Formation of CaCO3 hollow microspheres in carbonated distiller waste from Solvay soda ash plants

doi:10.1007/s11705-022-2173-z

Frontiers of Chemical Science and Engineering

2022, Vol. 16

Issue (11): 1659-1671 https://doi.org/10.1007/s11705-022-2173-z

本期目录

Formation of CaCO₃ hollow microspheres in carbonated distiller waste from Solvay soda ash plants

Wenjiao Xu, Huaigang Cheng(

), Enze Li, Zihe Pan, Fangqin Cheng(

)

Institute of Resources and Environmental Engineering, Engineering Research Center of CO2 Emission Reduction and Resource Utilization, Ministry of Education of the People’s Republic of China, Shanxi University, Taiyuan 030006, China

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Abstract：

For decades, distiller waste and CO₂ were not the first choice for production of high valued products. Here, CaCO₃ hollow microspheres, a high-value product was synthesized from such a reaction system. The synthetic methods, the formation mechanism and operational cost were discussed. When 2.5 L·min^–1·L^–1 CO₂ was flowed into distiller waste (pH = 11.4), spheres with 4–13 μm diameters and about 2 μm shell thickness were obtained. It is found that there is a transformation of CaCO₃ particles from solid-cubic nuclei to hollow spheres. Firstly, the Ca(OH)₂ in the distiller waste stimulated the nucleation of calcite with a non-template effect and further maintained the calcite form and prevented the formation of vaterite. Therefore, in absence of auxiliaries, the formation of hollow structures mainly depended on the growth and aging of CaCO₃. Studies on the crystal morphology and its changes during the growth process point to the inside–out Ostwald effect in the formation of hollow spheres. Change in chemical properties of the bulk solution caused changes in interfacial tension and interfacial energy, which promoted the morphological transformation of CaCO₃ particles from cubic calcite to spherical clusters. Finally, the flow process for absorption of CO₂ by distiller waste was designed and found profitable.

Key words： distiller waste CO₂ hollow microsphere CaCO₃ Ca(OH)₂ inside−out Ostwald effect

收稿日期: 2022-01-28 出版日期: 2022-12-13

Corresponding Author(s): Huaigang Cheng,Fangqin Cheng

引用本文:

. [J]. Frontiers of Chemical Science and Engineering, 2022, 16(11): 1659-1671.
Wenjiao Xu, Huaigang Cheng, Enze Li, Zihe Pan, Fangqin Cheng. Formation of CaCO₃ hollow microspheres in carbonated distiller waste from Solvay soda ash plants. Front. Chem. Sci. Eng., 2022, 16(11): 1659-1671.

链接本文:

https://academic.hep.com.cn/fcse/CN/10.1007/s11705-022-2173-z
https://academic.hep.com.cn/fcse/CN/Y2022/V16/I11/1659

Fig.1

Fig.2

Fig.3

Reaction time/min	pH of solution	Concentration/(mol·L^–1)		Coefficient activity		Activity/(mol·L^–1)		J
Reaction time/min	pH of solution	$c C a 2 +$	$c O H −$	$γ C a 2 +$	$γ O H −$	$α C a 2 +$	$α O H −$	J
0 ^a)	11.4	0.85	2.51 × 10⁻³	1.19826	1.2079	1.018521	3.03 × 10⁻³	9.36 × 10⁻⁶
0 ^b)	11.4	0.85	2.51 × 10⁻³	0.30722	0.728888	0.261137	1.83 × 10⁻³	5.42 × 10⁻⁶
2	10.49	0.79	3.09 × 10⁻⁴	0.19488	0.652078	0.1539552	2.01 × 10⁻⁴	1.82 × 10⁻⁸
5	9.89	0.77	7.76 × 10⁻⁵	0.172587	0.634418	0.13289199	4.92 × 10⁻⁵	9.20 × 10⁻¹⁰
10	9.31	0.74	2.04 × 10⁻⁵	0.146964	0.612986	0.10875336	1.25 × 10⁻⁵	4.80 × 10⁻¹¹
15	8.46	0.72	2.88 × 10⁻⁶	0.133638	0.601384	0.09621936	1.73 × 10⁻⁶	8.13 × 10⁻¹³
20	5.66	0.71	4.57 × 10⁻⁹	0.127701	0.596131	0.09066771	2.72 × 10⁻⁹	1.90 × 10⁻¹⁸
60	5.16	0.71	1.45 × 10⁻⁹	0.127701	0.596131	0.09066771	8.64 × 10⁻¹⁰	1.85 × 10⁻¹⁹

