Amino-functionalized magnetic particles (Fe3O4@SiO2-NH2) with core-shell structure were synthesized and evaluated for rapid boron removal from aqueous solution. Results showed that the specific surface area of Fe3O4@SiO2-NH2 (165.17 m2⋅g− 1) increased greatly compared to the pure Fe3O4 (49.07 m2⋅g− 1). The adsorption equilibrium was less than 2 h with an adsorption capacity of 29.76 mg⋅g− 1at pH = 6 of 15°C. The quasi second-order kinetic model described well the boron adsorption process and the Freundlich model was more suitable for characterizing the adsorption isotherms. Furthermore, the negative value of Gibbs free energy indicated that the adsorption was spontaneous and an exothermic process. The zeta potential and XPS analysis before and after adsorption revealed that the main adsorption mechanism was the hydrogen bonding formation between the terminal –NH2 groups of the adsorbent and the boric acid. In addition, the adsorbent still maintained a high adsorption performance after five adsorption-desorption cycles, which illustrated that the Fe3O4@SiO2-NH2 may be a potential adsorbent for the environmental boron removal treatment.
Research Article
Facile synthesis of core-shell magnetic Fe3O4@SiO2-NH2 nanoparticles and their application for rapid boron removal from aqueous solution
https://doi.org/10.21203/rs.3.rs-3431188/v1
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Synthesis
Magnetic nanoparticles
Fe3O4@SiO2-NH2
Boron adsorption
Boron and boron compounds has been widely used in glass, ceramics, nuclear power and chemical industry, etc. due to its characteristics of lightweight, heat-resistant, wear-resistant, high-strength and high thermal neutron absorption[1]. Boron is also an indispensable trace element for animals, plants and humans [2] and was used as boron fertilizer in agriculture. Nevertheless, an excessive intake of boron can do seriously harm to the organisms, causing the declined crop production and human nervous diseases [3, 4]. So the amount of boron in drinking water was no more than 2.4 mg·L− 1 limited by the World Health Organization (WHO) [5], and this value was even less than 1.0 mg·L− 1 in both drinking and irrigation water in China [6, 7]. Therefore, the boron recovery/removal from aqueous solution (salt lake brine, seawater, drinking water and wastewater, etc.) is crucial for the boron resource utilization and environmental treatment.
Mainly technologies for boron extraction include electro-flocculation[8], membrane filtration [9], chemical precipitation [10], solvent extraction [11], and adsorption (including ion exchange) [12, 13]. Among of which, adsorption has become one of the most effective methods due to its simple operation, high selectivity and low energy consumption. Currently, Study on boron adsorption has being focused on various absorbents, such as ion exchange resins, activated carbon, metal oxides and hydroxides, polymers, metal-organic frameworks (MOFs) and magnetic adsorbents [14–18], and each kind of these absorbents has its own advantage and disadvantage during boron removal process. The magnetic nanoparticles (MNPs) and their functional composites had embodied high boron adsorption efficiency, simple magnetic separation and easy regeneration because of their large surface area, strong magnetic property, low cost and environmentally friendly. The Fe3O4 nanoparticles are the most frequently used as magnetic absorbents for the boron absorption [19]. However, these materials are susceptible to autoxidation, aggregation and have fewer surface functional groups interacting with the boron. Thus, functionalized magnetic nanoparticles with chelating species are often necessary. Based on the amphoteric property of amino groups, the amino-based MNPs, performing surface modification by covalently linking organosilane species with surface silanol groups, has been extensively studied and used as absorbents in water treatment [20]. Liu Z [21] et al. synthesized Fe3O4@SiO2-NH2 and modified its surface with polyacrylamide for the removal of heavy meatal ions of Cd2+, Pb2+ and Zn2+ ions from wastewater, and the adsorption capacity of this material was in the order of Pb2+>Cd2+>Zn2+. Ghorbani F [22] et al. synthesized the core-shell magnetic nanocomposite Fe3O4@SiO2@NH2 with the silica source extracted from rice husk and the 3-aminopropyltrimethoxysilane functional group and then used it for the adsorption of Methyl Red dye. The maximum adsorption was 125 mg·g− 1 much higher than most of the other absorbents. Furthermore, the removal efficiency was just decreased by 10% after five regeneration cycles. Donga C et al [23] coupled graphene oxide on Fe3O4@SiO2-NH2 to obtain composites for the adsorption of three heavy metal ions on Pb(II), Cd(II) and Ni(II), and showed the absorption capacity followed the order Pb(II) > Cd(II) > Ni(II). From the above studies, it is known that the amino-based magnetic absorbents are chemical stable, reusable and show great application potential of heavy metals removal during the water/wastewater treatment process. However, to the best of our knowledge, boron adsorption from aqueous solution and its interaction mechanism with amino-based magnetic absorbent still remains unknown. Therefore, in this work, the Fe3O4@SiO2-NH2 was prepared by a facile sol–gel method and then applied to remove boron from solution. The pH effect, adsorption isotherm, kinetics, and regeneration were studied.
