Silica-pillared Clay Research Articles

Copper oxide-incorporated pillared clay granular nanocomposite for efficient single and binary, batch and fixed bed column adsorption of levofloxacin and crystal violet

This study investigates single and binary removal of levofloxacin (LV) and crystal violet (CV) using granular CuO-silica pillared clay (G-CuO-SPC) in batch and continuous setups. Silica pillared clay (SPC) synthesized by sol–gel with SiO2 agents and cationic surfactants exhibited a 15-fold increase in surface area after column formation. CuO nanoparticles were incorporated into SPC by direct thermal decomposition, and alginate biopolymer facilitated granulation. Characterization techniques (XRD, N2 adsorption–desorption, FTIR, FESEM and EDS-mapping) confirmed uniformly-dispersed monoclinic CuO nanoparticles in G-CuO-SPC. LV adsorption peaked at pH:5–6, while CV adsorption was almost pH-independent. Sips isotherm modeling revealed maximum capacities for LV (705.2–731.1 mg/g) and CV (914.4–992.4 mg/g) at 25-55℃, with capacities decreasing in binary systems. LV and CV adsorption on G-CuO-SPC was spontaneous, exothermic, and occurred via mechanisms, including electrostatic interaction, van der Waals forces, hydrogen-bonding, and n-π interaction. Fixed-bed analysis favored the Yan model, indicating multilayer adsorption without a classical S-shaped profile.

Reusable granulated silica pillared clay for wastewater treatment, selective for adsorption of Ni(II)

The article presents a study on the suitability of silica pillared clay (SPC) encapsulated with biopolymers, such as alginate, chitosan, or a combination of both, for the adsorption of Ni(II) from aqueous solutions. In the current age of stringent environmental regulations, there is an urgent requirement to identify novel sorbents that can be readily commercialized and employed in large-scale systems to efficiently remove and recover metal compounds from wastewater. Therefore, the study aimed to encapsulate powdered silica pillared clay to produce stable granules via a modified solution casting method, which was confirmed through various characterization studies (FESEM, XRF, XRD, BET, and FTIR). The study found that ALG-SPC showed the best adsorption capacity, owing to its relatively high specific surface area and the negative charge of the alginate. In contrast, encapsulation with chitosan resulted in poor performance due to a significant reduction in porosity. The study also investigated the behaviour of ALG-SPC in a binary solution containing both Ni(II) and Cr(VI) and found that it exhibited selectivity for Ni(II) over Cr(VI). The presence of Cr(VI) did not negatively affect Ni(II) adsorption; in contrast, Ni(II) helped to Cr(VI) adsorption under a limited pH range. The study also conducted adsorption mechanism, kinetic, and equilibrium modelling. Recovery of adsorbed Ni(II) from saturated ALG-SPC was most effective in acidic solutions in comparison with electrolyte solution and methanol. The study's findings have important implications for the development of effective and selective adsorbents for heavy metal removal and recovery from wastewater.

Catalytic wet peroxide oxidation of phenol through mesoporous silica-pillared clays supported iron and/or titanium incorporated catalysts

Catalytic performances of Silica Pillared Clay (SPC) supports synthesized in different silica amounts both from standard SWy-2 clay mineral and Hançılı region bentonite rock (HWB), and iron (Fe) and/or titanium (Ti) incorporated SPCs in different combinations were evaluated in various advanced Catalytic Wet Peroxide Oxidation (CWPO) of phenol. Host clay mineral type led to different oxidation performances and metal loading created significant increases in the catalytic performance. CWPO performance of Fe-loaded SPCs was better than Ti-loaded ones, so oxidation parameters for Fe–SPCs were studied in detail. Catalyst amount and rise in temperature increased phenol conversion values significantly, and catalysts were more effective in lower pH reaction medium. Aromatic intermediates such as catechol, hydroquinone and benzoquinone formed at the beginning of oxidation were oxidized to carboxylic acids with an advancing oxidation time. The presence of carboxylic acids such as oxalic and formic acid resulted in relatively low total organic carbon (TOC) conversion values. The highest catalytic activity was obtained with high silica content Fe–SPCs synthesized with both host clays. Complete conversion was nearly achieved within 60 min with an experimental condition of T = 30 °C, pH = 3.7 and catalyst/solution ratio = 2 g/L for SWy-2 based catalyst by applying either CWPO or PCWPO (Photo Catalytic Wet Peroxide Oxidation) techniques. SCWPO (Sono Catalytic Wet Peroxide Oxidation) technique also yielded this value at the same oxidation conditions for HWB based catalyst. TOC conversion values at 240 min oxidation time were determined as 33% and 48% for SWy-2 based catalyst with CWPO and PCWPO techniques, respectively, and 37% for HWB based catalyst with SCWPO technique. SWy-2 based catalyst still retained its performance after 3 cycles.

