微通道连续沉淀法制备球形BaTiO3颗粒及其在医学检测干片上的应用

doi:10.11949/0438-1157.20190786

摘要/Abstract

摘要：

以BaCl₂、TiCl₄、NaOH为原料，采用微通道连续沉淀法制备纳米级球形形貌的BaTiO₃颗粒。考察了钡浓度、体积流量、反应温度及两分支物料流量比等因素对产物形貌及粒径大小的影响，并将其与间歇沉淀法得到的产物进行了比较。实验结果表明：钡浓度0.15 mol/L，碱浓度3 mol/L，两分支物料体积流量均为2 ml/min，反应温度90℃条件下可制备得到具有规整球形形貌、粒径分布均匀的纳米级BaTiO₃颗粒，其粒径为80～150 nm。最后，将所得BaTiO₃扩散层应用到肌酸激酶干片中，重复性较好，且浓度梯度明显，光反射率值与浓度的关系与之对应。结果具有较高的可信度，说明微通道连续沉淀法得到的BaTiO₃颗粒在医用干片上应用是可行的。

关键词: 微通道, 沉淀, 制备, BaTiO₃, 医学检测干片

Abstract:

Using BaCl₂, TiCl₄ and NaOH as raw materials, BaTiO₃ particles with nanometer spherical morphology were prepared by the method of microchannel continuous precipitation. The effects of barium concentration, volume flow rate, reaction temperature and flow ratio of two branches on the morphology and particle size of the products were investigated. And the products were compared with those obtained by batch precipitation. The results show that spherical BaTiO₃ particles with uniform particle size distribution can be prepared under the condition of 90℃, 0.15 mol/L Ba concentration, 3 mol/L alkali concentration, and 2 ml/min of each branch volume flow. The particle size of prepared powders was 80－150 nm. The obtained BaTiO₃ diffusion layer was applied to the creatine kinase dry sheet, and the repeatability was good. Besides, the apparent concentration gradient was showed, and the relationship between the light reflectance value and the concentration was corresponding to the reaction phenomenon. The results have high reliability, indicating that the BaTiO₃ particles obtained by the microchannel continuous precipitation method are feasible to be applied in medical test dry film.

Key words: microchannel, precipitation, preparation, BaTiO₃, medical test dry film

中图分类号:

TQ 132.3

张宝丹, 翟佳羽, 靳海波, 郭晓燕, 杨索和, 何广湘, 马磊. 微通道连续沉淀法制备球形BaTiO₃颗粒及其在医学检测干片上的应用[J]. 化工学报, 2020, 71(3): 1370-1379.

Baodan ZHANG, Jiayu ZHAI, Haibo JIN, Xiaoyan GUO, Suohe YANG, Guangxiang HE, Lei MA. Preparation of spherical BaTiO₃ particles using microchannel continuous method and its application in medical test dry film[J]. CIESC Journal, 2020, 71(3): 1370-1379.

图/表 12

图1 微通道连续沉淀法实验装置

Fig.1 Experimental apparatus for microchannel precipitation method

图2 不同钡浓度对应的BaTiO3形貌图

Fig.2 Morphology of BaTiO3 obtained at different barium concentrations

图3 不同体积流量对应的BaTiO3形貌图

Fig.3 Morphology of BaTiO3 obtained at different volume flows

图4 不同体积流量对应BaTiO3的粒径分布

Fig.4 Particle-size distributions of BaTiO3 particles obtained at different volume flows

图5 微通道连续法制备的BaTiO3的XRD谱图

Fig.5 XRD patterns of BaTiO3 powders obtained by microchannel continuous method

图6 不同反应温度对应的BaTiO3形貌图

Fig.6 Morphology of powders obtained at different reaction temperatures

图7 不同反应温度对应BaTiO3的FT-IR谱图

Fig.7 FT-IR spectra of BaTiO3 powders obtained at different reaction temperatures

图8 不同反应温度对应BaTiO3的XRD谱图

Fig.8 XRD patterns of BaTiO3 powders obtained at different reaction temperatures

图9 不同体积流量比V A/V B对应的BaTiO3形貌图

Fig.9 Morphology of BaTiO3 obtained at different volume flow ratios of V A/V B

图10 不同制备方法所得产物的形貌图

Fig.10 Morphology of BaTiO3 obtained at different preparation methods

图11 样品重复性测试

Fig.11 Repeatability test

图12 不同浓度梯度反应后扩散层反射率及显色斑点图

Fig.12 Diffusion layer reflectivity and color pattern after reaction at different concentration

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微通道连续沉淀法制备球形BaTiO₃颗粒及其在医学检测干片上的应用

Preparation of spherical BaTiO₃ particles using microchannel continuous method and its application in medical test dry film

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