草酸酸浸处理钛石膏实验研究
收稿日期: 2023-06-30
网络出版日期: 2024-05-15
基金资助
河南省重大公益专项(201300311000);河南省科技攻关项目(232102320335)
Study on leaching treatment of titanium gypsum with oxalic acid
Received date: 2023-06-30
Online published: 2024-05-15
硫酸法酸浸钛石膏虽能有效浸出铁杂质但易引起石膏相变，对环境影响较大，工艺危险性高。基于此，采用草酸代替硫酸酸浸钛石膏浸出铁杂质，探究了酸浸温度、酸浸时间、草酸质量分数、液固质量比等因素对浸出铁效果的影响。结果表明：在草酸酸浸过程中以扩散过程为主，温度和时间是主要影响因素；在酸浸时间为110 min、酸浸温度为90 ℃、草酸质量分数为6%、液固质量比为8条件下，草酸浸出铁率可达84%；结合FT-IR、XRD、SEM表征结果发现，钛石膏中铁杂质以絮凝状吸附在石膏晶体表面，适量草酸能有效去除钛石膏中铁杂质，过量草酸则会造成石膏部分溶解并在晶体表面生成草酸钙影响晶体形貌。采用草酸酸浸处理钛石膏可以有效去除钛石膏中的铁杂质，是一种环保、有效的除铁工艺，该实验结果可为钛石膏除铁研究提供参考。
王露威 , 王杰 , 李珂珂 , 冯春花 , 张文艳 , 朱建平 . 草酸酸浸处理钛石膏实验研究[J]. 无机盐工业, 2024 , 56(5) : 108 -114 . DOI: 10.19964/j.issn.1006-4990.2023-0345
Although the acid leaching of titanium gypsum with sulfuric acid can effectively leach iron impurities，it is easy to cause the phase transformation of gypsum，which has great influence on the environment and high process risk.Based on this，oxalic acid was used instead of sulfuric acid to leach titanium gypsum for iron impurities.The influences of leaching temperature，leaching time，mass fraction of oxalic acid and ratio of liquid to solid on the leaching effect of iron were investigated.The results showed that the diffusion process was the main process in oxalic acid leaching，and temperature and time were the main influencing factors.Under the conditions of leaching time of 110 min，leaching temperature of 90 ℃，mass fraction of oxalic acid of 6% and liquid-solid mass ratio of 8，the leaching rate of iron by oxalic acid reached 84%.Combined with FT-IR，XRD and SEM characterization results，it was found that the iron impurities in the titanium gypsum were adsorbed on the surface of the gypsum crystal in a flocculating manner.Appropriate amount of oxalic acid could effectively remove iron impurities in titanium gypsum，and excessive oxalic acid would cause partial dissolution of gypsum and the formation of calcium oxalate on the crystal surface，which affected the crystal morphology.Oxalic acid leaching treatment of titanium gypsum could effectively remove iron impurities in titanium gypsum，which was an environmentally friendly and effective iron removal process.The experimental results could provide reference for the study of iron removal of titanium gypsum.
Key words： titanium gypsum; oxalic acid; iron impurities; calcium oxalate
| 1 | 龚家竹.钛石膏与磷石膏固废耦合资源化利用技术进展［J］.无机盐工业，2019，51（1）：1-6，11. |
| GONG Jiazhu.Progress in coupling utilization technology of titanium gypsum and phosphogypsum solid waste［J］.Inorganic Che-Industry micals，2019，51（1）：1-6，11. | |
| 2 | YANG Yuhong， KOU Lidong， CHEN Huan，et al.Synthesis of magnetic adsorbents from titanium gypsum and biomass wastes for enhanced phosphate removal［J］.Bioresource Technology，2023，371：128609. |
| 3 | 杜传伟，李国忠，陈娟.利用天然石膏形态组成模拟钛石膏及其性能研究［J］.建筑材料学报，2014，17（3）：511-516. |
| DU Chuanwei， LI Guozhong， CHEN Juan.Simulation of titanium gypsum with morphology and composition of natural gypsum and its property［J］.Journal of Building Materials，2014，17（3）：511-516. | |
| 4 | PENG Xiaoqian， ZHENG Jiayi， LIU Qian，et al.Efficient removal of iron from red gypsum via synergistic regulation of gypsum phase transformation and iron speciation［J］.The Science of the Total Environment，2021，791：148319. |
