Extraction of vanadium and preparation of aluminum phosphate from phosphorus-silicate slag produced in phosphorus chemical industry

doi:10.16085/j.issn.1000-6613.2018-0292

Abstract

Abstract: The phosphorus-silicon slag as solid-waste is derived from dephosphorization by calcification and desiliconization by aluminum salt during the extraction of V from the phosphorus-rich raw material containing V. With the high content of heavy metal in the slag, it would become a potential threat to the environment and result in waste of resources without a reasonable processing route. However, researches related with the slag were rarely reported. In this article, the main mineral components and their contents in the phosphorus-silicon slag were analyzed and a route of disposing the slag was developed that P and Al contained in the slag was used to produce aluminum phosphate. The impact of reaction time, reaction temperature and pH on the processes of the neutralization and desulfurization and the preparation of aluminum phosphate was investigated. The investigation indicated that during the process of the neutralization and desulfurization, the loss of P, V and Al could be eliminated at pH=0.5, room temperature. During separating vanadium from aluminum and phosphorus, choosing pH=8.0 can eliminate the adsorption of vanadium on aluminum phosphate, and separation efficiency is improved. During purification of aluminum phosphate, the optimal condition was that pH, reaction temperature and reaction time were 12.0, 80℃ and 2h, respectively. The production of qualified aluminum phosphate was under the conditions of pH=8.0. The filter performance of the slurry was 30 times of that is not disposed, after the slurry of aluminum phosphate was disposed at 130℃.

Key words: phosphorus-silicon slag, extraction of vanadium, aluminum phosphate, adsorption

摘要： 磷硅渣作为高磷含钒原料提钒过程中钙化脱磷和铝盐脱硅的固体废弃物，其中含有较多的重金属，如不进行合理处置，不仅造成资源浪费，也会对环境产生较大的威胁，而目前有关该种渣的研究鲜有报道。本文采用多种检测技术分析了磷硅渣中主要成分含量，并开发了一种合理化利用途径——以磷硅渣为原料制备磷酸铝。考察了pH、温度和时间等条件对氧化钙中和脱硫和磷酸铝制备过程的影响。氧化钙中和脱硫过程中，控制终点pH=0.5可以有效消除有价元素P、Al、V的损失，且常温即能达到反应要求；P、Al、V分离过程中，控制终点pH=8.0可以有效消除磷酸铝对V的吸附作用，提高分离效率；净化除杂过程的最优条件为：反应终点pH=12，反应时间2h，反应温度80℃；磷酸铝产品制备过程中，控制终点pH=8.0，磷铝比为最佳，130℃高温转型处理能够使磷酸铝浆料的过滤性能提升30倍。

关键词: 磷硅渣, 提钒, 磷酸铝, 吸附

CLC Number:

X753

LIU Jiuchuan, WU Hepei, ZHANG Jianxia, FAN Bingqiang, ZHENG Shili, ZHANG Yang. Extraction of vanadium and preparation of aluminum phosphate from phosphorus-silicate slag produced in phosphorus chemical industry[J]. Chemical Industry and Engineering Progress, 2018, 37(10): 4080-4087.

刘久传, 吴和培, 张建霞, 范兵强, 郑诗礼, 张洋. 磷硅渣提钒及制备磷酸铝工艺[J]. 化工进展, 2018, 37(10): 4080-4087.

