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. 2024 Aug 21;40(37):19324–19331. doi: 10.1021/acs.langmuir.4c00801

Correlation between Na–Cs Ion Exchange Properties in the Alkaline Form and Acid Strength in the Proton Form of Zeolite

Naonobu Katada †,*, Hayato Tamura ‡, Takuya Matsuda †, Yuya Kawatani †, Yu Moriwaki †, Manami Matsuo †, Ryota Kato †
PMCID: PMC11411716  PMID: 39167672

Abstract

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The ion exchange function of zeolite is useful for such a purpose as the removal of radioactive Cs species from water. In the very early days of zeolite science, the affinity of zeolites for metal cations was explained based on geometry. After the explanation presented above was proposed, many new zeolites and related materials were discovered or synthesized. Furthermore, it has become clear that the chemical nature of the ion exchange sites is strongly dependent on the framework topology. In this study, the ion exchange behavior between Na-form zeolites with different framework topologies and Cs-containing aqueous solutions was analyzed, and the equilibrium constant was calculated based on the Langmuir type equation to investigate the influence of the chemical nature of the zeolite framework on ion selectivity. The equilibrium constants at room temperature were in the order FAU < LTA < MFI < YFI < MOR. This order is the same as the order of Bro̷nsted acid strengths in the corresponding proton form zeolites. It is suggested that the delocalization of charge around the ion exchange site stabilizes a large cation whose charge is delocalized. In contrast, the equilibrium constant was not related to the pore and cavity size. This opens new insight into the influence of the chemical nature of zeolite on the affinity to cation.

Introduction

Separation of Cs+ from aqueous solutions containing Na+ is necessary for the removal of radioactive Cs species in effluents from nuclear facilities1−36 and for the recovery of Cs as a resource from seawater.37−40 Na-form zeotypes (zeolites and related materials with zeolitic frameworks) have been utilized in many studies for the separation of Cs+ as ion exchangers or promoters.5−7,9,10,13,14,17,19,20,22,23,26,29,30,35,36,41,42 Leaching of Cs+ from zeolites has also been investigated for the purpose of immobilizing radioactive Cs species.41,43−48

Zeolites are a group of crystalline materials that have a three-dimensional framework consisting of Si–O covalent bonds and micropores resulting from the framework structure, and some of the Si atoms in the framework are replaced with Al atoms. Various types of framework topologies have been discovered and categorized by three-letter framework type codes (FTCs).49 On the other hand, replacing Si with an oxidation number of +4 with Al with an oxidation number of +3 creates a negative charge that is shared by the Al and the four surrounding O atoms, or the AlO4 unit. In most cases, zeolites are synthesized in basic media containing alkaline cations where one cation is weakly bound to the AlO4 unit. Cations can be exchanged in a variety of media, usually aqueous solutions, and this is the origin of the ion exchange function of zeolite.50

The behavior of ion exchange between Na+ and Cs+ on zeolites is classified as Langmuir type,19,31,51 if it is based on the simplifying assumption that the thermodynamic properties of the ion exchange sites are homogeneous. The ion exchange between Na form zeolite and Cs-containing solution can be depicted as 1

graphic file with name la4c00801_m001.jpg 1

where the equilibrium constant K is shown by 2.

graphic file with name la4c00801_m002.jpg 2

where cJ(aq) and cJ(Z) denote the molarity of chemical species J in the aqueous solution normalized by the volume of the solution and the molarity of species J in the zeolite normalized by the weight of the zeolite, respectively. The symbol Inline graphic indicates the molar concentration under standard conditions (1 kmol m–3).

Ion exchange capacity cIES(Z) and equilibrium constant K characterize the ion exchange properties of a particular zeolite. The ion exchange capacity cIES(Z) = cNa+(Z) + cCs+(Z), i.e., the concentration of exchangeable cations per unit weight of the zeolite, depends primarily on the Al content (cAl(Z)) but can be influenced by structural properties such as steric hindrance. The equilibrium constant K should reflect the chemical nature of the zeolite.

