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Front. Environ. Sci. Eng.    2023, Vol. 17 Issue (12) : 149    https://doi.org/10.1007/s11783-023-1749-2
REVIEW ARTICLE
Research progress on synthesis of zeolites from coal fly ash and environmental applications
Xingyue Chen1, Peng Zhang1(), Yang Wang1, Wei Peng1, Zhifeng Ren1, Yihong Li1, Baoshuai Chu1, Qiang Zhu2
1. College of Materials Science and Engineering, Taiyuan University of Science and Technology, Taiyuan 030024, China
2. Australia Institute for Innovative Materials, University of Wollongong, Wollongong, NSW2500, Australia
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Abstract

● Up-to-date information on the preparation of zeolite from CFA were summarized.

● The applications of CFA zeolites in environmental protection field were reviewed.

● The feasibility analysis of industrial production of CFA zeolites were discussed.

The by-product of coal combustion, coal fly ash (CFA), has become one of the world’s most emitted solid wastes, and bulk utilization while achieving high value-added products is the focus of current research. Using CFA to prepare zeolite cannot only reduce environmental pressure, but also obtain high value-added products, which has a good market prospect. In this paper, the research progress of hydrothermal synthesis method of CFA zeolites is reviewed in detail and summarized several other synthetic methods of CFA zeolites. This review also presents an overview of CFA zeolites application in environmental applications like water treatment, gas adsorption and soil remediation. However, a considerable number of literature data have documented using CFA zeolites for water treatment, whereas research on CFA zeolites application to gas adsorption and soil remediation is still limited. In addition, the current status of basic research on the industrial production of CFA zeolites is briefly summarized, and the development trend of the synthetic zeolite of CFA is prospected. After the feasibility analysis of the industrial production of CFA zeolite, it is concluded that the only two methods with high feasibility for industrial application are two-step hydrothermal and alkali melting methods, and the industrial production technology still needs to be studied in depth.
Keywords Coal fly ash      Zeolite      Synthetic method      Environmental application      Industrialization     
Corresponding Author(s): Peng Zhang   
Issue Date: 24 July 2023
 Cite this article:   
Xingyue Chen,Peng Zhang,Yang Wang, et al. Research progress on synthesis of zeolites from coal fly ash and environmental applications[J]. Front. Environ. Sci. Eng., 2023, 17(12): 149.
 URL:  
https://academic.hep.com.cn/fese/EN/10.1007/s11783-023-1749-2
https://academic.hep.com.cn/fese/EN/Y2023/V17/I12/149
Fig.1  Production and comprehensive utilization of CFA in China from 2015 to 2020.
Fig.2  The characterization results of CFA, (A−C) the SEM images, (D) The cluster map showing distinction of phases considering major and minor elements, (E) XRD patterns of FBC and PCC-fly ashes, and EDS elemental maps of CFA (Yao et al., 2015; Mohebbi et al., 2022; Chindaprasirt et al., 2011).
Composition (wt.%) Bituminous Subbituminous Lignite Anthracite
SiO2 20−60 40−60 15−45 28−57
Al2O3 5−35 20−30 10−25 18−36
Fe2O3 10−40 4−10 4−15 3−16
CaO 1−12 5−30 15−40 1−27
MgO 0−5 1−6 3−10 1−4
Na2O 0−4 0−2 0−6 0−1
K2O 0−3 0−4 0−4 0−4
P2O5 0−4 0−2 0−10 0−5
LOI 0−15 0−3 0−5 1−8
Tab.1  Chemical compositions of CFA obtained from different coals (Ahmaruzzaman, 2010; Sahoo et al., 2016)
Fig.3  Schematic illustration of one-step method, two-step method and alkali melting method synthesis of zeolites from CFA.
Fig.4  (A, B) X-ray diffraction intensities of the zeolite P synthesized in various alkali; (C) Proposed reaction mechanism for zeolite synthesis; (D) SEM images of CFA and the products obtained in various synthesis parameters (Murayama et al., 2002).