Adsorption of chromium(VI) and crystal violet onto granular biopolymer-silica pillared clay composites from aqueous solutions

The present study deals with the adsorption of chromium oxyanions (Cr(VI)) as a metallic pollutant and Crystal Violet (CV) dye from an aqueous solution. Silica Pillared Clay (SPC) was prepared using the sol–gel method by SiO2 pillaring agent and cationic surfactant template. The main results of the pillaring process were the significant increase in specific surface area (40 to 600 m2/g), pore volume (0.13 to 1.43 cm3/g), and the formation of a mesopore structure. The powdered SPC was granulated by a combination of biopolymers (alginate and chitosan), which led to a decrease in SBET to 455 m2/g and the addition of functional groups (amine and carboxyl). The best pH for Cr(VI) adsorption was 3; however, CV adsorption varied slightly by pH. GBP-SPC's maximum monolayer adsorption capacities for Cr(VI) and CV were 66.33 and 208.9 mg/g, respectively. The kinetic studies showed the higher initial sorption rate of CV (29 mg/g.h) compared to Cr(VI) (18 mg/g.h). The adsorption of Cr(VI) was exothermic with an activation energy of 22.08 kJ/mol; in contrast, the adsorption of CV was endothermic with an activation energy of 13.95 kJ/mol, both in the range of physical adsorption. The higher affinity of GBP-SPC towards CV is related to the same behavior in the raw clay and SPC. Due to their permanent negative charge structure, these samples showed higher attraction towards cationic dye. Binary solution adsorption revealed that the presence of CV had a negligible negative effect on Cr(VI) uptake, whereas CV adsorption was significantly improved in the presence of Cr(VI).

Synthesis of C21H38ClN Assisted Si Pillared Clays and the Effects of CeO2 Addition on Its Supported Palladium Catalyst for Benzene Oxidation

Mesoporous silica-pillared clays (SPC) were prepared with C21H38ClN cationic surfactant as template and supported PdOx catalysts were prepared by impregnation method. The influence of addition of CeO2 on benzene combustion was evaluated. The samples were characterized by N2 adsorption–desorption, XRD, XPS, HRTEM and TPSR. Compared with the raw montmorillonite, the d001 value of SPC increased from 0.96 to 3.45 nm. Furthermore, the surface area was increased from 30 to 835 m2/g and the pore volume was increased from 0.11 to 1.30 cm3/g, respectively. The addition of CeO2 increased oxygen vacancies and improved the dispersion of PdOx on SPC, and the optimal addition of CeO2 was 10%. Therefore, of all the catalysts, 0.3%Pd/10%Ce/SPC could completely oxidize benzene at 280 °C, showing the highest catalytic activity. This catalyst showed high activity for benzene oxidation in wet conditions with or without Cl− displaying good durability, which should be related to the presence of Ce3+ on the surface of catalyst after reaction. The excellent pore structure of SPC, improved dispersion of PdOx and high concentration of Ce3+ on the catalyst surface were the key factors for the high catalytic activity of 0.3%Pd/10%Ce/SPC. Mesoporous silica-pillared clays (SPC) were synthesized and SPC supported CeO2 and PdO catalysts were prepared by impregnation method. The 0.3% Pd/10% Ce/SPC catalyst displayed the highest activity for benzene combustion.