Affinities to Na+ and Cs+, reflected by the above parameters, are different among zeolites with different compositions and framework topologies. It is known that, among zeolites with a relatively high aluminum concentration, A-type zeolite with LTA framework topology has a high Cs+ removal efficiency,6,8,19 and among zeolites with a moderate Al concentration, mordenite with MOR framework topology has a high Cs+ removal efficiency.17,20 In the very early days of zeolite science, around the 1960s, the affinity of zeolites for metal cations was explained based on geometry, that is, the fitting of the cations to the zeolite cavities.50,52,53 Differences in the affinity for Na+ and Cs+ between different zeolite species are mainly explained by the sizes of cations and micropores.23,42,54 In other words, the influences of geometry on the differences in the affinity for Na+ and Cs+, i.e., selectivity in the ion exchange, have been discussed, but the influence of a chemical nature such as acid strength of the zeolite has not been studied.

After the above explanation was proposed, many types of zeotypes with different framework topologies and chemical compositions were discovered or synthesized. Furthermore, over the past three decades, it has become clear that the chemical nature of the ion exchange sites is strongly dependent on the framework topology, as indicated by the striking differences in the Bro̷nsted acid strengths of the H-form.55,56 It is speculated that the acid strength of H-form zeolite depends on the local geometry, such as the Al–O–Si angle and Al–O distance,57 and we propose that compression of the Al–OH–Si group from both ends enhances the Bro̷nsted acidity of the proton.58−60 It is considered necessary to reflect these new findings in the interpretation of the ion exchange properties of the zeolites.

In this study, we analyze the influence of the chemical properties of ion exchange sites on Na–Cs exchange. The equilibrium constant K was analyzed based on the Langmuir model and compared with the Bro̷nsted acid strength of H-form zeolite with the same framework topology.

Experimental Section

The Na-form zeolites shown in Table 1 were used as parent samples. All of them did not contain binders. They are named as shown in Table 1. For example, FAU 6.1 is a zeolite with FAU framework topology and 6.1 mol kg–1 Al. The structural properties were analyzed as follows: Powder X-ray diffraction (XRD) was recorded using an Ultima IV diffractometer (Rigaku) with a Cu Kα X-ray source operated at a voltage of 40 kV and a current of 40 mA, and the reference XRD patterns were obtained from the International Zeolite Association (IZA) Structure Database.49 The nitrogen adsorption capacity at 77 K was measured using a BEL-Sorp Max (Microtrac BEL) or a BEL-Sorp Mini (Microtrac BEL) after pretreatment at 573 K in a vacuum. The micropore volume and external surface area were estimated from the t-plot method.61 In addition, the micropore volume was estimated also from the amount of liquid nitrogen that filled the micropores when the capillary condensation was completed at p/p0 = 0.005 (p and p0 are the observed pressure and equilibrium vapor pressure at 77 K, respectively, of nitrogen).62

Table 1. Origin, Chemical Composition of Employed Zeolite Samples and Measured Ion Exchange Parameters.

sample name origin framework type Si/Al molar ratio cAl(z) (mol kg–1) cIEZ(z) (mol kg–1) K
FAU 6.1 Na-X type zeolite, Reference Catalyst JRC-Z-NaX2.5(1) supplied by Reference Committee, Catalysis Society of Japan65 FAU 1.37 6.08 0.55 3.41
LTA 6.7 Na-A type zeolite, Zeolum A-4, powder, > 100 mesh, purchased from Tosoh Corp. LTA 1.12 6.69 0.18 20.4
MFI 1.2 Na-ZSM-5 type zeolite, International Reference Zeolite IRZ-MFI002 (NH4-MFI, supplied by Catalysis Commission, International Zeolite Association66), ion-exchanged with excess of NaNO3. MFI 12.3 1.22 1.00 50.9
YFI 1.3 Na-YNU-5 type zeolite, synthesized according to literature,79 and ion-exchanged with excess of NaNO3. YFI 11.1 1.33 0.83 73.1
MOR 1.5 Na-mordenite, HSZ-642NAA supplied by Tosoh Corp. MOR 9.88 1.48 1.44 177
MOR 1.7 Na-mordenite, Reference Catalyst JRC-Z-M15(1) supplied by Reference Committee, Catalysis Society of Japan65 MOR 8.37 1.71 1.59 187
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Ion exchange between Na form zeolite and Cs-containing solution was examined as follows. An aqueous solution containing 60–360 g m–3 of Cs and 1000 g m–3 of Na was prepared from ion-exchanged water, cesium nitrate, and sodium nitrate (FUJIFILM Wako Pure Chemicals, Inc.). At room temperature, about 298 K, Na-form zeolite powder (0.1 g) was added to the solution (100 cm3), stirred for 5 min with a magnetic stirrer at about 400 rpm in a conical flask (inner volume 300 cm3), and filtered with a filter paper (No. 101, Advantec, retention particle size 5 μm). The Cs content of the solution was analyzed by an inductively coupled plasma (ICP) optical emission spectrometer (Agilent 5110). In some cases, the Cs content of the solid was confirmed by ICP analysis after dissolving the solid using hydrofluoric acid.