Method Zeolite Hydrothermal conditions Ref. Remarks
NaOH orNaOH/CFA Solid/liquid(g/cm3) or Si/Al T (°C) t (h)
One-step method Na-P1 2 mol/L 1/4 120 3−24 Murayama et al. (2002) NaOH, Na2CO3 and KOH
Na-X 2−13 − 90−100 8−48 Mondragon et al. (1990) Na-P1
Blend 2.5−3.5 0.88−1.10 159 3.8 Moriyama et al. (2005) Na-A, Na-G
Na-P1 2.8−5.0 0.28−0.5 25 48 Ma et al. (1998) −
Na-P1 2 mol/L − 90−150 12 Steenbruggen & Hollman (1998) −
K-CHA 3 mol/L − 160 3 Murayama et al. (2008) KOH
Na-P1 2 mol/L 150 24 Querol et al. (2001) SOD, TOB
Na-P1 2/3.5 mol/L 1/4−1/8 100 24 Inada et al. (2005) −
Two-step method Na-P1 2 mol/L 2.0 90 48 Hollman et al. (1999) −
Na-X 2 mol/L 1.8 90 48 −
Na-A 2 mol/L 1.2 90 67 SOD
Na-P1 3 mol/L 2/9 80 36 Wdowin et al. (2014) −
Na-P1 3 mol/L 2/9 80 26 Kunecki et al. (2018) −
Na-P1 2 mol/L 1.5/9 95 24 Xie et al. (2013) Na-A
Na-P1 1 mol/L 1/10 150 60 Kumar et al. (2022) −
SOD 5 mol/L 1/10 150 20 −
Analcime 3 mol/L 1/10 150 20 −
Na-A 2 mol/L Si/Al=1 90−95 1.5−2.5 Iqbal et al. (2019) Aging time: 12 h
Na-A 4 mol/L Si/Al=1.93 100 4 Amoni et al. (2022) −
Na-A 2 mol/L − 90 1.5 Hui et al. (2008) Second reaction T: 95 °C 2.5 h
Na-A − Si/Al=0.9 85 24 Tanaka et al. (2004) SiO2/Al2O3≥1.7, Na-X
MOR − Si/Al=3.92 150 24 Zhou et al. (2021) −
MFI − Si/Al=5.8 160 72 Missengue et al. (2017) Structure-directing agent: TPABr
Na-A 2.2 mol/L Si/Al=0.5 85 24 Tanaka et al. (2009) Trace amount of sod
Na-A 2.2 mol/L Si/Al=1.0 85 24 Single phase
Na-X 2.2 mol/L Si/Al=4.5 85 24 2≤SiO2/Al2O3＜4.5, Blend
Na-P1 3 mol/L Si/Al=1.43 105 24 Derkowski et al. (2006) −
SOD 5 mol/L Si/Al=1.21 105 24 Add: 3 mol/L NaCl
Na-X 3 mol/L Si/Al=1.1 75 24 -
NaA-X Na2O/SiO2=1.4 Si/Al=2.1 90 8 El-Naggar et al. (2008) Ageing T: 24 h
Alkali melting method (Fusion: 550−600 °C for 1−2 h) Na-X 1.2 1/10 90 7 Verrecchia et al. (2020) NaOH/CFA>1.2, SOD
Na-Y 0.9 Si/Al=4, 5 90 12 Ren et al. (2020) Ageing for 24 h at 55 °C
Na-X 1.0−1.2 Si/Al<5 90 6 Molina & Poole (2004) −
Na-X − 1.6−2.4 90 4−8 Boycheva et al. (2021) −
Na-A 1.5 Si/Al=1 100 24 Hong et al. (2017) −
Na-X 1.2 Si/Al=1.78 90 15 Zhang et al. (2017) −
SOD 1.0 Si/Al=1.25 105 24 He et al. (2016) −
Na-X 0.5 Si/Al=2.25 90 2 Kalvachev et al. (2016) 60% conversion
Na-A 0.33 Si/Al=1.22 100 24 He et al. (2020) With addition 3% HCl
Na-P1 2 mol/L Si/l=2.01 100 13 Ye et al. (2008) Fusion: 830 °C, 1 h
Na-A 2 mol/L Si/l=0.91 100 5 10% Na-A seed
Na-X 2 mol/L Si/l=0.91 100 5 2 vol.% directing agents
Na-A 2−1.2 Si/Al=1.6 100 12 Fotovat et al. (2009) Si/Al=3, FAU
Na-X N.A. - 35−60 48 Belviso et al. (2010) ZK-5, using sea water
Na-P1 0.2 mol/L Si/Al=2.0 120 4 Kazemian et al. (2010) −
Na-X 1.2 Si/Al=1.0−1.2 100 24 Izidoro et al. (2013) −
Na-A 1.2 − 100 7 −
Na-X 1.25 −2 80−100 5−10 Sivalingam et al. (2018) NaOH/CFA=1.0, Na-Y
CZC 2 − 750 1 (N2) Zhao et al. (2022) Carbon-zeolite composite (CZC)
Tab.2  Zeolite synthesized by conventional hydrothermal method from CFA
Method Zeolite Hydrothermal conditions Ref. Remarks
NaOH orNaOH /CFA Solid/liquid(g/cm3) or Si/Al Heating Time
Microwave-assisted hydrothermal conversion Na-A 1 Si/Al =1 100–300 W 10–30 min Behin et al. (2014) Crystallinity [%]: 67.24
Na-P1 2 mol/L − 500 W 15 min Inada et al. (2005) −
Phillipsite 2 mol/L − 2.45 GHz Less 2 h Fukui et al. (2007) Rice husk ash as a silica source
K-MER 4 mol/L Si/Al =7 1000 W 5 min Chen et al. (2021) Ultrasound frequency was 25 kHz
Phillipsite KOH 1.5 mol/L − 2.45?GHz 2–32 h Fukasawa et al. (2018) KCl and K2CO3
Seed-assisted method ZSM-5 − 30 90 72 h Zhang et al. (2020) Seeds was 3 wt% to Si
FAZ-A 2 mol/L 1–1.1 90–105 °C 3 h Rayalu et al. (2001) Zeolite-A was added as seed
MRE 0.125 − 150 7 d Ma et al. (2022) Yield (%): 73
SFE 0.125 − 150 7 d Yield (%): 71
MWW 0.125 − 150 4 d Yield (%): 90
MFI 0.125 − 150 5 d Yield (%): 88
IWV 0.125 − 150 7 d Yield (%): 89
TON 0.3 − 150 4 d Yield (%): 45
ERI 0.3 − 150 6 d Yield (%): 44
EUO 0.3 − 150 7 d Yield (%): 53
Molten-salt method Cancrinite Sodalite − − 350 12 h Choi et al. (2001) NaOH-NaNO3
Cancrinite Sodalite Na-P 3 mol/L − 350±5 24 h Park et al. (2000) NaOH-NaNO3 (KNO3)
