高镁炉渣酸解液硅酸自聚-离心脱硅工艺研究

doi:10.19964/j.issn.1006-4990.2022-0076

摘要/Abstract

摘要：

利用酸法提取高炉渣中有价元素的过程中，存在着酸解液硅浓度过高的问题，不利于后续的过滤和金属元素的进一步富集，因此需要进行脱硅操作。针对溶液中硅的脱除问题，基于硅酸自聚原理，提出了硅酸自聚-离心脱硅的实验方法，该方法避免了沉淀法容易引入杂质的问题，适合酸性环境下高浓度硅的脱出。研究了不同实验条件对脱硅率的影响，采用电感耦合等离子体发射光谱（ICP-OES）对脱硅液成分进行分析，并通过X射线衍射（XRD）、扫描电镜-能谱（SEM-EDS）对离心硅渣的晶体结构和微观形貌进行分析，同时采用傅里叶红外（FT-IR）和核磁共振谱（NMR）研究硅酸聚合过程。通过实验发现，脱硅的最适宜工艺条件为：c（H⁺）为3.5 mol/L，反应温度为70 ℃，保温时间为2 h，离心转速为3 500 r/min，离心时间为3 min。在该条件下达到了99.5%的脱硅率。

关键词: 炉渣, 脱硅, 硅酸自聚, 离心脱硅

Abstract:

The extraction of valuable elements from blast furnace slag by using the acid method suffers from the problem of high silicon concentration in the acid solution，which is not conducive to subsequent filtration and further enrichment of metallic elements，so desilication operations are required.For the problem of desilication from solution，an experimental method of silicic acid self-polymerization-centrifugal desilication was proposed based on the principle of silicic acid self-polymerization，which avoided the problem of easy introduction of impurities by precipitation method and was suitable for the removal of high concentration of silicon under acidic environment.The effects of different experimental conditions on the desilication rate were investigated.The composition of the desilication solution was analyzed by inductively coupled plasma optical emission spectroscopy（ICP-OES），and the crystal structure and microscopic morphology of centrifugal silica slag were analyzed by X-ray diffraction analysis（XRD） and scanning electron microscopy-energy dispersive specterometer（SEM-EDS），while fourier transform infrared spectroscopy（FT-IR） and nuclear magnetic resonance spectroscopy（NMR） were used to study the silicic acid polymerization process.It was found that the optimum process conditions for desilication were：c（H⁺） of 3.5 mol/L，reaction temperature of 70 ℃，holding time of 2 h，centrifugal speed of 3 500 r/min and centrifugal time of 3 min，and the desilication rate of 99.5% was achieved under these conditions.

Key words: slag, desilication, silicic acid self-polymerization, centrifugal desilication

中图分类号:

X705

姚衡,汤建伟,刘咏,刘鹏飞,化全县,王保明. 高镁炉渣酸解液硅酸自聚-离心脱硅工艺研究[J]. 无机盐工业, 2022, 54(11): 83-89.

YAO Heng,TANG Jianwei,LIU Yong,LIU Pengfei,HUA Quanxian,WANG Baoming. Study on desilication process of silicic acid from high magnesium slag acidolysis solution by self-polymerization and centrifugal[J]. Inorganic Chemicals Industry, 2022, 54(11): 83-89.