2.1 Materials
Ferric chloride hexahydrate (FeCl3·6H2O), sodium acetate anhydrous (NaOAc), ethylene glycol (EG), tetraethyl orthosilicate (TEOS), 3-Aminopropyltriethoxysilane (APTES), ethanol (EtOH), and ammonia solution (NH3·H2O), boric acid (H3BO3) are analytically pure reagents, and can be used directly without further purification.
2.2 Synthesis of Fe3O4 MNPs
The Fe3O4 MNPs were synthesized by the solvothermal method [24] with mirror changes. In brief, 2.0 g of FeCl3·6H2O, 2.89 g NaOAc and 1.5 g PEG-4000 were added in 70 mL of ethylene glycol. The mixture was stirred vigorously until completely dissolved, then sealed in a Teflon-lined stainless-steel autoclave (100 mL) after adding 10 mL H2O and heated at 198 ºC for 12 h. When the reactor was cooled down to room temperature, the product was collected with a magnet and washed with ultrapure water. After that, it was dispersed in a mixture of ethanol and water for further use.
2.3 Synthesis of Fe3O4@SiO2-NH2 MNPs
Fe3O4@SiO2-NH2 was synthesized by the sol-gel method [25]. Firstly, 0.5 g freshly prepared Fe3O4 MNPs were dispersed in a mixed solution of 200 mL ethanol and 100 mL water, ultra-sonicated for 3 min. Then 6 mL NH3·H2O (25–28 wt%) was added to adjust the solution pH to be alkaline, followed by the addition of 2–8 mL TEOS, and the reaction was carried out under mechanical stirring for 40 min. Finally, the reaction was further performed for 4 h prior to the addition of 1–10 mL APTES. Afterward the precipitate was collected, washed with water, and dried in an oven at 60 ºC overnight. The overall synthesis steps were shown in Scheme 1. During the above process, the amount of TEOS and APTES were investigated to obtain the key preparation parameters for boron absorption property.
2.4 Characterization of Fe3O4 and Fe3O4@SiO2-NH2 MNPs
The XRD (X-ray diffraction) spectrum was recorded by XRD diffractometer (D8 Discover, Germany). The operating conditions were 60 kV and 60 mA using Cu - Kα source (λ = 0.154 nm) and the samples were scanned in the 2θ range of 5–70º. The morphology of as-prepared functionalized MNPs was determined with scanning electron microscopy (SEM, SU8010, Japan) and transmission electron microcopy (TEM, FEI Tecnai G2 F30, America). The SEM and TEM images were acquired at an accelerating voltage of 30 to 200 kV, respectively. The chemical structure was analyzed by the fourier transform infrared spectra (FTIR, Nexus, America) which were recorded with a resolution of 4 cm− 1 in the region of 400–4000 cm− 1. Specific surface area, pore size distribution and pore volume of the samples were measured by a fully automated specific surface and pore size analyzer (Autosorb IQ2, America). The zeta potential (pHzpc) was measured by Zetasizer Nano ZS analyzer (Malvern, ZS90, UK).
