Synthesis of vaterite CaCO3 micro-spheres by carbide slag and a novel CO2-storage material

Journal of CO2 Utilization 18 (2017) 23–29

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Synthesis of vaterite CaCO3 micro-spheres by carbide slag and a novel CO2-storage material Bo Guo, Tianxiang Zhao, Feng Sha, Fei Zhang, Qiang Li, Jing Zhao, Jianbin Zhang* College of Chemical Engineering, Inner Mongolia University of Technology, Huhhot 010051, China

A R T I C L E I N F O

Article history: Received 21 May 2016 Received in revised form 9 January 2017 Accepted 10 January 2017 Available online 14 January 2017 Keywords: Crystallization Vaterite CaCO3 micro-spheres Utilization of CO2 CO2-storage material Carbide slag

A B S T R A C T

A facile and direct hydrothermal method for the crystallization of vaterite CaCO3 micro-spheres in the presence of carbide slag saturated limpid solution and a new CO2-storage material (CO2SM), which was obtained from an equimolar system of 1,2-ethylenediamine (EDA) + 1,2-ethylene glycol (EG) uptaking CO2 (ChemPhysChem., 16 (2015) 2106), was presented without any outside additives. It’s worth noting that the morphologies of CaCO3 precipitates could be controlled as homogeneous spherical-like (pure vaterite) at the 100 g L
1 CO2SM concentration for 90 min at 100  C, in which released EDA and/or EG from the CO2SM was used as surfactants. After the precipitation of CaCO3 crystals in 100 g L
1 CO2SM solution, the filtered solution could not only be reused to absorb CO2, but also to prepare the same crystal phase CaCO3 micro-particles repeatedly with the addition of carbide slag. Thus, this novel synthesis process of CaCO3 micro-particles with carbide slag and the CO2SM offers an alternative way for the comprehensive utilization of CO2 and the solid waste carbide slag. © 2017 Elsevier Ltd. All rights reserved.

1. Introduction Carbon dioxide (CO2) is believed to be the most significant contributor to climate change, and the scientific community is researching alternative energy sources and developing systems for the capture, storage and utilization of CO2 [1–5]. Currently, a variety of strategies were adopted to limit and reduce CO2 emission, including CO2 capture and storage (CCS) technique [6– 13] and CO2 capture and utilization (CCU) technique [14,15]. In the CCS and CCU techniques, the traditional alkanolamine-based technologies, including monoethanolamine (MEA), diethanolamine (DEA), and methyldiethanolamine (MDEA) were often used to capture CO2 [16]. However, the volatility and corrosive nature of amines were the major drawbacks of those alkanolamine-based technologies. Recently, Jessop [17] reported a series of innovative CO2 binding organic liquids (CO2BOLs) from alcohols and amidine (or guanidine) superbases, which could reduce the volatility of amines and convert CO2 into ammonium or guanidinium alkycarbonate salts. Nevertheless, the systems of containing amidine (or guanidine) superbases were too expensive to attract much attention in industry. Specially, our previous work [18] had

* Corresponding author. E-mail address: [email protected] (J. Zhang). http://dx.doi.org/10.1016/j.jcou.2017.01.004 2212-9820/© 2017 Elsevier Ltd. All rights reserved.

reported a new CO2 capture and storage method, which converted CO2 into a novel solid CO2SM by the equimolar EDA + EG system. Carbide slag is a type of alkaline waste from the chlor-alkali industry, and millions of tons of carbide slag are produced each year [19,20]. Moreover, carbide slag is identified as an industrial solid waste that can not be recovered with an economical way, and most of them are disposed in landfills, which will result in wastes of calcium and land resources and cause environmental pollution [21]. Currently, as carbide slag is mainly composed of Ca(OH)2 (about 90 wt%), some efforts have been made to reuse carbide slag and convert it into harmless and useful materials [22,23] including as a part of cement raw materials [24] and as a cementing paste [25]. It is generally known that CaCO3 has three anhydrous crystalline polymorphs: vaterite, aragonite and calcite [26]. The vaterite form can crystallize in either an orthorhombic or a hexagonal structure, and vaterite particles do not show well defined morphologies and usually aggregate into spherical particles [27]. Vaterite is rarely found in either biological or nonbiological systems, as it easily and irreversibly transforms into a more thermodynamically stable phase via a solvent-mediated process [28]. Vaterite, however, is expected to be used for various purposes, because it has some features such as higher specific surface area, higher solubility, higher dispersion, and smaller specific gravity compared to the other two crystal systems [29]. Therefore, the control of the particle size of spherical vaterite is more important for application as pigments, fillers, and dentifrice.