The analysis was performed from the measured relationship between the Cs content in the zeolite and the solution after ion exchange (Figure S1) as follows. The ion exchange between Na zeolite and a Cs-containing solution can be expressed as 2 where the equilibrium constant is shown by 2. It is assumed that the ion exchange site is covered by Na+ or Cs+. Therefore,

graphic file with name la4c00801_m004.jpg

where cIES(Z) denotes the concentration of ion exchange sites responsible for the ion exchange reaction under discussion. Since the substitution of one Si atom (oxidation number +4) by one Al atom (oxidation number +3) in the zeolite framework generates one ion exchange site for charge compensation, the number of ion exchange sites should be equal to cAl(Z), but some ion exchange sites may not be responsible due to steric hindrance or other reasons. Therefore, only functional exchange sites are considered, and in the following analysis, cIES(Z) is used.

From these, 3 is derived.

graphic file with name la4c00801_m005.jpg 3

Equation 3 shows that Inline graphic is a linear function of cCs+(aq), when measured with varying the Cs+/zeolite ratio and maintaining cNa+(aq) a constant and high value on one zeolite. Therefore, cIES(Z) and K were determined from the slope and intercept of the plot of Inline graphic against cCs+(aq). From K, the standard Gibbs energy Inline graphic of reaction 1 was calculated by 4.

graphic file with name la4c00801_m009.jpg 4

where R = 8.3145 J K–1 mol–1 and T was the temperature (298 K).

Results and Discussion

Quality of Parent Zeolite

XRD measurements of the parent samples showed diffraction patterns consistent with those simulated based on the corresponding crystal types (Figure 1).49 Nitrogen adsorption on FAU, MFI, YFI, and MOR type samples at 77 K showed isotherms classified as type I (Figure 2).63 The micropore volumes are estimated from the t-plot method61 and also from the micropore condensation capacity.62 The values estimated by the two methods are similar and are higher than 0.14 cm3 g–1 for the parent samples of FAU, MFI, YFI, and MOR types (Table 2). These observations demonstrate high crystallinity. In addition, MFI 1.2 is an International Reference Zeolite supplied by IZA (IRZ-MFI002). FAU 6.1 and MOR 1.7 are Reference catalysts from the Catalysis Society of Japan [JRC-Z-NaX2.5 (1) and JRC-Z-M15 (1), respectively]. The physicochemical properties of these samples analyzed by multiple research groups have been opened public.64−66 On the other hand, LTA 6.7 (Na-A zeolite) showed a quite low nitrogen adsorption capacity at 77 K due to the blocking of the pore opening by Na+ cation.67−69 This is characteristic of the LTA-type zeolite. These results confirm the high crystallinity of the parent zeolites.

Figure 1.

Figure 1

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X-ray diffraction of parent (Na-form) zeolites. The sample name should be referred to Table 1. Simulated patterns were obtained from the International Zeolite Association (IZA) structure database.49

Figure 2.

Figure 2

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Nitrogen adsorption isotherms at 77 K of parent (Na-form) zeolites. Solid and dotted lines show the adsorption and desorption branches, respectively. p and p0 represent the observed pressure and equilibrium vapor pressure at 77 K, respectively, of nitrogen.