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参考文献 15

1	杜小旺,仲剑初,王孝天.高硅水镁石钠化焙烧法除硅工艺研究[J].无机盐工业,2020,52(10):92-95.
	DU Xiaowang, ZHONG Jianchu, WANG Xiaotian.Study on removal of silicon from high-silicon brucite by sodium roasting method[J].Inorganic Chemicals Industry,2020,52(10):92-95.
2	李兵,李杰,张遵乾.高炉渣热资源回收及利用展望[J].科技风,2022(4):87-91.
	LI Bing, LI Jie, ZHANG Zunqian.Blast furnace slag heat resource recovery and prospect of utilization[J].Technology Wind,2022(4):87-91.
3	李晨.空冷高钛型高炉渣中主要组分的分离提取研究[D].成都：成都理工大学，2012.
	LI Chen.Study on the separation and extraction of the main components from air-cooled high Ti-bearing blast furnace slag[D].Chen-gdu：Chengdu University of Technology,2012.
4	HUANG Yukun, GENG Yangbo, HAN Guihong, et al.A perspective of stepwise utilization of hazardous zinc plant purification residue based on selective alkaline leaching of zinc[J].Journal of Hazardous Materials,2020,389.Doi:10.1016/j.jhazmat.2020.122090. doi: 10.1016/j.jhazmat.2020.122090
5	WANG Lingyun, LEE M S.Separation of zirconium and hafnium from nitric acid solutions with LIX 63，PC 88A and their mixture by solvent extraction[J].Hydrometallurgy,2014,150: 153-160.
6	连水瑕.高炉渣中二氧化硅选择性提取及应用研究[D].太原：太原理工大学，2021.
	LIAN Shuixia.Study on selective extraction and application of silicon oxide from blast furnace slag[D].Taiyuan：Taiyuan University of Technology，2021.
7	杜阳.富钨渣中回收钨的研究[D].西安：西安建筑科技大学，2014.
	DU Yang.Research on recovery of tungsten from enriched tungsten residue[D].Xi'an：Xi'an University of Architecture and Technology，2014.
8	韩东,张强,张敏.含碱硅酸钠溶液的回收和利用工艺研究[J].无机盐工业,2022,54(2):106-110.
	HAN Dong, ZHANG Qiang, ZHANG Min.Study on recovery and utilization process of alkali containing sodium silicate solution[J].Inorganic Chemicals Industry,2022,54(2):106-110.
9	孙双双,仲剑初,王洪志.铜冶炼废渣脱硅工艺研究[J].无机盐工业,2021,53(9):83-87.
	SUN Shuangshuang, ZHONG Jianchu, WANG Hongzhi.Study on desiliconization process of copper smelting slag[J].Inorganic Che-Industry micals,2021,53(9):83-87.
10	张向超.水溶液中硅、铁、铜杂质的脱除研究[D].天津：河北工业大学，2017.
	ZHANG Xiangchao.Removal of silicon，iron and copper impurities in aqueous solution[D].Tianjin：Hebei University of Technology，2017.
11	袁杰,和晓才,宋宁,等.铝酸钠溶液氧化钙深度脱硅研究[J].矿冶,2015,24(1):57-60.
	YUAN Jie, HE Xiaocai, SONG Ning, et al.Deep desiliconization of sodium aluminate solution with CaO[J].Mining and Metallurgy,2015,24(1):57-60.
12	吴江,王雨,薛天艳,等.氧氯化锆生产中转型料酸解与絮凝脱硅过程[J].过程工程学报,2013,13(6):986-991.
	WU Jiang, WANG Yu, XUE Tianyan, et al.Acid decomposition and desilication by flocculation of transformation mass in production of zirconium oxychloride[J].The Chinese Journal of Process Engineering,2013,13(6):986-991.
13	杨丽静,田辉平,龙军,等.碱性硅溶胶稳定性的研究[J].石油炼制与化工,2010,41(6):12-16.
	YANG Lijing, TIAN Huiping, LONG Jun, et al.Study on the stability of alkaline silica sol[J].Petroleum Processing and Petrochemicals,2010,41(6):12-16.
14	陈和生,孙振亚,邵景昌.八种不同来源二氧化硅的红外光谱特征研究[J].硅酸盐通报,2011,30(4):934-937.
	CHEN Hesheng, SUN Zhenya, SHAO Jingchang.Investigation on FT-IR spectroscopy for eight different sources of SiO₂ [J].Bulletin of the Chinese Ceramic Society,2011,30(4):934-937.
15	朱振峰,李晖,朱敏.微乳液法制备无定形纳米二氧化硅[J].无机盐工业,2006,38(6):14-16.
	ZHU Zhenfeng, LI Hui, ZHU Min.The preparation of amorphous silica nanoparticls by microemulsion method[J].Inorganic Che-Industry micals,2006,38(6):14-16.

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