2.5 Adsorption experiments
Stock solutions of boric acid were prepared with ultrapure water. A certain amount of Fe3O4@SiO2-NH2 was added into the boric acid solution and shaken for 12 h in a shaker for the boron adsorption. Then the boron-loaded adsorbent was separated by magnetic separation. The boron concentration was determined by the mannitol titration method. During the absorption process, the effects of adsorbent dosing, initial solution pH, contact time and reaction temperature on the adsorption were investigated.
The adsorption capacity of boron was calculated by the following equation:
1Where c0 and ce represent the boron concentration in solution before and after adsorption, respectively. V is the solution volume (L), m represents the adsorbent dosage (g), and q represents the adsorption capacity (mg·g− 1).
2.6 Regeneration and reuse study
Desorption experiments were conducted by mixing 0.6 g of the boron loaded Fe3O4@SiO2-NH2 materials with 30 mL alkaline solution (pH = 10). The mixture was shaken at 250 rpm for 1 hour during room temperature and magnetic separated, and this process was repeated for three times to make sure completely adsorbent desorption. Then, the adsorbent was regenerated with a mixture of ethanol and ammonia (pH = 11). And this material dried overnight at 60°C and reused for the further adsorption.
3.1 Material synthesis process optimization
The optimization synthesis process was carried out by varying the addition amounts of TEOS and APTES based on the boron adsorption capability of the materials. As shown in Fig. 1, the suitable dosages of APTES and TEOS were 7 mL, 6 mL, respectively.
3.2 Structural and morphological characterization
In order to obtain the structural information of Fe3O4 and Fe3O4@SiO2-NH2, XRD characterization was carried out and the results were shown in Fig. 2a. It can be seen that the diffraction peaks of as-prepared Fe3O4 at 2θ = 18.32º、30.16º、35.46º、43.11º、53.46º、57.00º and 62.54º are corresponding to (111), (220), (311), (222), (400), (422), (511), and (440) crystal planes, respectively, which agreed well with the pure Fe3O4 standard PDF card (JCPDS: 89–0691). The diffraction peaks of Fe3O4@SiO2 and Fe3O4@SiO2-NH2 are identical with the synthesized pure Fe3O4 except for the broad peak at 2θ = 20–30º of the Fe3O4@SiO2-NH2, which can be attributed to the formation amorphous structure of SiO2 coating on the Fe3O4 surface.
According to the FTIR spectra (Fig. 2b), the peak at 575 cm− 1 appeared in the Fe3O4, Fe3O4@SiO2 and Fe3O4@SiO2-NH2 samples was the stretching vibration peak of Fe-O [26]. The bands at about 465 cm− 1, 797 cm− 1 and 1097 cm− 1 in Fe3O4@SiO2 and Fe3O4@SiO2-NH2 samples were related to the bending mode, symmetric and asymmetric stretching vibrations of Si-O-Si band [27], respectively. These indicated that the SiO2 layer has been successfully coated around the Fe3O4 MNPs surface. The spectrum of Fe3O4@SiO2-NH2 showed the characteristic peak at 1565 cm− 1 that can be attributed to the functional group of N-H bending vibrations [28]. Moreover, the adsorption peaks at 2923 cm− 1 and 2856 cm− 1 can be generated by the symmetric or antisymmetric C-H stretching vibrations of methyl or methylene. In addition, the bending and stretching vibrations of -OH bands around 1632 cm− 1 and 3438 cm− 1 in all samples were associated with the water molecules adsorption. It was noted that the spectrum of Fe3O4@SiO2-NH2 at 3438 cm− 1 became sharper compared with the Fe3O4 sample, which may be attributed to the N–H symmetric stretching vibrations.