Cancrinite Sodalite Na2CO3/CFA=0.5:1 NaCl/CFA=0.3:1 790−950 5−10 h Yao et al. (2011) Na2CO3, NaCl
Ultrasound-assisted hydrothermal conversion Na-A Sodalite 1−2 h = 60 °C; 3 h = 65 °C and 4 h = 75 °C − (240 W; 35 kHz) 4 h Belviso (2018) −
Na-A − 4 80−94 6 h Hums et al. (2016) (Fusion: 550−600 °C for 1−2 h)
Na-A 2.4 mol/L − 100 2 h Ojumu et al. (2016)
ZSM-5 − − 24 kHz 95−145 h Chen et al. (2020) Irradiation powers (97, 194, 323 W)
Supercritical hydrothermal method Sodalite Cancrinite 8 mol/L 2–4 mol/L 15:1 400 5 min Wang et al. (2015) −
Cancrinite 5:1 2.5:1 400 5 min Zhao et al. (2016) Na2CO3 as activator
Tab.3  Zeolite synthesized by new composite hydrothermal method from CFA
Fig.5  (A) Relationships between the ratio of XRD peak intensities and treatment time for microwave and oil-bath heating; (B) Schematic representations of the temperature distributions around CFA and zeolite (Fukasawa et al., 2018).
Fig.6  (A, C, D) XRD patterns, FT-IR spectra, SEM images and particle size distributions of the products obtained different ultrasonic irradiation powers; (B) Variation of Si/Al, amount of TPA+, and relative crystallinity with synthesis time under w/o ultrasonication (■) and 323 W ultrasonic (●) systems (Chen et al., 2020).
Method Advantage Disadvantage Advise
One-step method Simple synthetic procedure The more side reactions, long hydrothermal time, and lower purity Selecting high activity CFA as raw materials and produce products with low purity requirements
Two-step method High conversion and crystallinity Technological complexity, high cost and The reaction conditions are difficult to control Develop a more cost-effective and simplified protocol for the second step, while maintaining high conversion and crystallinity
Alkali melting method High yield and purity Procedures trival, and high energy consumption It is currently the most promising solution to achieve industrial production, further studying the synthesis mechanism of zeolite, and improving conversion rate and crystallinity
Microwave-assisted method Fast reaction rate and low energy consumption More by product is produced and lower purity Optimize reaction parameters to minimize byproduct formation and improve purification methods to increase purity
Seed-assisted method Simple synthetic procedure and fast reaction rate Technological complexity and lower purity Simplify the procedure and improve purification methods to increase yield and purity
Molten-salt method Avoids the use of water solvents High temperature, high salt dosages and impurity substance Explore ways to reduce salt dosages and improve purification methods to increase product purity
Ultrasound-assisted method Shortening reaction time, and reducing reaction temperature Complicated infrastructure, high costs Develop more cost-effective infrastructure and adjust parameters to maximize efficiency and reduce costs
Supercritical hydrothermal method Very fast reaction rate and high crystallinity The reaction mechanism is complex and high cost Further investigate the mechanism of the reaction to optimize conditions and develop more cost-effective ways to run the process
Solvent-free method High yield, better utilization of autoclaves, and reduction of pollutants The raw material pretreatment process is complex, and lower purity Streamline raw material pretreatment and develop more efficient purification methods to increase product purity
Dialysis hydrothermal The relative crystallinity and purity of the product are both high Dialysis requires a long reaction period, and the solution cannot be recovered Investigate new materials for dialysis membranes to reduce reaction time and improve solution recovery
Gradual heating method Relatively high crystallinity and high purity Conversion rate and utilization rate of fly ash are both low Develop new catalysts or additives to increase fly ash utilization rate and improve conversion efficiency
Tab.4  Characteristics of zeolites synthesized by different methods from CFA
Ionic species Zeolite CEC (meq/100 g) η (%) qe (mg/g) Operating conditions Ref.