Table 2. Textural Properties Estimated from Nitrogen Adsorption Behavior at 77 K.

sample name micropore volumea (cm3 g–1) external surface areab (m2 g–1)
FAU 6.1 0.278 (0.270) 12.1
LTA 6.7 not measuredc not measuredc
MFI 1.2 0.146 (0.148) 22.3
YFI 1.3 0.148 (0.142) 6.0
MOR 1.5 0.175 (0.168) 8.8
MOR 1.7 0.169 (0.163) 10.5
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a

Estimated from t-plot method61 (value from capillary condensation capacity62 is shown in parentheses).

b

Estimated from the t-plot method.61

c

Not able to be estimated from nitrogen adsorption due to blocking by Na+.67−69

The external surface areas of the FAU-, MFI-, YFI-, and MOR-type samples are estimated from the nitrogen adsorption isotherms. In general, the external surface area was small (<23 m2 g–1), indicating relatively large crystallite sizes (Table 2).

Acidic Properties

Infrared/mass spectroscopy temperature-programmed desorption (IRMS-TPD) of ammonia quantifies the number and strength of each of Bro̷nsted and Lewis acid sites.70,71 This method has shown that the ammonia desorption enthalpy from the Bro̷nsted acid sites on H-form zeolite, an index of Bro̷nsted acid strength, depends mainly on the type of framework but not on the aluminum concentration.55,72−75 This is because the Al–O distance mainly controls the acid strength of the Si–OH–Al bridge.58,60,76 Therefore, it is speculated that an aluminosilicate framework has its own inherent acidity, or electron-withdrawing property, due to its framework topology, and in this study, we compare the Bro̷nsted acid strength of the H-form zeolite and the ion exchange property of the Na-form zeolite.

The ammonia desorption enthalpy from the Bro̷nsted acid sites of H-form zeolite has been found to be 130–140 kJ mol–1 for MFI with 0.3–1.3 mol kg–1 of Al,55,77 averagely 143 kJ mol–1 for YFI with 0.3–1.4 mol kg–1 of Al76 and averagely 148 kJ mol–1 for MOR with 0.4–2.4 mol kg–1 of Al.55,70,72 The Al contents of the parent Na-zeolites (MFI: 1.2 mol kg–1, YFI: 1.3 mol kg–1 and MOR: 1.5–1.7 mol kg–1 as shown in Table 1) were within the above ranges for which the acid strengths of the corresponding H-zeolites have been revealed.

Furthermore, we studied the properties of YFI 1.3 in detail. Although the synthesis lot was different from that in the present study, the composition and synthesis methods were the same. Infrared (IR) spectra of adsorbed d3-acetonitrile, pyridine, and ammonia, the conventional ammonia TPD profile, the TPD profile from Bro̷nsted acid site, and the ammonia desorption enthalpy distribution can be referred to our paper.76 The applied techniques showed that the Lewis acidity was negligible (0.1 mol kg–1), and the number of Bro̷nsted acid sites (1.3 mol kg–1) was similar to the number of Al atoms (1.4 mol kg–1). These results indicate that most of the Al is incorporated into the framework. The ammonia desorption enthalpy from the Bro̷nsted acid sites was 143 kJ mol–1. Therefore, it can be concluded that the Bro̷nsted acid strength of H-form YFI, which corresponds to the presently used Na-form sample, is indicated by the ammonia desorption enthalpy of 143 kJ mol–1.

MFI 1.2 is an international reference zeolite, and it is opened public66 that the Bro̷nsted acid amount (1.3 mol kg–1) was close to the Al content (1.3 mol kg–1), whereas the Lewis acid amount was negligible (0.002 mol kg–1), indicating that most of the Al is incorporated into the framework. The ammonia desorption enthalpy of the H-form is reported to be 136 kJ mol–1. The conventional ammonia TPD profile, the TPD profile from the Bro̷nsted acid site, and the ammonia desorption enthalpy distribution can be found in public databases, as well as other analytical results.66

MOR 1.7 was the subject of group study, and various characterization techniques such as nuclear magnetic resonance (NMR), ammonia TPD, and IR of CO and pyridine showed that most of Al atoms were incorporated into the framework.64

The above zeolites (MFI, YFI and MOR) allow comparison of the acidic property of the H-form and the ion exchange property of the Na-form in the same Al concentration range.