Tab.1

Fig.4

Fig.5

Fig.6

Fig.7

Fig.8

Liquid value		Water	Distiller waste	The solution after reaction for
Liquid value		Water	Distiller waste	5 min	10 min	20 min
$θ$ /(° )	Test value	28.5	37.2	33.7	28.2	32.0
	Test value
	MD simulation results ^a)	–	35.6	–	26.2	31.5
	MD simulation results ^a)	–		–
$γ l g$ /(mN·m^–1)		73.43	69.25	67.73	68.50	69.78
$γ l g$ /(mN·m^–1)
$γ l s$ /(mN·m^–1) calc.		35.27	34.60	31.53	30.16	32.81

Tab.2

Fig.9

Fig.10

Tab.3

Tab.4

X_V	the molar fractions of vaterite
X_C	the molar fractions of calcite
I_c¹⁰⁴	104 crystal plane peak intensities of calcite
I_v¹¹⁰	110 crystal plane peak intensities of vaterite
$V C O 2$	the total amount of CO₂ consumed during the carbonation reaction for 1 h, L
V	the volume of solution, L
V_m	the standard molar volume of a gas, L·mol^–1
$n C a (O H) 2$	the amount of insoluble Ca(OH)₂ reacted part at time t (negligible), mol
M	molecular weight of Ca(OH)₂, g·mol^–1
n	the amount of undissolved Ca(OH)₂, mol
$c C a 0 2 +$	the initial concentration of Ca²⁺ in the solution, mol·L^–1
$c C a t 2 +$	the concentration of Ca²⁺ in the solution at time t, mol·L^–1
$c C a 2 +$	the concentration of Ca²⁺, mol·L^–1
$c O H −$	the concentration of OH^–, mol·L^–1
J	the activity products
K	solubility product constant of Ca(OH)₂, K = 5.6 × 10⁻⁶ (25 °C)
$γ C a 2 +$	the activity coefficients of Ca²⁺
$γ O H −$	the activity coefficients of OH^–
$α C a 2 +$	activity of Ca²⁺ in solution, mol·L^–1
$α O H −$	activity of OH⁻ in solution, mol·L^–1
$θ$	contact angle between calcite and liquid, (°)
$γ l s$	solid–liquid interfacial tension, mN·m^–1
$γ l g$	liquid–vapor interfacial tension, mN·m^–1
$γ s g$	solid–vapor interfacial tension, mN·m^–1, $γ s g$ = 43.5 mN·m^–1
$c C a 20 m i n 2 +$	the concentration of Ca²⁺ in the system reacted for 20 min, mol·L^–1
Y	the output of CaCO₃ hollow microspheres, kg
T	cycle times of carbonation of distiller waste
V'	the volume of distiller waste, L
M'	the molecular weight of CaCO₃, g·mol^–1