pH T (°C) t (min) Ci (mg/L) Dosage (g/mL)
Cr3+ SOD, Na-P1 − 75.5 − 3.4 20 240 − 400 Wu et al. (2008)
Na-A 105 100 − − − 24 h − 0.2 Koukouzas et al. (2010)
Phillipsite − 100 − 1.55 20 60 1000 0.02 Itskos et al. (2015)
Thomsonite − 98 − 1.55 20 60 1000 0.02 Itskos et al. (2015)
Na-A − 87.3 35.6 3 25 240 200 0.005 Hui et al. (2005)
ZSM-18 120 100 − − − 24 h − 0.02 Koukouzas et al. (2010)
Cu2+ Na-A 500 99.7 − 3 25 240 200 0.5 Wang et al. (2009)
FAU − 100 39.7 − 25 90 100 5 Joseph et al. (2020)
FAA-CS − 71 119.1 10.2 − 120 350 0.002 Visa & Chelaru (2014)
Zn2+ Na-A 560 93.2 29.7 3 25 240 200 0.5 Wang et al. (2009)
FAU − 100 34.7 25 90 100 5 Joseph et al. (2020)
Phillipsite − 95 − 1.55 20 60 1000 0.02 Itskos et al. (2015)
Thomsonite − 60 − 1.55 20 60 1000 0.02 Itskos et al. (2015)
Na-A 500 − 22.4 3 25 240 200 − Wang et al. (2009)
Na-P1 290 80.8 − 303 − 30 0.13 0.01 Cardoso et al. (2015)
Ni2+ Na-A 105 99.9 − − − 24 h − 0.2 Koukouzas et al. (2010)
Na-A − 94 47 − 25 180 100 2 He et al. (2020)
Na-X 270.4 91 15.9 5 30 30 100 1 Zhang et al. (2018)
Na-P1 228.7 48.3 − 4.6 − − 0.52 0.08 Prasad et al. (2011)
Pb2+ FAU − 100 40 − 25 90 100 5 Joseph et al. (2020)
Na-A − 99.9 − 5.8 25 12 h 50 − Zhu et al. (2018)
CZC − − 185.68 7 − 40 − 0.1 Zhao et al. (2022)
Phillipsite − − 48 1.55 20 60 1000 0.02 Itskos et al. (2015)
Cd2+ FAU 100 40.3 25 90 100 5 Joseph et al. (2020)
FAA-CS − 60 156.2 10.2 − 120 515 0.002 Visa et al. (2014)
Na-P1 290 94.1 − 3.3 − 30 0.22 0.01 Cardoso et al. (2015)
As5+ Na-X − 83 27.8 2.14 25 240 − 0.1 Yang et al. (2019)
Na-P1 290 100 − 3.3 − 30 0.04 0.01 Cardoso et al. (2015)
Tab.5  Heavy metal ions uptake characteristics of CFA zeolites
Fig.7  Microstructure of hierarchical morphology NaX-type zeolite made from CFA (Muriithia et al., 2020).