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In this work, a novel CCU and waste resource reuse approach was developed, in which the equimolar EDA + EG system could absorb CO2 to afford the CO2SM, and then the CO2SM and carbide slagsaturated limpid solution were used to control the morphology of vaterite CaCO3 micro-particles (Fig. 1), and the released EDA and/or EG from the CO2SM was used as surfactant. Additionally, the filtered solution after synthesis without a CaCO3 precipitate could not only be reused to absorb CO2, but it could also prepare the same crystal phase vaterite CaCO3 micro-particles repeatedly with the addition of carbide slag. 2. Experimental section

diffraction (XRD) patterns were collected on a powder X-ray diffractometer (XD8-Adrance, Bruker, Germany) with Cu Ka radiation and scanning rate of 0.05 s
1. A mixed crystal containing calcite, vaterite and aragonite is expected to molar content (%) yield an intensity described by Eqs. (1)–(3) [30]: XA ¼

XC ¼

2.1. Materials Analytical grade EDA was purchased from Tianjin Reagent Company. Analytical grade EG was purchased from Beijing Reagent Company. Compressed CO2 (99.999 vol.%) was purchased from the Standard Things Center (China). The carbide slag sample was obtained from Chayouhouqi carbide factory (Chayouhouqi city, China). The CO2SM was derived from the equimolar EDA + EG system uptaking CO2 and confirmed as alkycarbonate salt [18]. All the reagents used were analytical grade. 2.2. Synthetic procedures The crystallization of CaCO3 was carried out in a temperature range of 80–120  C with 50 mL of carbide slag saturated limpid solution and 0.1–5 g of CO2SM via hydrothermal reaction method. Typically, approximately 5 g of CO2SM was mixed with 50 mL carbide slag saturated solution firstly, then the mixture was transferred into a 100 mL Teflon-lined stainless steel hydrothermal reactor and heated at 100  C for 90 min. The as-obtained precipitate was separated under vacuum filtration and washed with distilled water three times. The as-synthesized CaCO3 powder was dried under vacuum at 120  C for 5 h. 2.3. Characterization The morphology of the synthesized CaCO3 particles was examined on a scanning electron microscope (SEM, Quanta FEG 650, Japan) with an energy dispersive X-ray spectrometer (EDX), and a high resolution transmission electron microscope (HR-TEM, JEM-2100, Japan) with an accelerating voltage of 200 kV. X-ray

3:157  I221 A I104 C

ð1Þ

þ 3:157  I221 þ 7:691  I110 A V

I104  X A

ð2Þ

3:157  IA 221

X V ¼ 1:0
X A
X C

ð3Þ

CaCO3 samples containing only vaterite and calcite were analyzed by the following set of equations: IC 104 IV 110

¼ 7:691

Xc XV

ð4Þ

X C þ X V ¼ 1:0

ð5Þ

where XA, XC, and XV are the molar fraction of aragonite, calcite and vaterite, respectively. Peak intensities of 221 plane (IA221), 110 plane (IV110) and 104 plane (IC104) represent aragonite, vaterite and calcite, respectively. FTIR was recorded on a Nexus 670 infrared spectrophotometer (America). Thermogravimetry analysis (TGA, Entzsch-Sta 449, Germany) was employed to measure the weight percentage of the CaCO3 precipitate. Nitrogen sorption data were gained on a Tristar II3020 automated gas adsorption analyzer (America). pH meter (Sartorius, PB-10, China) was employed to measure the pH value of the as-prepared solution. The composition of carbide slag was analyzed using a focused-beam X-ray fluorescence spectrometer (XRF, Model: EAGLE III, America). 3. Results and discussion 3.1. The composition of the carbide slag The chemical components of carbide slag were analyzed by the X-ray fluorescence (XRF) as shown in Table 1. 3.2. Characterizations of CO2SM The CO2SM was characterized by the XRD, FTIR, and 13C NMR technologies. XRD analysis (Fig. S1) showed that similar crystalline structures (14.72, 19.06, 22.48, 25.62, 28.48, and 29.79)  are evident in CO2SM. Subsequently, FTIR spectra (Fig. S2) suggested the CO2SM was an alkylcarbonate salt [31–33]. The peaks at 3308 cm
1 and 2175 cm
1 were attributed to N

H and

NH3+
1 groups [34,35]. Two intense absorption peaks at 1575 cm and 1483 cm
1 were associated to

CO2
groups [36]. Specially, the
1 peak at 1370 cm denoted carbonate (CO32
) rather than bicarbonate because the typical peaks of bicarbonate appeared at 1360 cm
1 and 835 cm
1 [37,38]. Moreover, the formation of

Fig. 1. Morphology control in the synthesis of CaCO3 micro-spheres by using carbide slag and CO2SM, which was prepared from the equimolar system EDA + EG absorbing CO2. A and B represent the hydrothermal reactor. In the processes, the filtered solution without CaCO3 precipitate could not only repeatedly absorb CO2, but also be recycled to produce the same crystal phase CaCO3 micro-particles after bubbling CO2.