References

[1] 陈文祥. 含钒炭质页岩提钒废渣资源化利用研究进展[J].湿法冶金, 2011, 30(4):268-271. CHEN Wenxiang. Advances in research and utilization of vanadium-rich carbonaceous shale waste recovery resources[J]. Journal of Hydrometallurgy, 2011, 30(4):268-271.
[2] HILLS C D, KOE L, SOLLARS C J, et al. Early heat of hydration during the solidification of a metal plating sludge[J]. Cement & Concrete Research, 1992, 22(5):822.
[3] 涂洁, 侯浩波. HAS土壤固化剂对电镀污泥处理效果的研究[J]. 环境工程, 2003, 21(4):44-47. TU J. Studies on the effect of electroplating sludge stabilized by HAS solil-hardening agent[J]. Environmental Engineering, 2003, 21(4):44-47.
[4] BEWTRA J K, BISWAS N, HENDERSON W D, et al. Recent advances in treatment of selected hazardous wastes[J]. Water Quality Research Journal of Canada, 1995, 30(1):115-125.
[5] 吴乾箐, 宋颖, 李昕, 等. 电镀超高浓度铬废水微生物治理工程的研究[J]. 水处理技术, 1996, 34(7):165-167. WU Qianjing, SONG Ying, LI Xin, et al. Study on microorganism treatment project of electroplating ultra-high concentration chromium wastewater[J]. Technology of Water Treatment, 1996, 34(7):165-167.
[6] 祝万鹏, 叶波清. 溶剂萃取法提取电镀污泥氨浸出渣中的金属资源[J]. 环境科学, 1998, 11(3):35-38. ZHU Wanpeng, YE Boqing. Extraction of metallic resources from ammonia leaching residue of electroplating sludge by solvent extraction[J]. Journal of Environmental Sciences, 1998, 11(3):35-38.
[7] 祝万鹏, 杨志华. 溶剂萃取法回收电镀污泥中的有价金属[J]. 给水排水, 1995, 32(12):16-18. ZHU Wanpeng, YANG Zhihua. Recovery of valuable metals from electroplating sludge by solvent extraction[J]. Water &Wastewater Engineering, 1995, 32(12):16-18.
[8] 齐美富, 郑园芳. 从电镀污泥中回收镍、铜和铬的工艺研究[J]. 电镀与涂饰, 2010, 29(9):43-45. QI Meifu, ZHENG Yuanfang. Study on the process of recovery copper, nickel and chromium from electroplating sludge[J]. Electroplating & Finishing, 2010, 29(9):43-45.
[9] 张冠东, 张登君, 李报厚. 从氨浸电镀污泥产物中氢还原分离铜、镍、锌的研究[J]. 过程工程学报, 1996, 34(3):214-219. ZHANG Guandong, ZHANG Dengjun, LI Baohou. Study on hydrogen reduction separation of copper, nickel and zinc from ammonia-leach electroplating sludge product[J]. The Chinese Journal of Process Engineering, 1996, 34(3):214-219.
[10] 陈凡植, 陈庆邦, 聂晓军, 等. 电镀污泥的综合利用试验研究[J]. 化工进展, 2001, 20(7):25-28. CHEN Fanzhi, CHEN Qingbang, NIE Xiaojun, et al. Study on comprehensive utilization of electroplating sludge[J]. Chemical Industry and Engineering Progress, 2001, 20(7):25-28.
[11] 陈凡植, 张岸飞, 陈淦康, 等. 含铜含镍电镀污泥的综合利用[J]. 环境与开发, 2001, 21(1):20-21. CHEN Fanzhi, ZHANG Anfei, CHEN Jinkang, et al. Comprehensive utilization of nickel-containing electroplating sludge containing copper[J]. Journal of Environment and Development, 2001, 21(1):20-21.
[12] 刘俊, 赵一先, 陈秋则. 从电镀锌废渣中回收制备锌盐的研究[J]. 上海环境科学, 2002, 23(11):672-675. LIU Jun, ZHAO Yixian, CHEN Qiuze. Study on recovery and preparation of zinc salt from electrolytic zinc residue[J]. Journal of Shanghai Environmental Sciences, 2002, 23(11):672-675.
[13] 高官金, 伍珍秀, 殷兆迁, 等. 一种回收除硅渣中钒的方法:CN103572062A[P]. 2014-02-12. GAO Guanjin, WU Zhenxiu, YIN Zhaoqian, et al. A method of recovering vanadium in silicon slag:CN103572062A[P]. 2014-02-12.
[14] 殷兆迁, 杨仰军, 李千文, 等. 一种从除磷底流渣中回收钒的方法:CN103911521A[P]. 2014-07-09 YIN Zhaoqian, YANG Yangjun, LI Qianwen, et al. A method of recovering vanadium from phosphorus removal underflow slag:CN103911521A[P]. 2014-07-09.
[15] 刘安华, 李辽沙, 余亮. 含钒固废提钒工艺及比较[J]. 安徽工业大学学报, 2003, 20(4):126-130. LIU Anhua, LI Liaosha, YU Liang. Techonoly and comparison of vanadium extraction from solid waste containing vanadium[J]. Journal of Anhui University of Technology, 2003, 20(4):126-130.
[16] 许晓海, 冯改山. 耐火材料技术手册[M]. 北京:冶金工业出版社, 2000. XU Xiaohai, FENG Gaishan. Refractory technology manual[M]. Beijing:Metallurgical Industry Press, 2000.
[17] QI X, ZHANG L, XIE W, et al. Synthesis of copper-substituted aluminophosphate molecular sieves (CuAPO-11) and their catalytic behavior for phenol hydroxylation[J]. Applied Catalysis A:General, 2004, 276(1):89-94.
[18] 巴申科, 钱清扬. 新型水泥[M]. 北京:中国建筑工业出版社. 1983. BA Shenke, QIAN Qingyang. New type cement[M]. Beijing:China Architecture & Building Press, 1983.
[19] 贡长生. 磷酸铝系分子筛的研究进展[J]. 天然气化工(C1化学与化工), 1995, 11(3):50-54. GONG Changsheng. Research progress of aluminum phosphate molecular sieves[J]. Natural Gas Chemical Industry (C1 Chemistry and Chemical Engineering), 1995, 11(3):50-54.
[20] 陈腾飞, 龚伟平, 黄伯云, 等. 航空刹车用炭/炭复合材料坯体结构研究进展[J]. 矿冶工程, 2005, 25(6):74-77. CHEN Tengfei, LONG Weiping, HUANG Boyun, et al. Research progress on the blank structure of carbon/carbon composites for aviation braking[J]. Mining and Metallurgical Engineering, 2005, 25(6):74-77.
[21] STRIFE J R, SHEEHAN J E. Ceramic coatings for carbon-carbon composites[J]. American Ceramic Society Bulletin, 1988, 67(2):369-374.
[22] 王励生, 万先达, 廖华书. 磷复肥及磷酸盐工艺学[M]. 成都:成都科技大学出版社, 1993. WANG Lisheng, WAN Xianda, LIAO Huashu. Phosphate compound fertilizer and phosphate technology[M]. Chengdu:Chengdu University of Science and Technology Press, 1993.
[23] 陈梓云, 彭梦侠. 微波诱导合成磷酸铝的研究[J]. 无机盐工业, 1999, 13(5):11. CHEN Ziyun, PENG Mengxia. Researches in microwave-induced synthesis of aluminum phosphate[J]. Inorganic Chemicals Industry, 1999, 13(5):11.