1	M Trypuć, K Białowicz. CaCO3 production using liquid waste from Solvay method. Journal of Cleaner Production, 2011, 19( 6-7): 751– 756 https://doi.org/10.1016/j.jclepro.2010.11.009
2	T Calban, E Kavci. Removal of calcium from soda liquid waste containing calcium chloride. Energy Sources, Part A: Recovery, Utilization, and Environmental Effects, 2010, 32( 5): 407– 418 https://doi.org/10.1080/15567030903261816
3	B C Sun, X M Wang, J M Chen, G W Chu, J F Chen, L Shao. Synthesis of nano-CaCO3 by simultaneous absorption of CO2 and NH3 into CaCl2 solution in a rotating packed bed. Chemical Engineering Journal, 2011, 168( 2): 731– 736 https://doi.org/10.1016/j.cej.2011.01.068
4	C Z Gao, Y Dong, H J Zhang, J M Zhang. Utilization of distiller waste and residual mother liquor to prepare precipitated calcium carbonate. Journal of Cleaner Production, 2007, 15( 15): 1419– 1425 https://doi.org/10.1016/j.jclepro.2006.06.024
5	X Zhang, E Asselin, Z Li. CaCO3 precipitation kinetics in the system CaCl2−CO2−Mg(OH)2−H2O for comprehensive utilization of soda production wastes. ACS Sustainable Chemistry & Engineering, 2020, 9( 1): 398– 410 https://doi.org/10.1021/acssuschemeng.0c07467
6	X P Luo, X W Song, Y W Cao, L Song, X Z Bu. Investigation of calcium carbonate synthesized by steamed ammonia liquid waste without use of additives. RSC Advances, 2020, 10( 13): 7976– 7986 https://doi.org/10.1039/C9RA10460G
7	C Dong, X Song, Y Li, C Liu, H Chen, J Yu. Impurity ions effect on CO2 mineralization via coupled reaction−extraction−crystallization process of CaCl2 waste liquids. Journal of CO2 Utilization , 2018, 27 : 115– 128
8	X W Song, H Liu, J F Wang, Y W Cao, X P Luo. A study of the effects of NH4+ on the fast precipitation of vaterite CaCO3 formed from steamed ammonia liquid waste and K2CO3/Na2CO3. CrystEngComm, 2021, 23( 24): 4284– 4300 https://doi.org/10.1039/D1CE00365H
9	Z Yan, Y Wang, H Yue, C Liu, S Zhong, K Ma, W Liao, S Tang, B Liang. Integrated process of monoethanolamine-based CO2 absorption and CO2 mineralization with SFGD slag: process simulation and life-cycle assessment of CO2 emission. ACS Sustainable Chemistry & Engineering, 2021, 9( 24): 8238– 8248 https://doi.org/10.1021/acssuschemeng.1c02278
10	A Alamdari, A Alamdari, D Mowla. Kinetics of calcium carbonate precipitation through CO2 absorption from flue gas into distiller waste of soda ash plant. Journal of Industrial and Engineering Chemistry, 2014, 20( 5): 3480– 3486 https://doi.org/10.1016/j.jiec.2013.12.038
11	Y Li, X Song, G Chen, Z Sun, Y Xu, J Yu. Preparation of calcium carbonate and hydrogen chloride from distiller waste based on reactive extraction−crystallization process. Chemical Engineering Journal, 2015, 278 : 55– 61 https://doi.org/10.1016/j.cej.2014.12.058
12	F Sha, N Zhu, Y J Bai, Q Li, B Guo, T X Zhao, F Zhang, J B Zhang. Controllable synthesis of various CaCO3 morphologies based on a CCUS idea. ACS Sustainable Chemistry & Engineering, 2016, 4( 6): 3032– 3044 https://doi.org/10.1021/acssuschemeng.5b01793
13	Y Ma, Q Feng, X Bourrat. A novel growth process of calcium carbonate crystals in silk fibroin hydrogel system. Materials Science and Engineering C, 2013, 33( 4): 2413– 2420 https://doi.org/10.1016/j.msec.2013.02.006
14	T W Zheng, X Zhang, H H Yi. Spherical vaterite microspheres of calcium carbonate synthesized with poly(acrylic acid) and sodium dodecyl benzene sulfonate. Journal of Crystal Growth, 2019, 528( 15): 125275 https://doi.org/10.1016/j.jcrysgro.2019.125275
15	H G Chen, S L Leng. Rapid synthesis of hollow nano-structured hydroxyapatite rnicrospheres via microwave transformation method using hollow CaCO3 precursor microspheres. Ceramics International, 2015, 41( 2): 2209– 2213 https://doi.org/10.1016/j.ceramint.2014.10.021
16	T W Zheng, H H Yi, S Y Zhang, C G Wang. Preparation and formation mechanism of calcium carbonate hollow microspheres. Journal of Crystal Growth, 2020, 549 : 125870 https://doi.org/10.1016/j.jcrysgro.2020.125870
17	J Wang, J S Chen, J Y Zong, D Zhao, F Li, R X Zhuo, S X Cheng. Calcium carbonate/carboxymethyl chitosan hybrid microspheres and nanospheres for drug delivery. Journal of Physical Chemistry C, 2010, 114( 44): 18940– 18945 https://doi.org/10.1021/jp105906p