The SEM image of Fig. 3a showed a uniform spherical structure of Fe3O4 MNPs with a diameter of 30–40 nm. After coating SiO2 on Fe3O4 and grafting the amino group (Fig. 3b), the morphology remains the same but the diameter is larger than that of Fe3O4. Furthermore, as seen from Fig. 3bi-bⅱ, the TEM image of Fe3O4@SiO2-NH2 showed a core-shell structure, with the darker part of Fe3O4 core and the lighter colored part of SiO2 shell.
Figure 4a showed the N2 adsorption/desorption isotherms curves of Fe3O4 and Fe3O4@SiO2-NH2 measured at 77 K. Isotherms of these two samples exhibited typical IV isotherms, indicating they were mesoporous materials. The Brunauer-Emmett-Teller (BET) surface area of Fe3O4@SiO2-NH2 was 165.17 m2/g (Table S1) much larger than that of pure Fe3O4 (49.07 m2/g), and the pore diameter (6.57 nm) was much smaller, which also indicated the mesoporous structure of Fe3O4@SiO2-NH2 adsorbent material. In Fig. 4b, the zeta potential of the Fe3O4@SiO2-NH2 was also conducted at solution pH ranging from 3 to 10. According to the results, the isoelectric point value was 4.59, which indicated that when the pH was lower than 4.59, the surface of Fe3O4@SiO2-NH2 was positively charged; on the contrary, it became negative.
3.3 Adsorption studies
3.3.1 Factors affecting adsorption
Firstly, the dosage effect of adsorbent on boron adsorption was shown in Fig. 5a, it ranged from 0.2 to 5 g·L− 1 at 25 ºC and the initial boron concentration was 0.3 mol·L− 1. It can be seen that the adsorption capacity increased with the increase of the dosage and then gradually kept stable when the added dosage was more than 5 g·L− 1. This can be attributed to the availability of more adsorbent adsorption sites for the boron adsorption. However, when the effective active sites reached a state of equilibrium due to the utilization of all boron in the solution at higher dosage, the adsorption capacity barely increased and kept constant. The optimum dosage was found to be 5 g·L− 1 and used for the following experiments.
The influence of initial solution pH from 3 to10 on the adsorption capacity was also observed and shown in Fig. 5b. It is noted that the adsorption capacity of Fe3O4@SiO2-NH2 for boron firstly increased at acidic pH and then decreased at alkaline pH. The optimum pH value was about 6. This can be interpreted by the surface charge variation of the adsorbent and solution structure changes of boric acid with pH. Based on the zeta potential of Fe3O4@SiO2-NH2 (Fig. 4b), the acid-base behavior of the functional -NH2 groups under differential pH acted as the following equation [29]:
\(-\text{N}{\text{H}}_{2}+ {\text{H}}_{3}^{+}\text{O }\text{⇌}\text{ }\text{N}{\text{H}}_{3}^{+}+{\text{H}}_{2}\text{O}\) (< isoelectric point 4.59)
\(-\text{N}{\text{H}}_{2}+\text{O}{\text{H}}^{-}\text{⇌}\text{ }\text{N}{\text{H}}^{-}+{\text{H}}_{2}\text{O }\) (> isoelectric point 4.59)
The pH-dependent of boron species in boric acid solution was shown in Fig.S1 [30]. It can be seen that more than 94% of the boron species was the neutral boric acid when the pH was below 6. While the boric acid gradually changed into borate anions with the increasing of pH value. At acidic condition, the terminal -NH2 groups were protonated which is not favorable for the boron acid adsorption. Moreover, the acidic environment could facilitate the dissolution of the adsorbent and also decreased the adsorption capability. While at alkaline condition, the terminal -NH2 groups were deprotonated and the electrostatic repulsion between the deprotonation –NH2 groups and the borate anions decreased the adsorption sharply. Therefore, the near-neutral pH was more suitable for the boron adsorption.
