针状碳酸钙制备中氯化镁晶型导向剂的套用研究

doi:10.3724/SP.J.1077.2011.01199

无机材料学报 ›› 2011, Vol. 26 ›› Issue (11): 1199-1204.DOI: 10.3724/SP.J.1077.2011.01199

针状碳酸钙制备中氯化镁晶型导向剂的套用研究

马俊, 刘华彦, 陈银飞

(浙江工业大学化学工程与材料学院, 绿色化学合成技术省部共建国家重点实验室培育基地, 杭州 310014)

收稿日期:2010-12-21 修回日期:2011-02-21 出版日期:2011-11-20 网络出版日期:2011-11-11
作者简介:马俊(1985-), 男, 硕士研究生. E-mail: mj3488388@163.com

Reuse of MgCl₂ as Crystal Controlling Agent in the Synthesis Process of Needle-like Calcium Carbonate

MA Jun, LIU Hua-Yan, CHEN Yin-Fei

(College of Chemical Engineering and Materials Science, Zhejiang University of Technology, State Key Laboratory Breeding Base of Green Chemistry-Synthesis Technology, Hangzhou 310014, China)

Received:2010-12-21 Revised:2011-02-21 Published:2011-11-20 Online:2011-11-11

摘要/Abstract

摘要： 以MgCl₂为晶型导向剂制备了形貌规整的文石相针状碳酸钙, 其粒径为2.5~5.0μm, 长径比为10~20. 采用EDTA络合滴定碳化后回收滤液中Ca²⁺、Mg²⁺含量以确定需补加MgCl₂量, 并在相同的碳化工艺条件下逐步改进套用回收液的方法制备针状碳酸钙. 产品用SEM、XRD进行形貌观察和晶型组成分析. 结果表明, 随着套用次数的增加, 碳酸钙产品中文石相的含量逐渐降低, 当文石相的含量低于80%时, 针状碳酸钙的长径比也大幅下降, 同时生成大量微细立方状方解石相碳酸钙, 将不适合继续套用. 直接套用回收液时只能循环使用1次, 而将套用的回收液经补加Mg²⁺、加酸调节pH等优化处理后可使套用次数延长至12次, 这将大幅降低针状碳酸钙的生产成本.

关键词: 针状碳酸钙, 氯化镁, 络合滴定, 套用

Abstract: MgCl₂ was used as crystal controlling agent for the synthesis of regular needle-like calcium carbonate with diameter of 2.5-5μm and aspect ratio of 10-20. Complexometric titrating method was employed to determine the contents of Ca²⁺ and Mg²⁺ in filtrated solution after carbonization and the fresh MgCl₂ was added to balance the Mg²⁺ content as same as the raw solution. The morphology, particle size and polymorphs of calcium carbonate were characterized by SEM and XRD. The results show that the content of aragonite phase CaCO₃ decreases with the recycle time increasing. When the content of aragonite phase CaCO₃ is lower than 80%, the aspect ratio of need-like calcium carbonate decreases significantly companied with the production of calcite cubic CaCO₃ particles, thus the filtrated MgCl₂ solution is unsuitable to recycled anymore. The direct recycle filtrate can be used for only once while the reused time by the MgCl2 filtrate can reach 12 by optimizing the recycle process through the addition of Mg²⁺ and the justification of pH of the filtrate.

Key words: needle-like calcium carbonate, magnesium chloride, complexometric titration, reuse

中图分类号:

TQ132

马俊, 刘华彦, 陈银飞. 针状碳酸钙制备中氯化镁晶型导向剂的套用研究[J]. 无机材料学报, 2011, 26(11): 1199-1204.

MA Jun, LIU Hua-Yan, CHEN Yin-Fei. Reuse of MgCl₂ as Crystal Controlling Agent in the Synthesis Process of Needle-like Calcium Carbonate[J]. Journal of Inorganic Materials, 2011, 26(11): 1199-1204.

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针状碳酸钙制备中氯化镁晶型导向剂的套用研究

Reuse of MgCl₂ as Crystal Controlling Agent in the Synthesis Process of Needle-like Calcium Carbonate

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针状碳酸钙制备中氯化镁晶型导向剂的套用研究

Reuse of MgCl2 as Crystal Controlling Agent in the Synthesis Process of Needle-like Calcium Carbonate

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Reuse of MgCl₂ as Crystal Controlling Agent in the Synthesis Process of Needle-like Calcium Carbonate