Removal of Acid Blue 92 by Using Amino‐Functionalized Silica‐Pillared Clay as a New Nano‐Adsorbent: Equilibrium, Kinetic and Thermodynamic Parameters

AbstractIn this study, silica‐pillared clay (SPC) and functionalized samples by chitosan (SPC/CTS) and different amounts of poly diallyl dimethylammonium chloride (SPC/PDDA‐10, SPC/PDDA‐20, and SPC/PDDA‐30) have been synthesized and have been employed as some low‐cost and eco‐friendly adsorbents in the adsorptive removal of Acid Blue 92 (AB 92) from contaminated waters. The structural variation of functionalized and unfunctionalized samples confirmed by different techniques such as Scanning electron microscopy (SEM), Energy Dispersive X‐ray spectroscopy (EDX), X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FT‐IR) and N2 adsorption‐ desorption analysis. The SPC/PDDA‐30 was selected for further studies due to its effective adsorption. The optimum values of adsorbent dosage, dye concentration, contact time and pH were found 0.02 g, 120 mg/L, 120 min and 5.0 respectively by applying response surface methodology (RSM). The adsorption equilibrium data were satisfactorily predicted by the Langmuir model and the adsorption process best fitted with a pseudo‐second‐order model. Adsorption thermodynamic analysis indicated the uptake of AB 92 on SPC/PDDA‐30 was exothermic and spontaneous. The high adsorption capacity of the selected nanocomposite could maintain after five successive adsorption‐desorption cycles by using 0.5 M NaOH.

In-situ mesoporous silica pillared clay synthesis and effect of titanium and iron incorporation to structural properties

Abstract Standard Wyoming SWy-2 mineral as a clay source was modified by use of cetyltrimethylammonium bromide as surfactant before Silica Pillared Clays (SPCs) synthesis, while octylamine (OA) was chosen as an auxiliary surfactant. Using tetraethyl orthosilicate as a silica source by ranging silica/modified clay (Si/C+) molar ratio within 20–150, SPC supports were synthesized keeping OA/C+ molar ratio as 20. Hydrothermal syntheses of titanium and iron containing SPC catalysts were carried out with M/Si molar ratios in between 0.03 and 0.15. Structural characterization results explained well the proposed mechanism for formation of MCM-41 like silica pillars between clay layers. With an increase of (001) peak reflection yielding basal spacing values up to 6.9 nm, polycrystalline structure observed in XRD patterns was confirmed by TEM images in SPCs. TEM also showed silica phase formations between clay bundles. Structural properties at Si/C+ molar ratio as 50 were the best with a surface area of 1874 m2/g. Titanium loading resulted in some decreases in surface area values while structural properties of iron incorporated catalyst at low iron content were found to be closer to that of the support. The highest Lewis and Bronsted acidities were observed by low titanium and iron incorporation to high silica containing support, respectively. TGA results showed that calcination temperature of 550 °C was sufficient for stable structures formation. ICP analysis and TEM images indicated that titanium species settled locally nearly 100% loading success and presence of titanium increased iron loading success. XPS results showed presences of TiO2 and mostly Fe2O3 forms.

La2O3 modified silica-pillared clays supported PtOx nanocrystalline catalysts for catalytic combustion of benzene

La2O3 modified silica-pillared clays (SPC) was synthesized by a soft template method. Both the basal spacing and the specific surface area increased after pillaring and modification, and the thermal stability was also improved, all of which could reduce the mass transfer resistance and improve the adsorption capacity of benzene. PtOx nanocrystalline catalysts were prepared by a high-temperature liquid reduction method. Among them, the catalyst with 0.2 wt% Pt loading and a La/KSF molar ratio of 0.5:1 (0.2% Pt/LaSPC (0.5:1)) showed the highest catalytic combustion activity and higher CO2 selectivity, and the reaction temperature for benzene combustion was about 200 °C. Besides, the Pt0, Pt2+ and Pt4+ with particle sizes of about 3–5 nm coexisted on the surface of LaSPC (0.5:1). And this catalyst also exhibited good stability during the 100 h continuous reactions at 195 °C. The high dispersion of Pt particles, active oxygen species and strong redox property are responsible for the high activity of 0.2% Pt/LaSPC (0.5:1) for benzene combustion.