On the other hand, in this study, we used Na-form samples of FAU and LTA with high Al concentrations; FAU: 6.1 mol kg–1 (X type zeolite), LTA: 6.7 mol kg–1 (A type zeolite). Zeolites with such high Al concentrations are destroyed in acidic conditions, so conversion into the NH4- or H-form is not possible. However, as mentioned in the previous paragraphs, we speculate that the inherent acidity of the aluminosilicate framework is mainly controlled by the framework topology, allowing us to compare the ion exchange behavior of the Na-form and the acidic property of the H-form even though they have different the aluminum concentrations. The ammonia desorption enthalpy from the Bro̷nsted acid sites was observed to be ca. 110 kJ mol–1 for FAU (Y type zeolite) with 4.4–5.5 mol kg–1 of Al,72,74,78 and 132 kJ mol–1 for LTA (UZM-9 type zeolite) with 4.8 mol kg–1 of Al,60 and will be compared with the ion exchange properties in the next section.

Ion Exchange Properties

Throughout this study, the ion exchange properties were evaluated by the Cs concentration in the aqueous solution after the ion exchange procedure and the analysis of the Cs contents in the solid was omitted. There are two reasons for this. (1) The final objective of the study is to understand the ion exchange function for the removal of Cs species from water. (2) The dissolution of a small amount of zeolite containing a low concentration of Cs after filtration would result in a large experimental error. However, the analysis of the Cs content was performed on LTA 6.7 under equilibrium with an aqueous solution containing 0.851 mol m–3 Cs+ (final composition), followed by dissolution in hydrofluoric acid for ICP analysis. The Cs content in the solid was 0.0579 mol kg–1, in agreement with 0.0582 mol kg–1 estimated from the solution composition, supporting its validity.

Then, from the analysis of the solutions, the relationship between the compositions of zeolite and solution was estimated in 0–3 mmol m–3 region for the zeolite samples used, as shown in Figure S1. From these results, plots of Inline graphic against cCs+(aq) are obtained as shown in Figure 3. Nearly straight lines were obtained, showing the availability of Langmuir-type analysis using eq 3. From the slope and intercept, the ion exchange capacity cIEZ(Z) and the equilibrium constant K were estimated as shown in Table 1. For reference, the ion-exchange isotherms calculated based on the determined cIEZ(Z) are shown in Figure S2.

Figure 3.

Figure 3

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Plots of cCs+(aq)/cCs+(Z) against cCs+(aq) on (A) FAU and LTA, and (B) MFI, YFI and MOR type zeolites.

For MFI-, YFI-, and MOR-type zeolites, the estimated cIEZ(Z) (the number of sites playing a role of ion exchange sites under the present experimental conditions) was approximately in agreement with cAl(Z) (Figure 4), confirming that one ion exchange site was generated by substitution of one Si (+4) atom by one Al (+3) atom in the framework. However, FAU and LTA showed far lower cIEZ(Z) values than cAl(Z). Presumably, some of the cations in the sodalite cage, which is separated from the outside by the 6-ring windows, which require high temperature for passage of cations,50 were not exchanged under these conditions (room temperature). It is noteworthy that wastewater treatment is performed at ambient temperature, and the present experiments demonstrate the ion exchange functions applicable to practical treatment processes.

Figure 4.

Figure 4

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Plots of estimated amount of ion exchange sites cIES(Z) against aluminum content cAl(Z). The thick line shows cIES(Z) = cAl(Z).

On the other hand, the calculated K was clearly different among zeolite species as FAU < LTA < MFI < YFI < MOR, while the difference in cAl(Z) between the two MOR samples did not change K. The larger K indicates the high ability of Na-form zeolite to remove Cs+ from aqueous solutions in the coexistence of Na+. The high exchange ability of MOR is consistent with the preceding literature.20

As shown in Figure 5, the standard Gibbs energy Inline graphic of the ion exchange (1) decreases with the increase in ammonia desorption enthalpy from the Bro̷nsted acid sites of the corresponding H-form zeolite. Since ammonia desorption enthalpy (heat of ammonia adsorption) is an indicator of acid strength, this indicates that the zeolite framework, which generates strong Bro̷nsted acidity in the H-form, strongly stabilizes Cs+.

Figure 5.

Figure 5

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Plots of standard Gibbs energy of reaction 1Inline graphic of zeolites against ammonia desorption enthalpy ΔHdes NH3 of corresponding H-form zeolites.

