Preparation of calcium carbonate by bubble disturbance enhanced impinging stream co-precipitation method

doi:10.11949/0438-1157.20250029

Abstract

Abstract:

In order to investigate the mechanism of the preparation of calcium carbonate (CaCO₃) powders by the bubble disturbance enhanced impinging stream reactor, CaCO₃ powders with different crystal structures and contents were prepared by the impinging stream co-precipitation method. The effects of reaction temperature on the precipitation form and transformation process of CaCO₃ crystals under bubble disturbance were investigated, and the crystal phase content, nucleation rate and particle size of CaCO₃ crystals at different gas-liquid flow ratios were studied. The experimental results show that the reaction temperature is the key factor affecting the crystal morphology, and with the increase of temperature, the precipitation form of CaCO₃ crystals changes in the order of calcite, vaterite and aragonite. The bubble disturbance can effectively regulate the CaCO₃ crystal content and particle size. With the increase of gas-liquid flow ratio, the content of vaterite CaCO₃first decreases and then increases, the nucleation rate first increases and then decreases, and the average particle size first decreases and then increases. When the gas-liquid flow ratio r=1.00, the content of vaterite in the product reaches the highest level and the average particle size is the smallest. This research provides a reference for regulating the morphology of CaCO₃ crystals in impinging stream reactor.

Key words: impinging stream reactor, particle, powder technology, crystallized, calcium carbonate

摘要：

为了探究气泡扰动强化撞击流反应器制备碳酸钙（CaCO₃）粉体机制，通过撞击流共沉淀法，制备了具有不同晶体结构和含量的CaCO₃粉体，考察了气泡扰动下反应温度对CaCO₃晶体析出形式和转化过程的影响，研究了不同气液流量比下CaCO₃晶体的晶相含量、成核速率及粒径尺寸。实验结果表明，反应温度是影响晶体形貌的关键因素，随着温度升高，CaCO₃晶体析出形式依次为方解石、球霰石、文石。气泡扰动可有效调控CaCO₃晶体含量和粒径尺寸。随着气液流量比增大，球霰石型CaCO₃含量先降低后升高，成核速率先增大后减小，平均粒径先减小后增大。当气液流量比r=1.00时，产物中球霰石的含量达到最高水平，且平均粒径最小。为撞击流反应器可控制备CaCO₃提供了参考。

关键词: 撞击流反应器, 粒子, 粉体技术, 结晶, 碳酸钙

CLC Number:

TQ 027.1

Jianwei ZHANG, Yucheng LIU, Xin DONG, Ying FENG. Preparation of calcium carbonate by bubble disturbance enhanced impinging stream co-precipitation method[J]. CIESC Journal, 2025, 76(8): 4052-4060.

张建伟, 刘玉成, 董鑫, 冯颖. 气泡扰动强化撞击流共沉淀法合成碳酸钙粉体[J]. 化工学报, 2025, 76(8): 4052-4060.

Figures/Tables 13

Fig.1 Experimental system diagram of impinging stream reactor

Fig.2 Structure of impinging stream reactor

Table 1 Experimental parameter

组别	反应温度T/℃	气液流量比r	组别	反应温度T/℃	气液流量比r
1	20	1.00	10	30	0.75
2	30	1.00	11	30	1.00
3	40	1.00	12	30	1.25
4	50	1.00	13	50	0
5	60	1.00	14	50	0.25
6	70	1.00	15	50	0.50
7	30	0	16	50	0.75
8	30	0.25	17	50	1.00
9	30	0.50	18	50	1.25

Fig.3 Preparation process of calcium carbonate

Fig.4 SEM images of CaCO3 prepared at different reaction temperatures

Fig.5 XRD patterns of CaCO3 prepared at different reaction temperatures

Fig.6 Trends in the solubility of the three crystals at different reaction temperatures

Fig.7 The transformation process of CaCO3 crystals at different reaction temperatures

Fig.8 Content of three crystals of CaCO3 at different reaction temperatures

Fig.9 Content of crystals of CaCO3 at different gas-liquid flow ratio

Fig.10 Crystal particle number density under different gas-liquid flow ratio

Table 2 Crystallization kinetics parameters under different gas-liquid flow ratio

流量比 $r$	晶核粒数密度n⁰/(10⁹ μm^-1·ml^-1)	生长速率G/(μm/min)	成核速率B⁰/ (10⁸ ml^-1·min^-1)	悬浮密度M_T/(g/ml)
0	4.995	0.0432	2.159	0.0114
0.25	15.037	0.0386	5.810	0.0115
0.50	25.693	0.0322	8.265	0.0122
0.75	23.595	0.0332	7.843	0.0119
1.00	3.287	0.0581	1.910	0.0127
1.25	4.825	0.0497	2.397	0.0115

Table 2 Crystallization kinetics parameters under different gas-liquid flow ratio

流量比 $r$	晶核粒数密度n⁰/(10⁹ μm^-1·ml^-1)	生长速率G/(μm/min)	成核速率B⁰/ (10⁸ ml^-1·min^-1)	悬浮密度M_T/(g/ml)
0	4.995	0.0432	2.159	0.0114
0.25	15.037	0.0386	5.810	0.0115
0.50	25.693	0.0322	8.265	0.0122
0.75	23.595	0.0332	7.843	0.0119
1.00	3.287	0.0581	1.910	0.0127
1.25	4.825	0.0497	2.397	0.0115

Fig.11 Mean particle size of vaterite at different gas-liquid flow ratio

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