| 引用本文: | 于攀,汪李超,苗继娟,刘志福,王操,赵喆.高通量合成方法制备球霞石相CaCO3材料及表征[J].材料科学与工艺,2017,25(5):6-12.DOI:10.11951/j.issn.1005-0299.20170044. |
| YU Pan,WANG Lichao,MIAO Jijuan,LIU Zhifu,WANG Cao,ZhAO Zhe.Preparation and characterization of nepheline phase CaCO3 by high throughput synthesis[J].Materials Science and Technology,2017,25(5):6-12.DOI:10.11951/j.issn.1005-0299.20170044. |
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| 摘要: |
| 高通量合成CaCO3方法为该材料的工业生产提供一定的理论基础，其目的是为了获得粒度分布均匀、比表面积高、球霞石相含量高的花蕊状CaCO3.利用高通量合成材料的优势，设计并构建了自动加注试剂、独立控温及控速的高通量自动合成装置，并进行了合成CaCO3的工作.以氯化钙、碳酸钠、咖啡酸为原料，在同一时间内完成不同实验条件下CaCO3的合成，采用X射线衍射(XRD)、扫描电镜(SEM)、激光粒度仪，对样品的结构、形貌、粒径分布进行表征和分析，并利用高通量合成实验方法进行CaCO3合成优化实验.结果表明：在水和乙醇分别作为溶剂时，合成球霞石相(晶形)CaCO3的含量不同.即咖啡酸浓度20 mg/mL(乙醇为溶剂，10 mL)、CaCl2与Na2CO3的物质的量之比为3:1时，合成粒度分布均匀、花蕊状、球霞石相(晶形)含量高达98.31%、比表面积为51.9 m2/g的CaCO3材料.与传统合成实验方法相比，高通量合成将会缩短研发及合成时间.
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| 关键词: 高通量合成 共沉淀法 CaCO3 制备 优化实验 |
| DOI：10.11951/j.issn.1005-0299.20170044 |
| 分类号:TQ132.32；TP23 |
| 文献标识码:A |
| 基金项目:上海市扬帆计划(14YF1410800)；上海高校青年教师培养资助计划(ZZyy15086). |
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| Preparation and characterization of nepheline phase CaCO3 by high throughput synthesis |
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YU Pan1, WANG Lichao2, MIAO Jijuan1, LIU Zhifu3, WANG Cao3, ZhAO Zhe3
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(1.College of Mechanical Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2.College of Materials Science and Engineering, Donghua University, Shanghai 201418, China; 3. College of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China)
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| Abstract: |
| The high-throughput synthesis of CaCO3 provides a theoretical basis for its industrial production, aiming to achieve an uniform distribution of particle size, a high specific surface area, and a high content of nepheline phase flower-like CaCO3. Taking advantages of the high-throughput materials-synthesis method, an automatic high-throughput synthesis apparatus with agent-filling and independent temperature and speed controlling, was designed and fabricated. The synthesis of CaCO3 powder under different experimental conditions was carried out at the same time with calcium chloride, sodium carbonate and caffeic acid as raw materials. The structure, morphology, and particle size were examined using X-ray diffraction (XRD), scanning electron microscope (SEM) and laser particle size analyzer, and the optimization experiments of CaCO3 synthesis were performed. The results indicated that, when used the water or ethanol as a solvent, the synthetic nepheline phase (crystalline) CaCO3 content is different. The well-ordered particle size, flower-like, celestite phase content of up to 98.31%, specific surface area (51.9 m2/g) of CaCO3 was obtained with the optimum synthesis conditions in the presence of caffeic acid concentration of 20 mg/mL (in an ethanol solvent, 10 mL), n(CaCl2):n(Na2CO3)=3:1. Compared with the traditional synthesis method, high-throughput automatic synthesis will effectively shorten the R & D and synthesis time.
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| Key words: high-throughput synthesis Co-precipitation process CaCO3 synthesis optimization experiment |