18	R J Park, F C Meldrum. Synthesis of single crystals of calcite with complex morphologies. Advanced Materials, 2002, 14( 16): 1167– 1169 https://doi.org/10.1002/1521-4095(20020816)14:16<1167::AID-ADMA1167>3.0.CO;2-X
19	S Kim, J W Ko, C B Park. Bio-inspired mineralization of CO2 gas to hollow CaCO3 microspheres and bone hydroxyapatite/polymer composites. Journal of Materials Chemistry, 2011, 21( 30): 11070– 11073 https://doi.org/10.1039/c1jm12616d
20	G W Yan, J H Huang, J F Zhang, C J Qian. Aggregation of hollow CaCO3 spheres by calcite nanoflakes. Materials Research Bulletin, 2008, 43( 8-9): 2069– 2077 https://doi.org/10.1016/j.materresbull.2007.09.014
21	G Hadiko, Y S Han, M Fuji, M Takahashi. Synthesis of hollow calcium carbonate particles by the bubble templating method. Materials Letters, 2005, 59( 19-20): 2519– 2522 https://doi.org/10.1016/j.matlet.2005.03.036
22	T Tomioka, M Fuji, M Takahashi, C Takai, M Utsuno. Hollow structure formation mechanism of calcium carbonate particles synthesized by the CO2 bubbling method. Crystal Growth & Design, 2012, 12( 2): 771– 776 https://doi.org/10.1021/cg201103z
23	P Yan, Y P Guo, Z Xu, Z C Wang. Influence of surfactant-polymer complexes on crystallization and aggregation of CaCO3. Chemical Research in Chinese Universities, 2012, 28( 4): 737– 742
24	H Watanabe, Y Mizuno, T Endo, X W Wang, M Fuji, M Takahashi. Effect of initial pH on formation of hollow calcium carbonate particles by continuous CO2 gas bubbling into CaCl2 aqueous solution. Advanced Powder Technology, 2009, 20( 1): 89– 93 https://doi.org/10.1016/j.apt.2008.10.004
25	J Chen, L Xiang. Controllable synthesis of calcium carbonate polymorphs at different temperatures. Powder Technology, 2009, 189( 1): 64– 69 https://doi.org/10.1016/j.powtec.2008.06.004
26	B Wang, Z H Pan, Z P Du, H G Cheng, F Q Cheng. Effect of impure components in flue gas desulfurization (FGD) gypsum on the generation of polymorph CaCO3 during carbonation reaction. Journal of Hazardous Materials, 2019, 369 : 236– 243 https://doi.org/10.1016/j.jhazmat.2019.02.002
27	E Z Li, Y Lu, F Q Cheng, X M Wang, J D Miller. Effect of oxidation on the wetting of coal surfaces by water: experimental and molecular dynamics simulation studies. Physicochemical Problems of Mineral Processing, 2018, 54( 4): 1039– 1051
28	C Marcolli. Technical note: fundamental aspects of ice nucleation via pore condensation and freezing including Laplace pressure and growth into macroscopic ice. Atmospheric Chemistry and Physics, 2020, 20( 5): 3209– 3230 https://doi.org/10.5194/acp-20-3209-2020
29	H G Cheng, X Wang, B Wang, J Zhao, Y Liu, F Q Cheng. Effect of ultrasound on the morphology of the CaCO3 precipitated from CaSO4−NH3−CO2−H2O system. Journal of Crystal Growth, 2017, 469 : 97– 105 https://doi.org/10.1016/j.jcrysgro.2016.10.017
30	Q J Chen, W J Ding, H J Sun, T J Peng, G H Ma. Utilization of phosphogypsum to prepare high-purity CaCO3 in the NH4Cl−NH4OH−CO2 system. ACS Sustainable Chemistry & Engineering, 2020, 8( 31): 11649– 11657 https://doi.org/10.1021/acssuschemeng.0c03070
31	H G Cheng, X X Zhang, H P Song. Morphological investigation of calcium carbonate during ammonification−carbonization process of low concentration calcium solution. Journal of Nanomaterials, 2014, 2014 : 1– 7 https://doi.org/10.1155/2014/503696
32	H W Nesbitt. Activity coefficients of ions in alkali and alkaline-earth chloride dominated waters including seawater. Chemical Geology, 1984, 43( 1-2): 127– 142 https://doi.org/10.1016/0009-2541(84)90143-8
33	T Fanghänel, V Neck, J I Kim. The ion product of H2O, dissociation constants of H2CO3 and Pitzer parameters in the system Na+/H+/OH/HCO3−/CO32−/ClO4−/H2O at 25 °C. Journal of Solution Chemistry, 1996, 25( 4): 327– 343 https://doi.org/10.1007/BF00972890
34	J A Dean. Lang’s Handbook of Chemistry. New York: The Kingsport Press, 1985, 5– 8
35	B Li, H C Zeng. Architecture and preparation of hollow catalytic devices. Advanced Materials, 2019, 31( 38): 1801104 https://doi.org/10.1002/adma.201801104