Table 1 The composition of carbide slag. Component

CaO

SiO2

Al2O3

Fe2O3

MgO

Na2O

Others

Percentage (wt%)

80

3

1

0.6

0.2

0.2

5

B. Guo et al. / Journal of CO2 Utilization 18 (2017) 23–29

alkylcarbonate salts (

CO3
+H3N-) was confirmed by observing the characteristic alkylcarbonate peak at 164.21 ppm (Fig. S3) in the solid-state 13C NMR spectra [39,40]. The spectral results provide the information summarized in Scheme 1. In addition, TGA-DSC results (Fig. S4) indicated the CO2SM could release CO2 between 60  C and 118  C. Observably, the decomposition of CO2SM was accelerated at about 95  C and completely decomposed at about 118  C. 3.3. Effect of CO2SM concentration on crystallization of CaCO3 Preparation of CaCO3 crystals with different CO2SM concentrations was investigated and the as-prepared CaCO3 crystals were characterized by SEM, XRD, and FTIR spectral techniques. The crystallization of CaCO3 was carried out with 50 mL of carbide slag saturated limpid solution and 0.1–5 g of CO2SM via hydrothermal reaction method at 100  C for 90 min. According to SEM images in Fig. 2, CaCO3 morphologies were significantly affected with the changing CO2SM concentrations. When the CO2SM concentration was 2 g L
1, a class of flower-like clusters with irregular rod-shaped structures was obtained (Fig. 2A). As the CO2SM concentration increased to 10 g L
1, some littery morphologies of the CaCO3 precipitates were formed, which included the aggregate of rodshaped and sphere (Fig. 2B). With the CO2SM concentration further increased to 100 g L
1, uniform spheres with a size about 4 mm were formed (Fig. 2E). Fig. 3 showed that XRD and FTIR of as-prepared CaCO3 precipitates synthesized with different concentrations of CO2SM. From Fig. 3(1), all the XRD pattern peaks were consistent with a pure calcite crystal structure in sample A, mixed calcite and vaterite in sample B, and pure vaterite in samples C, D, and E. The relative percentages of each crystalline phase of CaCO3 were calculated and listed in Table 2. The results were further demonstrated by the FTIR spectra as given in Fig. 3(2). Sample A had two characteristic peaks at 875 and 711 cm
1 (y4 mode of calcite), which indicated that the pure calcite phase was formed [41]. With the increasing CO2SM concentrations, a new peak appeared at 745 cm
1 (y4 mode of vaterite), which showed the mixed phase of calcite and vaterite in samples B [42]. What’s more, the phase of calcite disappeared with the continuously increasing CO2SM concentrations, and there was only the phase of pure vaterite in samples C, D, and E. The obtained results by FTIR were in good agreement with those obtained by XRD. On the basis of the XRD and FTIR results (Fig. 3), the lower concentration of CO2SM was favored to the formation of calcite. With the increasing CO2SM concentrations, the formation of the thermodynamically most stable calcite phase was restrained and the crystalline phase of vaterite was promoted, which might be due to EG and/or EDA in the solvent mixture inducing CaCO3 crystallization to transform from a thermodynamically controlled process into a kinetically controlled one, and this transformation changed the polymorph of the as-prepared CaCO3 from calcite to vaterite, since kinetic conditions usually induce and stabilize CaCO3 crystals in the phase of vaterite [43,44]. These results suggested that CO2, EG and/or EDA concentrations from the CO2SM were indispensable and might cooperatively help CaCO3 grow along different directions, in which EDA might be used to adjust the pH value [45] and EG could be considered as a co-solvent [46,47] of the reaction system. Thus, a possible formation process of CaCO3 micro-particles is shown as follows:

Scheme 1. Formation of the CO2SM from the reaction of EDA + EG with CO2.