Exhaust gas Zeolite Sorptioncapacity BET(m2/g) Conditions Ref. Remarks
CO2 Na-A About 100% 257 Flow rate of 20 mL/min; Degassed 200 °C for 1 h (He); Adsorption t: 4 h Muriithi et al. (2020) –
Zeolite A – 145 Pretreatment: 1 h at 350 °C; Adsorption: 25 °C; Desorption: 130 °C Soe et al. (2016) Comparable to commercial zeolite A and 13X
MOR zeolite 1.92 mmol/g 266.49 Flow rate of 50 mL/min; Degassed 200 °C for 1 h (N2); Sample: 12 mg Zhou et al. (2021) –
Na-Ca-X 3.16 mmol/g 486 0.40 g sample and 3 vol% CO2 from the CO2/N2 mixture at a flow rate of 30 mL/min Boycheva et al. (2021) CO2 adsorption in dynamic conditions
Zeolite X 60 mg/g – Pretreatment: 320 °C in Ar flow at rate of 5 °C/min; Sample: 12 mg;Adsorption: 22 °C Kalvachev et al. (2016) CO2 sorption capacity about 3 times lower than commercial zeolite
Zeolite A 2.8 mmol/g 486 0.40 g sample of 20−80 mesh and 10% CO2/N2 at a flow rate of 30 mL/min Popova et al. (2019) CO2 adsorption in dynamic conditions
Zeolite 4A-X 74 mg/g – Activation T: 200 °C; Adsorption T: −78 °C Querol et al. (2002) –
SO2 Zeolite Y 46 mg/g 102.4 Pretreatment conducted at 200 °C under N2 flow of 100 mL/min for 2 h Pedrolo et al. (2017) K+ as the “structure builder”
Zeolite 4A-X 297 mg/g – Activation T: 400 °C; Adsorption T: 25 °C Querol et al. (2002) Activation and adsorption T: 200/–10 ?°C; 22 mg/g
NH3 Zeolite 4A-X 111 mg/g – Activation T: 200 °C; Adsorption T: −23 °C Querol et al. (2002) Activation and adsorption T: 400/25 ?°C; 72 mg/g
NO SSZ-13 zeolites Nearly 100% 630 The feed gas containing 500 ppm NO, 500 ppm NH3, 5% O2, T: 100−700 °C Wang et al. (2021) Ion exchange with Cu
MOR zeolite 93.58 % 122.89 The feed gas contained 400 ppm NO, 440 ppm NH3, 5% O2, T: 200 °C Zhou et al. (2021) Modifed with Mn
Acetone adsorption Zeolite Y 134.0 mg/g 386.9 A sample (0.18 g, 40–60 meshes) was used and the total flow rate was 500 mL/min Ren et al. (2020) Exhibits cyclic adsorption stability
Toluene Zeolite X 525.03 μg/g 990.3 Pretreatment: 2 h 250 °CAdsorption temperature: 50−170 °C Zhu et al. (2019) Zeolite X had better adsorption performance than commercial, activated carbon
o-Xylene 545.26 μg/g
m-Xylene 563.82 μg/g
p-Xylene 582.91 μg/g
Cyclohexane 117 mg/g
Tab.6  CFA zeolites adsorbents for exhaust gas removal
Fig.8  The advantages and limitations of CFA zeolite in soil remediation.
Zeolite Pollution Type of soil Type of experiment Effect Ref.
Natural zeolite Cd, Pb, As, W Vegetable field Laboratory experiment The combination agent was a mixture of zeolite and biochar with a weight ratio of 1:1 Zheng et al. (2020)
Clinoptilolite Ni Wheat field Plot experiment Biochar and zeolite Shahbaz et al. (2021)
Faujasite Cu, Pb, Zn, Cd Including wastewater Plot experiment The zeolites were regenerated by NaCl solution (1 mol/L) Ji et al. (2017)
Zeolite from fly ash Cd Paddy soil Plot experiment Addition of natural zeolite strongly increased the soil pH, reduced the adsorption and transport of Cd in rice organs, as well as enhanced the rice growth and yield Zhao et al. (2020)
Zeolite from fly ash Cu Loamy sand Plot experiment Application of zeolite had a significant effect on soil properties; zeolite reduced the content of total nitrogen and widened the C:N ratio Wyszkowski (2019)
Natural zeolite added in amounted to 3.0% of the soil mass Cr, Zn, Pb, Cu, Ni Light loamy sand, Ni-contaminated soil Plot experiment Natural zeolite significantly reduced the average content of chromium Radziemska & Mazur (2016)
Zeolite X, P, and A Cu, Cd Soil samples were artificially Laboratory experiment Zeolite X and zeolite P for the Cu-contaminated soils, and zeolite X and zeolite A for the Cd-contaminated samples Terzano et al. (2007)
Zeolite from fly ash Cd, Pb, Zn Loamy sand Plot experiment Zeolite used individually as well as in a mixture with biochar effectively immobilized pollutants Mierzwa-Hersztek et al. (2019)
Tab.7  Effect of zeolite amendments on soil remediation
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