaching of Panzhihua Ti-slag and ilmenite[J].Chinese Journal of Rare Metals,2016,40(4):385-392.(in Chinese)
[24]DEMIRBAS A,ABALI Y,MERT E.Recovery of phosphate from calcinated bone by dissolution in hydrochloric acid solutions[J].Resour Conserv Recy,1999,26(3-4):251-258.
[2]DANISH R,AHMED F,ARSHI N,ANWAR M S,KOO B H.Facile synthesis of single-crystalline rutile Ti O2 nano-rods by solution method[J].Transactions of Nonferrous Metals Society of China,2014,24(S1):s152-s156.
[3]PAN Yin-cheng,ZOU Jian-xin,ZENG Xiao-qin,DING Wen-jiang.Hydrogen storage properties of Mg–Ti O2 composite powder prepared by arc plasma method[J].Transactions of Nonferrous Metals Society of China,2014,24(12):3834-3839.
[4]CROCE P S,MOUSAVI A.A sustainable sulfate process to produce Ti O2 pigments[J].Environmental Chemistry Letters,2013,11(4):325-328.
[5]NAYL A A,ISMAIL I M,ALY H F.Ammonium hydroxide decomposition of ilmenite slag[J].Hydrometallurgy,2009,98(1-2):196-200.
[6]XU Cong,YUAN Zhang-fu,WANG Xiao-qiang.Preparation of Ti Cl4 with the titanium slag containing magnesia and calcia in a combined fluidized bed[J].Chinese J Chem Eng,2006,14(3):281-288.
[7]SAHU K K,ALEX T C,MISHRA D,AGRAWAL A.An overview on the production of pigment grade titania from titania-rich slag[J].Waste Management&Research,2006,24(1):74-79.
[8]BALDERSON G F,MACDONALD C A.Method for the production of synthetic rutile:US patent,5885324[P].1999-03-23.
[9]EL-HAZEK N,LASHEEN T A,EL-SHEIKH R,ZAKI S A.Hydrometallurgical criteria for Ti O2 leaching from Rosetta ilmenite by hydrochloric acid[J].Hydrometallurgy,2007,87(1-2):45-50.
[10]WU Ling,LI Xin-hai,WANG Zhi-xing,WANG Xiao-juan,LI Ling-jun,FANG Jie,WU Fei-xiang,GUO Hua-jun.Preparation of synthetic rutile and metal-doped Li Fe PO4 from ilmenite[J].Powder Technology,2010,199(3):293-297.
[11]LI Zeng-he,WANG Zhen-cui,LI Ge.Preparation of nano-titanium dioxide from ilmenite using sulfuric acid-decomposition by liquid phase method[J].Powder Technology,2016,287:256-263.
[12]ZHENG Fu-qiang,CHEN Feng,GUO Yu-feng,JIANG Tao,YAKOVLEVICH T A,QIU Guan-zhou.Kinetics of hydrochloric acid leaching of titanium from titanium-bearing electric furnace slag[J].JOM,2016,68(5):1476-1484.
[13]ZHANG Li,LI Guang-qiang,ZHANG Wu.Synthesis of rutile from high titania slag by pyrometallurgical route[J].Transactions of Nonferrous Metals Society of China,2011,21(10):2317-2322.
[14]SUI Li-li,ZHAI Yu-chun.Reaction kinetics of roasting high-titanium slag with concentrated sulfuric acid[J].Transactions of Nonferrous Metals Society of China,2014,24(3):848-853.
[15]CHEN Guo,CHEN Jin,PENG Jin-hui,WAN Run-dong.Green evaluation of microwave-assisted leaching process of high titanium slag on life cycle assessment[J].Transactions of Nonferrous Metals Society of China,2010,20(S1):s198-s204.
[16]GUéGUIN M,CARDARELLI F.Chemistry and mineralogy of titania-rich slags.Part 1:Hemo-ilmenite,sulphate,and upgraded titania slags[J].Mineral Processing and Extractive Metallurgy Review,2007,28(1):1-58.
[17]LEDDY J J,SCHECHTER D L.Pressure leaching of titaniferous material:US patent,3060002A[P].1962-05-20.
[18]ELGER G W,HOLMES R A.Purifying titanium-bearing slag by promoted sulfation:US patent,4362557[P].1982-12-07.
[19]WANG Dong,CHU Jing-long,LI Jie,QI Tao,WANG Wei-jing.Anti-caking in the production of titanium dioxide using low-grade titanium slag via the Na OH molten salt method[J].Powder Technology,2012,232:99-105.
[20]LASHEEN T A.Soda ash roasting of titania slag product from Rosetta ilmenite[J].Hydrometallurgy,2008,93(3-4):124-128.
[21]DONG Hai-gang,JIANG Tao,GUO Yu-feng,CHEN Jia-lin,FAN Xing-xiang.Upgrading a Ti-slag by a roast-leach process[J].Hydrometallurgy,2012,113-114:119-121.
[22]SUI Li-li,ZHAI Yu-chun.Extraction of Ti O2 from high titanium slag through roasting by ammonium bisulfate[J].The Chinese Journal of Nonferrous Metals,2014,24(3):826-830.(in Chinese)
[23]ZHANG Jian-bo,LIAO Jun-hui,CHENG Xiao-zhe,YE Si-dong.Contrastive study on processes of redox modification-acid leaching of Panzhihua Ti-slag and ilmenite[J].Chinese Journal of Rare Metals,2016,40(4):385-392.(in Chinese)
[24]DEMIRBAS A,ABALI Y,MERT E.Recovery of phosphate from calcinated bone by dissolution in hydrochloric acid solutions[J].Resour Conserv Recy,1999,26(3-4):251-258.
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