Silica Pillared Montmorillonites as Possible Adsorbents of Antibiotics from Water Media

In this work, three silica pillared clays (Si-PILC) were synthetized, characterized, and evaluated as possible adsorbents of ciprofloxacin (CPX) and tetracycline (TC) form alkaline aqueous media. The pillared clays obtained showed significant increases in their specific surface areas (SBET) and micropore volumes (Vμp) regarding the raw material, resulting in microporosity percentages higher than 57% in all materials. The studies of CPX and TC removal using pillared clays were compared with the natural clay and showed that the Si-PILC adsorption capacities have a strong relationship with their porous structures. The highest adsorption capacities were obtained for CPX on Si-PILC due to the lower molecular size of CPX respect to the TC molecule, favoring the interaction between the CPX− and the pillars adsorption sites. Tetracycline adsorption on silica pillared clays evidenced that for this molecule the porous structure limits the interaction between the TCH− and the pillars, decreasing their adsorption capacities. However, the results obtained for both antibiotics suggested that their negative species interact with adsorption sites on the pillared structure by adsorption mechanisms that involve inner-sphere complex formation as well as van der Waals interactions. The adsorption mechanism proposed for the anionic species on Si-PILC could be considered mainly as negative cooperative phenomena where firstly there is a hydrophobic effect followed by other interactions, such as der Waals or inner-sphere complex formation.

Mesoporous silica-pillared clays supported nanosized Co3O4-CeO2 for catalytic combustion of toluene

Mesoporous silica-pillared clay (SPC) was synthesized by a soft template method. Compared with the raw montmorillonite (MMT), the basal spacing of SPC increased from 0.96 to 2.61 nm, the specific surface area increased from 30 to 453 m2/g, and the thermal stability was also improved, all of which could reduce the mass transfer resistance and improve the adsorption capacity of toluene. SPC supported Co3O4 and rare earth (Y, La, Ce, Pr and Nd) nano-composite catalysts were prepared by a deposition-precipitation method. Among them, 10% Co-5% Ce/SPC displayed the highest catalytic combustion activity, and the reaction temperature for toluene combustion was about 200 °C (98% conversion). This catalyst displayed good durability, and conversion of toluene dropped slightly from 96% to 90% in 1000 h continuous reaction at 190 °C. Co3O4 and CeO2 had particle sizes of 5–8 nm and were dispersed homogeneously on the surface of SPC. Introduction of CeO2 enhanced oxygen storage/transport capacity, and improved the dispersion of Co3O4 on SPC. The interaction of Co3O4-CeO2 and SPC, the co-existence of Co2+/Co3+ and the higher concentration of Ce3+ ions on the catalyst surface contribute to the high catalytic oxidative activity of 10% Co-5% Ce/SPC for toluene combustion.

Selective cyclohexane oxidation over vanadium incorporated silica pillared clay catalysts: The effect of VOx content and dispersion

The design of efficient and stable clay based materials for catalytic technologies is a great challenge. We demonstrated a new approach of fabricating vanadium incorporated silica-pillared clay by interlayered self-assembly synthetic route. And such synthetic route utilized tartaric acid as the complexing reagent, both dodecyl dimethyl benzyl ammonium bromide and octadecylamine as the mixed structure-directing agent. The obtained vanadium-containned silica-pillared clay samples were characterized by X-ray fluorescence, X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption isotherms, Fourier-transform infrared spectroscopy, diffuse reflectance ultraviolet–visible spectroscopy and X-ray photoelectron spectroscopy techniques. Characterization results indicate that there is an important correlation between the concentration of octadecylamine and uniform structure of the obtained vanadium-containned sample. The octadecylamine is not only used as swelling agency but also decreases the polarity to confirm the uniform mesoporous structure form in the interlayered regions. It was generally considered that hydrothermal synthesis bears the advantage of incorporating active metal ions into the framework in the tetrahedral coordination with V4+ state under the combined action of complexing reagent and mixed structure-directing agent. And the V2O5 phase was gradually formed via aggregation and agglomeration of increasing highly dispersed vanadium species. The catalytic behaviour and performance was examined using the selective oxidation of cyclohexane. The obtained catalyst possesses larger surface area and mesoporous volume and uniform slit-shaped mesopores, which are beneficial to the diffusion of the vanadium atom and responsible for higher yield of the KA oil. And the mechanism associated with the porous structure change has also been discussed.