Besides, the effect of initial boron concentration and the contact time on the adsorption was shown in Fig. 5c-d, respectively. The adsorption capacity showed a steady increase at lower boron concentration (0.05 to 0.3 mol·L− 1), and further concentration increase had no significant effect on the adsorption due to the saturation adsorption sites on the adsorbent surface. In Fig. 5d, it is noticeable that the adsorption reached its equilibrium quickly after 2 h contact time.
3.3.2 Adsorption mechanism
To investigate the possible adsorption mechanism of boron on the surface of the Fe3O4@ SiO2-NH2 adsorbent, XPS analysis of the adsorbent before and after boron adsorption was carried out and the spectra were shown in Fig. 6. It is clear that a weak binding energy peak of B 1s at 189.41 eV was observed after adsorption, indicating the successful boron adsorption on the surface of the adsorbent. Fe element was not detected due to the silica shell on the surface Fe3O4 particle. The N 1s XPS spectra can be deconvoluted into two peaks of C-N at 398.37 eV and N-H at 396.51 eV, respectively [31]. It is worth noting that both of these two binding energies increased after boron adsorption. Furthermore, the peak area percentage of N-H has increased from 23.10–46.83%, which can be inferred that some possible hydrogen bonding were formed between the nitrogen atom of terminal -NH2 groups and the hydroxyl of boric acid during boron adsorption process. The decreasing binding energy of C-N in C 1s spectra (in Fig. S2) may also be due to this hydrogen bonding formation.
3.3.3 Adsorption kinetics, isotherms and thermodynamic study
The adsorption kinetics of boron on Fe3O4@SiO2-NH2 adsorbent was studied using the pseudo-first-order kinetic [32] and the pseudo-second-order kinetic [33] models given as the following:
pseudo-first-order model: \(\text{l}\text{n}({q}_{\text{e}}-{q}_{t})=\text{l}\text{n}{q}_{\text{e}}-{k}_{1}t\)(2)
pseudo-second-order model: \(\frac{t}{{q}_{t}}=\frac{1}{{k}_{2}{q}_{\text{e}}^{2}}+\frac{t}{{q}_{\text{e}}}\) (3)
where qe and qt are the adsorption capacity (mg/g) at equilibrium and time of t, respectively. k1 and k2 are the rate constant (g·mg− 1·h− 1).
The fitting results were shown in Fig. 7, and the parameters calculated were listed in Table S1. Based on the high correlation coefficient R2 = 0.9998, it was known that the adsorption followed the pseudo-second-order kinetic model, which indicated the chemisorption process was mainly controlled by the rate-limiting step.
The isotherms adsorption process of boron at temperatures of 288.15, 298.15, 308.15 and 318.15 K were investigated using Langmuir [34] and Freundlich [35] isotherm models expressed as the following:
Langmuir: \({q}_{\text{e}}=\frac{{q}_{\text{max}}·{K}_{\text{L}}·{c}_{\text{e}}}{{1+q}_{\text{max}}·{K}_{\text{L}}}\) (4)
Freundlich: \({q}_{\text{e}}={K}_{\text{F}}\text{∙}{c}_{e}^{1/n}\) (5)
where qmax, qe are the maximum and equilibrium adsorption capacity adsorption capacity (mg·g− 1), respectively. ce is the boron concentration at equilibrium (mg·L− 1), KL, KF are the adsorption equilibrium constant (L·mg− 1) and the adsorption capacity constant (mg·g− 1), respectively. n is the heterogeneity factor indicating the strength of adsorption.
The fitting curves of Langmuir isothermal model and Freundlich isothermal model were shown in Fig. 8 and the corresponding parameters were listed in Table S2. In Fig. 8a, it can be seen that the boron adsorption capacity adsorbed by Fe3O4@SiO2-NH2 decreased with the rising of temperature. This phenomenon was different with other boron adsorbents reported previously [36, 37] and can be ascribed to the anti-correlation between hydrogen bonding and temperature. As we known above, the hydrogen bonding was the main interaction during boron adsorption process, and it would gradually became weaker and weaker with the rising of temperature, which was not favorable for the boron adsorption. According to Fig. 8b-c, It was noted that both Langmuir and Freundlich models could describe the boron adsorption isotherms well since the correlation coefficient R2 > 0.96, and the qmax for Fe3O4@SiO2@NH2 was 51.19 mg·g− 1 at room temperature. But compared to the Langmuir model, the Freundlich model was more suitable for characterizing the adsorption isotherms.