EG (and/or EDA) + Ca2+ ! EG (and/or EDA)-Ca2+ (complex)

25

(1)

EG (and/or EDA) + CO32
! EG (and/or EDA)-CO32
(complex) (2)

EG (and/or EDA)-Ca2+ + EG (and/or EDA)-CO32
! CaCO3 + EG (and/ or EDA) (3) 3.4. Effect of reaction temperature on crystallization of CaCO3 The effect of different reaction temperature on crystallization of CaCO3 was inspected at the CO2SM concentration of 100 g L
1 and the as-prepared CaCO3 crystals were characterized by SEM, XRD, and FTIR spectral techniques. According to SEM images in Fig. 4, reaction temperature was no important influence on crystallization of CaCO3. XRD patterns and FTIR spectra of the as-prepared samples with different reaction temperatures for 1 h in 100 g L
1 CO2SM solution were given in Fig. S5. The XRD patterns (Fig. S5(1)) showed that the polymorph kept the pure vaterite structure and did not change with the varying reaction temperatures. The result was further demonstrated by the FTIR spectra (Fig. S5(2)). All samples had two characteristic peaks at 875 and 745 cm
1 (y4 mode of vaterite), which indicated that the pure vaterite phase were formed. The polymorph of products was vaterite at all the reaction temperature. This might be caused by the kinetics of the crystallization processes [41,44], and the reaction temperature promoted the formation of vaterite [48,49]. In addition, the arrangement of Ca2+ was affected only by temperature, which also favored the crystallization of vaterite [50,51]. 3.5. Effect of reaction time on crystallization of CaCO3 Representative SEM images of as-prepared CaCO3 precipitates for different reaction times at 100 g L
1 concentration of CO2SM at reaction temperature of 100  C were presented in Fig. 5, in which the morphology of as-prepared CaCO3 had almost no change. Based on the XRD and FTIR results (Fig. S6), the polymorph of as-prepared CaCO3 precipitates were all vaterite. This phenomenon could be caused by the fast nucleation rate of products. Therefore, the extending of reaction time would only be helpful to micro-particle growth, not affect the morphology and polymorph of the as-prepared CaCO3 micro-particles. 3.6. Properties of CaCO3 micro-spheres To preferable understand the structure of CaCO3 micro-spheres and know their crystalline phase transformation and compositions, the properties of CaCO3 micro-spheres were systematically investigated. 3.6.1. HR-TEM To obtain detailed information on the end of CaCO3 microspheres, HR-TEM observations were performed (Fig. 6). As shown in Fig. 6, the lattice spacing of 3.27 Å corresponds to the (112) plane of vaterite [52]. 3.6.2. TGA The TGA curve (Fig. S7) of the as-prepared spherical-like shape CaCO3 was performed to confirm the presence of organics in the CaCO3 samples. From the result of Fig. S7, the first stage was from room temperature to 460  C with a mass loss of approximately 5.6% due to the evaporation of physically and chemically absorbed organic compounds, and the second endothermic stage was at

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B. Guo et al. / Journal of CO2 Utilization 18 (2017) 23–29

Fig. 2. SEM micrographs of CaCO3 micro-particles were acquired under different concentration of the CO2SM at 100  C for 90 min, when the concentration of CO2SM were: Sample A: 2 g L
1; Sample B: 10 g L
1; Sample C: 20 g L
1; Sample D: 60 g L
1; and Sample E: 100 g L
1.

Fig. 3. XRD patterns (1) and FTIR spectra (2) of as-obtained samples at 100  C for 90 min in different concentrations of CO2SM: (A) 2 g L
1; (B) 10 g L
1; (C) 20 g L
1; (D) 60 g L
1; and (E) 100 g L
1.

about 683  C due to the thermal decomposition of CaCO3 (CaCO3 ! CaO + CO2") [53]. Table 2 The CaCO3 samples prepared under different CO2SM concentration at 100  C for 90 min, experimental conditions, and polymorph compost for each sample. Samplesa

Preparation conditionsb

A B C D E

CO2SM CO2SM CO2SM CO2SM CO2SM

a

(2 g L
1); pH = 11.68 (10 g L
1); pH = 10.87 (20 g L
1); pH = 10.43 (60 g L
1); pH = 9.26 (100 g L
1); pH = 8.35

Polymorph compost (%)c Calcite

Aragonite

Vaterite

100 8 0 0 0

0 0 0 0 0

0 92 100 100 100

In the all case, 50 mL carbide slag saturated limpid solution was used. g L
1 of CO2SM was calculated as milligrams of CO2SM dispersed in 50 mL carbide slag saturated limpid solution, the reaction time and temperature were 90 min and 100  C, respectively. c calculated from the XRD patterns. b