Mesoporous Al-incorporated silica-pillared clay interlayer materials for catalytic hydroxyalkylation of phenol to bisphenol F

Mesoporous Al-incorporated silica-pillared clay interlayer materials for catalytic hydroxyalkylation of phenol to bisphenol F.

Facile synthetic route to Fe3O4/silica nanocomposites pillared clay through cationic surfactant-aliphatic acid mixed system and application for magnetically controlled drug release

The clay minerals have received considerable attention because of their environmental compatibility, low cost, high selectivity, reusability and operational simplicity. This article describes a new synthetic route to magnetic silica-pillared clay (SPC) composites through cationic surfactant-aliphatic acid mixed system method. The magnetic nanoparticles generated onto the silica-pillared clay host is mainly composed of Fe3O4, and such self-assembly process of SiO2–Fe3O4 magnetic nanoparticles occurs in the interlayered regions of layered clay. The formed magnetic silica-pillared clay keeps the ordered layered structure and uniform gallery pore size. The effect of varying added Fe source and oleic acid on the synthetic process has been studied experimentally. The results indicate that oleic acid plays a key role in Fe3O4 dispersion. The formed organic (C18H35COO)3Fe and (C18H35COO)2Fe could homogeneously dispersed in the intercalated compounds and formed C18H35COONH4 cooperating with cationic surfactants effects ordered and stable interlayered mixed micelles. Such process ensures the interlayered nano-sized magnetic particles formed with high dispersion and ordered mesoporous structure conserved. The in vitro drug release rate of the magnetic SPC loading ibuprofen was also studied on detail. Under an external magnetic field of 0.15 T, the drug release rate of the magnetic SPC composites decreases dramatically owing to the aggregation of the magnetic SPC composites' particles triggered by non-contact magnetic force. Additionally, the obtained magnetic SPC has a strong magnetization response, implying the possibility of application in magnetic drug targeting.

Restructuring of silica-pillared clay (SPC) through posthydrothermal treatment and application as phosphotungstic acid supports for cyclohexene oxidation

A facile posthydrothermal treated process has been successfully established for restructuring of silica-pillared clay. This approach involves the hydrothermal treated process utilizing octadecylamine as structural agency followed by calcination at high temperatures. The formation of expanded interlayered mesopores is a result of treatment with octadecylamine hydrothermal conditions. The following calcination at higher temperatures gives silica-pillared clay larger pore volume and conserved high surface area. The kind of pore expansion process has been confirmed by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 adsorption–desorption isotherms and transmission electron microscopy (TEM). The pore expansion mechanism of silica-pillared clay is proposed. The pore expanded silica-pillared clay has been used as the catalytic supports for H3PW12O40 loading as high as 26.9%, 35.8% and 48.2% for oxidation reaction of cyclohexene using H2O2 as oxidant. The stable charge force between H3PW12O40 and negative charged clay layers, together with big and open porous structure, large pore volume, and high loading of H3PW12O40 contributes to the efficiency conversion, high selectivity toward cyclohexene epoxide and brilliant reusability.

Nickel nanoparticles highly dispersed in silica pillared clay as an efficient catalyst for chlorobenzene dechlorination

A series of highly dispersed nickel nanoparticles (with a uniform size of 4.7 nm) between the lamellae of silica pillared clay was synthesized, which exhibit high catalytic performance for the hydrodechlorination of chlorobenzene.