As mentioned above, we propose that the Bro̷nsted acid strength of the Si–OH–Al bridge is controlled by the Al–O distance, suggesting that the acid strength (electron withdrawing property) is due to structural stress. An H-form zeolite has Al(−O–Si)4 units where H+ is bonded to one of the four O atoms. Theoretical calculations reveal that the O–H bond is a covalent bond, not an ionic bond, and the Al–O distance in Al–OH–Si becomes longer than the other three Al–O distances. In the NH4 form, the NH4+ cation does not have a covalent bond with the framework atoms and is usually coordinated to two oxygen atoms. The four Al–O distances are similar and shorter than the Al–O distance in the Al–OH–Si of the H-form.58 Meanwhile, there are complex mechanical forces around the Al–O–Si bridge. Theoretical calculations reveal that the stress and compression from both ends of Al–O–Si change the distance between Al–O, and the shorter the Al–O, the higher the desorption energy (enthalpy) of ammonia.58

In the case of Al–O–Si compressed from both ends, the geometry in which the distance between all four Al–Os is the same is relatively stable (Scheme 1A), whereas in the case of Al–O–Si stretched from both ends, the geometry in which one Al–O distance is longer is relatively stable (B). In the former, the negative charge generated by the isomorphous substitution of Si4+ by Al3+ is delocalized, and the charge is shared by four oxygen atoms. In contrast, in the latter, the negative charge is localized on one oxygen atom. A cation with a positive charge delocalized over a wide space, i.e., a soft Lewis acid, prefers the former Al–O–Si (soft Lewis base), while a hard Lewis acid prefers the latter hard Lewis base.

Scheme 1. Schematic Drawings of Influence of Local Geometry on Charge Localization around Ion Exchange Sites.

Scheme 1

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(A) shows a Si–O–Al bridge compressed from both ends, whose negative charge is delocalized, strongly acidic (prefers NH4+ than H+), and prefers Cs+ than Na+. (B) shows a Si–O–Al bridge stretched from both ends, whose negative charge is localized to an O atom, weakly acidic (prefers H+ than NH4+), and prefers Na+ than Cs+.

NH4+ is a larger and therefore softer Lewis acid than H+. The strong Bro̷nsted acidity means instability of H+, and more exactly, high ammonia desorption energy means the stability of NH4+ compared to H+ on the discussed ion exchange site. It reflects the softness of the Lewis base property of the site.

On the other hand, Cs+ is larger and therefore softer Lewis acid than Na+. Cs+ should prefer a soft Lewis base, i.e., the Al(−O–Si)4 group with equal Al–O distances and a shared negative charge on four oxygen atoms. This tendency should be common for the cases of ammonia adsorption (H+ → NH4+) and Na–Cs exchange (Na+ → Cs+). Thus, the influence of the chemistry of the silicate framework on the selectivity of ions can be explained.

In contrast, the equilibrium constant K or the Gibbs energy Inline graphic was not related to the pore and cavity size of these zeolites (representative parameters are shown in Table S1). At least for the four framework types treated in this study, it can be said that chemical properties have a stronger influence than porosity.

Conclusions

The analysis of ion exchange behavior between Na-type zeolite and Cs-containing aqueous solution showed that the equilibrium constants at room temperature were in the order FAU < LTA < MFI < YFI < MOR, as the order of Bro̷nsted acid strengths in the corresponding proton form zeolites. The Gibbs energy of ion exchange, which reflects the above equilibrium constant, showed a linear relationship with the ammonia desorption enthalpy from the Bro̷nsted acid sites on the proton form zeolites, an indicator of the Bro̷nsted acid strength. In contrast, the equilibrium constant was not related to the pore and cavity size. At least for the four framework types treated in the present study, it can be said that chemical properties have a stronger influence than porosity.

Acknowledgments

This research was carried out as part of the Tottori University Junior Doctor Training School, Environmental Research Program with support from the JST Next Generation Human Resources Development Project. We also received support from JSPS KAKENHI (21H01717, 23H05454).

Supporting Information Available

The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.langmuir.4c00801.

  • Microporous properties of frameworks, compositions of solvent and zeolite after the ion exchange, and ion exchange isotherms (PDF)

The authors declare no competing financial interest.

Supplementary Material

la4c00801_si_001.pdf (769.7KB, pdf)

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