36	X Yang, J Fu, C Jin, J Chen, C Liang, M Wu, W Zhou. Formation mechanism of CaTiO3 hollow crystals with different microstructures. Journal of the American Chemical Society, 2010, 132( 40): 14279– 14287 https://doi.org/10.1021/ja106461u
37	W Ding, L Hu, Z Sheng, J Dai, X Zhu, X Tang, Z Hui, Y Sun. Magneto-acceleration of Ostwald ripening in hollow Fe3O4 nanospheres. CrystEngComm, 2016, 18( 33): 6134– 6137 https://doi.org/10.1039/C6CE01021K
38	W Weng, J Lin, Y Du, X Ge, X Zhou, J Bao. Template-free synthesis of metal oxide hollow micro-/nanospheres via Ostwald ripening for lithium-ion batteries. Journal of Materials Chemistry A: Materials for Energy and Sustainability, 2018, 6( 22): 10168– 10175 https://doi.org/10.1039/C8TA03161D
39	W Zhao, C Zhang, F Geng, S Zhuo, B Zhang. Nanoporous hollow transition metal chalcogenide nanosheets synthesized via the anion-exchange reaction of metal hydroxides with chalcogenide ions. ACS Nano, 2014, 8( 10): 10909– 10919 https://doi.org/10.1021/nn504755x
40	Y D Yin, R M Rioux, C K Erdonmez, S Hughes, G A Somorjai, A P Alivisatos. Formation of hollow nanocrystals through the nanoscale Kirkendall effect. Science, 2004, 304( 5671): 711– 714 https://doi.org/10.1126/science.1096566
41	H J Fan, U Gösele, M Zacharias. Formation of nanotubes and hollow nanoparticles based on Kirkendall and diffusion processes: a review. Small, 2007, 3( 10): 1660– 1671 https://doi.org/10.1002/smll.200700382
42	H J Fan, M Knez, R Scholz, K Nielsch, E Pippel, D Hesse, M Zacharias, U Gösele. Monocrystalline spinel nanotube fabrication based on the Kirkendall effect. Nature Materials, 2006, 5( 8): 627– 631 https://doi.org/10.1038/nmat1673
43	J N Gao, Q S Li, H B Zhao, L S Li, C L Liu, Q H Gong, L M Qi. One-pot synthesis of uniform Cu2O and CuS hollow spheres and their optical limiting properties. Chemistry of Materials, 2008, 20( 19): 6263– 6269 https://doi.org/10.1021/cm801407q
44	V R Gayevskii, V Z Kochmarskii, S G Gayevska. Nucleation and crystal growth of calcium sulfate dihydrate from aqueous solutions: speciation of solution components, kinetics of growth, and interfacial tension. Journal of Crystal Growth, 2020, 548 : 125844 https://doi.org/10.1016/j.jcrysgro.2020.125844
45	K S Keller, M H Olsson, M Yang, S L Stipp. Adsorption of ethanol and water on calcite: dependence on surface geometry and effect on surface behavior. Langmuir, 2015, 31( 13): 3847– 3853 https://doi.org/10.1021/la504319z
46	Z Gao, C Li, W Sun, Y Hu. Anisotropic surface properties of calcite: a consideration of surface broken bonds. Colloids and Surfaces. A, Physicochemical and Engineering Aspects, 2017, 520 : 53– 61 https://doi.org/10.1016/j.colsurfa.2017.01.061
47	M A Tabar, Y Shafiei, M Shayesteh, A D Monfared, M H Ghazanfari. Wettability alteration of calcite rock from gas-repellent to gas-wet using a fluorinated nanofluid: a surface analysis study. Journal of Natural Gas Science and Engineering, 2020, 83 : 103613 https://doi.org/10.1016/j.jngse.2020.103613
48	U Ulusoy, C Hiçyılmaz, M Yekeler. Role of shape properties of calcite and barite particles on apparent hydrophobicity. Chemical Engineering and Processing, 2004, 43( 8): 1047– 1053 https://doi.org/10.1016/j.cep.2003.10.003
49	Z Q Chen. Colloid and Interface Chemistry. Peking: Higher Education Press, 2001, 95– 104 (In Chinese)
50	W R Tyson, W A Miller. Surface free energies of solid metals: estimation from liquid surface tension measurements. Surface Science, 1977, 62( 1): 267– 276 https://doi.org/10.1016/0039-6028(77)90442-3
51	S Y Pan, E E Chang, P C Chiang. Chiang P C. CO2 capture by accelerated carbonation of alkaline wastes: a review on its principles and applications. Aerosol and Air Quality Research , 2012, 12( 5): 770– 791 https://doi.org/10.4209/aaqr.2012.06.0149
52	J J Ruan, J X Huang, L P Dong, Z Huang. Environmentally friendly technology of recovering nickel resources and producing nano-Al2O3 from waste metal film resistors. ACS Sustainable Chemistry & Engineering, 2017, 5( 9): 8234– 8240 https://doi.org/10.1021/acssuschemeng.7b01900

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