3.6.3. BET measurement N2 adsorption–desorption was carried out and the isotherms were reported in Fig. S8. The CaCO3 micro-sphere sample gave a 42.77 m2/g specific surface area and the average pore size was mainly distributed at 11.45 nm. 3.6.4. EDX EDX (Fig. S9) showed that CaCO3 particles contained three major elements, including carbon, calcium, and oxygen. 3.6.5. FTIR of as-prepared CaCO3 micro-sphere As shown in Fig. S10, the non-symmetrical and symmetrical stretching vibrations of C

H (–CH2–) [54] in EDA and/or EG at 2925 and 2859 cm
1 indicate that the as-prepared products

B. Guo et al. / Journal of CO2 Utilization 18 (2017) 23–29

27

Fig. 4. SEM images of CaCO3 micro-spheres were acquired under different temperature for 90 min. When the concentration of CO2SM was 100 g L
1, the reaction temperature were: Sample A: 90  C; Sample B: 100  C; Sample C: 110  C; Sample D: 120  C; and Sample E: 130  C.

Fig. 5. SEM images of CaCO3 micro-spheres were acquired for different reaction time at 100  C. When the concentration of CO2SM was 100 g L
1, the reaction time were: Sample A: 60 min; Sample B: 90 min; Sample C: 120 min; Sample D: 150 min; and Sample E: 180 min.

contained not only CaCO3 crystals but also organic molecules including EDA and/or EG. 3.7. Circular preparation of CaCO3 micro-particles

Fig. 6. HR-TEM of as-obtained CaCO3 micro-sphere samples.

After forming the CaCO3 precipitate at the 100 g L
1 CO2SM concentration for 90 min at 100  C, the filtrate containing EDA and EG could be reused to absorb CO2, which was released from the steel cylinder. After the absorption of CO2, an appropriate amount carbide slag was added into the solution to prepare CaCO3 microparticles by hydrothermal reaction method. And then, the filtrate containing EDA and EG were additionally reused. As a result, the same morphology and polymorph CaCO3 microparticles were smoothly produced at 100  C within 90 min after five-successive absorption-preparation cycles. Each sample was

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B. Guo et al. / Journal of CO2 Utilization 18 (2017) 23–29

Fig. 7. (1) and (2) represent the SEM images of as-prepared CaCO3 at the first time and the last time in the process of cycle preparation CaCO3 micro-particles; (3) represents FTIR spectra of cycle preparation CaCO3 micro-particles with five cycles, and A–E represent the experimental number.

characterized by SEM and FTIR spectral techniques (Fig. 7), which showed that all CaCO3 micro-particles had the same morphology of spheres and crystal phase of vaterite. The mass of the CaCO3 crystals prepared from each cycle was respectively 0.6126 g, 0.6014 g, 0.5749 g, 0.5336 g, and 0.4957 g. The preparation efficiency of CaCO3 after the five successive cycles was 80.92%. Thus, the filtered solution without the CaCO3 precipitate could not only be repeatedly used to absorb CO2, but also used to produce the same morphology and crystal phase CaCO3 micro-particles after the bubbling of CO2. 4. Conclusion This paper provided a novel synthesis approach of vaterite CaCO3 micro-spheres by carbide slag and CO2SM through a hydrothermal reaction method, in which the released EDA and EG from CO2SM played an important role in controlling the morphology and polymorph of the CaCO3 micro-particles. Additionally, the filtered solution without CaCO3 precipitates could not only be reused to absorb CO2, but also used to produce the same crystal phase CaCO3 micro-particles repeatedly after the bubbling of CO2. Acknowledgements This work was supported by the National Natural Science Foundation of China (21666027), Program for New Century Excellent Talents in University (NCET-12-1017), the Natural Science Foundation of Inner Mongolia Autonomous Region (2016JQ02), the Program for Grassland Excellent Talents of Inner Mongolia Autonomous Region, the Inner Mongolia Science and Technology Key Projects, Key Laboratory of Coal-based CO2 Capture and Geological Storage (Jiangsu Province, China University of Mining and Technology, 2016A06), and training plan of academic backbone in youth of Inner Mongolia University of Technology. Appendix A. Supplementary data Supplementary data associated with this article can be found, in the online version, at http://dx.doi.org/10.1016/j.jcou.2017.01.004. References [1] Q. Wang, J. Luo, Z. Zhong, A. Borgna, CO2 capture by solid adsorbents and their applications: current status and new trends, Energy Environ. Sci. 4 (2011) 42– 55. [2] A. Goeppert, M. Czaun, G.K.S. Prakash, G.A. Olah, Air as the renewable carbon source of the future: an overview of CO2 capture from the atmosphere, Energy Environ. Sci. 5 (2012) 7833–7853.

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