| 5 | 顾汉念，郭腾飞，马时成，等.赤泥中铁的提取与回收利用研究进展［J］.化工进展，2018，37（9）：3599-3608. |
| GU Hannian， GUO Tengfei， MA Shicheng，et al.Review on separation，recovery，extraction and comprehensive utilization of iron from red mud［J］.Chemical Industry and Engineering Progress，2018，37（9）：3599-3608. | |
| 6 | LI Xiong， ZHU Rong， HU Shuxuan，et al.Leaching of arsenic from flue gas desulphurisation gypsum using ultrasound-enhanced sulfuric acid［J］.Journal of Cleaner Production，2022，381：135163. |
| 7 | 王倩，彭同江，孙红娟，等.钛石膏-H2SO4-H2O体系中石膏-硬石膏的相变规律［J］.硅酸盐通报，2022，41（2）：725-732. |
| WANG Qian， PENG Tongjiang， SUN Hongjuan，et al.Phase transformation law of gypsum-anhydrite in titanium gypsum-H2SO4-H2O system［J］.Bulletin of the Chinese Ceramic Society，2022，41（2）：725-732. | |
| 8 | 赵雪淞，刘鑫，李彩霞，等.混酸提纯制备高纯石英砂及浸出动力学分析［J］.硅酸盐学报，2021，49（3）：581-589. |
| ZHAO Xuesong， LIU Xin， LI Caixia，et al.Preparation of high-purity quartz sand by leaching with mixed acids［J］.Journal of the Chinese Ceramic Society，2021，49（3）：581-589. | |
| 9 | SULTANA U K， KURNY A S W.Dissolution kinetics of iron oxides in clay in oxalic acid solutions［J］.International Journal of Minerals，Metallurgy，and Materials，2012，19（12）：1083-1087. |
| 10 | 陈书锐，杨绍利，马兰，等.盐酸浸出钛石膏实验研究［J］.无机盐工业，2020，52（2）：65-68. |
| CHEN Shurui， YANG Shaoli， MA Lan，et al.Study on leaching of titanium gypsum with hydrochloric acid［J］.Inorganic Chemicals Industry，2020，52（2）：65-68. | |
| 11 | YU Zhanglong， SHI Zhixia， CHEN Yongmei，et al.Red-mud treatment using oxalic acid by UV irradiation assistance［J］.Transactions of Nonferrous Metals Society of China，2012，22（2）：456- 460. |
| 12 | 石志霞，余章龙，彭程，等.低品位铝土矿草酸光催化除铁研究［J］.材料导报，2015，29（S2）：125-128. |
| SHI Zhixia， YU Zhanglong， PENG Cheng，et al.Sunlight irradiation-assisted removal of iron oxide from low grade bauxite using oxalic acid［J］.Materials Reports，2015，29（S2）：125-128. | |
| 13 | 党晓娥，张婷.Fe3+-C2O4 2--H2O溶液中Fe（Ⅲ）的形态分布及其在硫酸烧渣和氰化尾渣除铁过程中的应用［J］.化工进展，2023（11）：6005-6014. |
| DANG Xiao′e， ZHANG Ting.Species distribution of Fe（Ⅲ）in Fe3+-C2O4 2--H2O solution and application in the process of iron removal from sulphuric acid cinder and syanide tailings［J］.Chemical Industry and Engineering Progress，2023（11）：6005-6014. | |
| 14 | 彭家惠，张建新，瞿金东，等.有机酸对α半水脱硫石膏晶体生长习性的影响与调晶机理［J］.硅酸盐学报，2011，39（10）：1711-1718. |
| PENG Jiahui， ZHANG Jianxin， QU Jindong，et al.Effect of organic acid on crystalline habit of α-hemihydrate desulfurization gypsum and its crystal modification mechanism［J］.Journal of the Chinese Ceramic Society，2011，39（10）：1711-1718. | |
| 15 | 陈岚，满瑞林，李志明.草酸钙结石形态的红外光谱分析［J］.分析测试学报，2007，26（4）：582-584. |
| CHEN Lan， MAN Ruilin， LI Zhiming.Analysis of calcium oxalate crystalline phases by infrared spectrophotometry［J］.Journal of Instrumental Analysis，2007，26（4）：582-584. | |
| 16 | 闫蔚，曾柏淋，孟江，等.石膏红外图谱鉴定研究［J］.光谱学与光谱分析，2016，36（7）：2098-2103. |
| YAN Wei， ZENG Bolin， MENG Jiang，et al.Study on the identification of gypsum fibrosum with FTIR［J］.Spectroscopy and Spectral Analysis，2016，36（7）：2098-2103. | |
| 17 | ZHANG Wenyan， ZHAO Liya， XUE Mengfen，et al.Effect of oxalic acid pretreatment on the mechanical properties and microstructure of phosphogypsum［J］.Construction and Building Materials，2023，362：129631. |
/
| 〈 |
|
〉 |