The thermodynamic parameters can be obtained from the following equations [38]:
$$\text{l}\text{n}\text{K}=\frac{\varDelta S}{R}-\frac{\varDelta H}{RT}$$
6
$${\Delta }G=-RT\text{l}\text{n}K$$
7
where R is the universal gas constant (8.314 J·mol− 1·K− 1); T is the temperature (K); K can be calculated from the Freundlich model at different temperatures.
Based on the plot of lnK against 1/T (Fig. 8d), the thermodynamic parameters were summarized in Table 1. The determined negative values of ΔG and ΔH indicated the boron adsorption on Fe3O4@SiO2-NH2was a spontaneous and exothermic process, and the negative entropy suggested a decreased confusion at the interface of adsorbent-adsorbate during the adsorption process.
|
T (K) |
ΔG (KJ·mol− 1) |
ΔH (KJ·mol− 1) |
ΔS (J·mol− 1·K− 1) |
|---|---|---|---|
|
288.15 |
-9.28 |
-0.20 |
-37.26 |
|
298.15 |
-9.13 |
||
|
308.15 |
-8.87 |
||
|
318.15 |
-8.10 |
3.4 Regeneration study
Five adsorption-desorption cycles were performed to study the regeneration and reusability of the adsorbent. The alkali solution (pH = 10) was used as an eluent to desorbed the boron loaded Fe3O4@SiO2-NH2 MNPs and then regenerated by the mixture of ethanol and ammonia with a pH of 11. The results (Fig. 9) showed that there was a slight absorption reduction during the adsorption-desorption process due to the decrease of adsorption sites on adsorbent. Nevertheless, the Fe3O4@SiO2-NH2 MNPs adsorbent can still maintain a high adsorption capability after five cycles. These indicated that the Fe3O4@SiO2-NH2 MNPs have an acceptable reusability and stability during adsorption-desorption process and can be the potential adsorbents for the environmental boron removal treatment.
The amino-modified magnetic core–shell Fe3O4–SiO2–NH2 nanoparticles were synthesized via a facile one-step method and also investigated for the rapid boron removal from aqueous solution. The results indicated that the boron adsorption on this synthesized magnetic nanoparticles was strongly influenced by the adsorbent dosage, solution pH, initial boron concentration and adsorption temperature. The adsorption equilibrium was less than 2 h and easy to be desorbed. Adsorption kinetics of boron can be well described by pseudo-second-order kinetics. Furthermore, the boron adsorption mechanism was mainly due to the hydrogen bonding interaction among boric acid molecular and the terminal –NH2 groups. The adsorption isotherm and thermodynamic data suggested the Freundlich isothermal model was more suitable and it is a spontaneous exothermic process. Based on the five adsorption-desorption experimental cycles, the regenerated adsorbent still exhibited good adsorption affinity for boron in aqueous solution, which highlighted that this amino-functionalized magnetic nanoparticles would be used as efficient and recyclable adsorbents for boron recovery from water and wastewater, etc.
Acknowledgements This work was financially supported by the Project for Young Scientists in Basic Research, CAS (YSBR-039), Youth Innovation Promotion Association, CAS (E010GC1501) and the National Natural Science Foundation of China (U1507112).
Conflict of interest The authors declare no conflict of interest and competing financial interest.
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Scheme 1 is available in the Supplementary Files section.
No competing interests reported.
- Scheme1.png
Scheme 1 Schematic preparation of Fe3O4@SiO2-NH2 MNPs
- Supplementaryinformation.docx