Oxidation of Cyclohexene over Mesoporous Silica Pillared Clay Incorporated with Heteropoly Acid Prepared by Sol Gel Method

Mesoporous silica pillared clay (SPC) materials with different contents of H4PMo11VO40 (PVMo) heteropoly acid were synthesized by introducingPVMo into clay interlayer template in an acidic suspension using sol–gel method. The results of the characterizations showed that PVMo was dispersed homogeneously in the encapsulated samples. The encapsulated materials exhibited good catalytic performance in oxidation of cyclohexene.

Synthesis of magnetic FexOy@silica-pillared clay (SPC) composites via a novel sol–gel route for controlled drug release and targeting

Novel magnetic silica-pillared clay (SPC) materials with an ordered interlayered mesopore structure were synthesized via a two-step method including gallery molecular self-assembly and sol–gel magnetic functionalization, resulting in the formation of FexOy@SPC composites. Small-angle XRD, TEM and N2 adsorption–desorption isotherms results show that these composites conserved a regular layered and ordered mesoporous structure after the formation of FexOy nanoparticles. Wide-angle XRD and XPS analyses confirmed that the FexOy generated in these mesoporous silica-pillared clay hosts is mainly composed of γ-Fe2O3. Magnetic measurements reveal that these composites with different γ-Fe2O3 loading amounts possess super-paramagnetic properties at 300K, and the saturation magnetization increases with increasing Fe ratio loaded. Compared to the pure SPC, the in vitro drug release rate of the FexOy@SPC composites was enhanced due to the fact that the intensities of the SiOH bands on the pore surface of SPC decrease after the generation of FexOy. However, under an external magnetic field of 0.15T, the drug release rate of the FexOy@SPC composites decreases dramatically owing to the aggregation of the magnetic FexOy@SPC particles triggered by non-contact magnetic force. The obtained FexOy@SPC composites imply the possibility of application in magnetic drug targeting.

Synthesis of titania modified silica-pillared clay (SPC) with highly ordered interlayered mesoporous structure for removing toxic metal ion Cr(VI) from aqueous state

Titanium-functionalized silica-pillared clays synthesized through post synthetic route was utilized as adsorbers for the removal of Cr(VI) ions from aqueous solutions under different temperatures and initial concentrations. The starting mesostructured silica-pillared clay is assembled by intragallery ammonia-catalyzed hydrolysis of tetraethoxysilane using cationic surfactant as gallery template, and subsequently, the formed interlayered pore walls were decorated with nano-sized TiO2 particle through organic titanium functionalization process. The kind of structural transformation has been confirmed by X-ray diffraction (XRD), nitrogen adsorption–desorption isotherms, Fourier transform infrared (FT-IR) analysis, UV–vis diffuse reflectance spectroscopy (DRS), elemental analysis (XRF), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Such results indicate that most of the grafted titanium species was combined with Si–OH on the surface of gallery pores. By changing the concentration of organic titanium source during synthesis, the porous structure system is effected. Under suitable conditions, these materials exhibit high adsorption capacity and efficiency. Qualitative estimates of the thermodynamic parameters showed that the overall adsorption process is spontaneous (ΔG°<0) and endothermic (ΔH°>0). The adsorption isotherms of Cr(VI) on titanium-functionalized silica-pillared clay were best fitted by Redlich–Peterson models. Detail results of thermodynamics and kinetics are also presented.

Fabrication of magnetic silica-pillared clay (SPC) nanocomposites with ordered interlayer mesoporous structure for controlled drug release

Magnetic silica-pillared clay with ordered layered structure and uniform gallery pore size distribution were synthesized by generating magnetic Fe3O4 nanoparticles onto the mesoporous silica-pillared clay hosts using molecular self-assembly method. The obtained magnetic silica-pillared clay samples have been characterized by elemental analysis (XRF), powder X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 adsorption–desorption isotherms, Fourier transform infrared (FT-IR) spectra, X-ray photoelectron spectrometer (XPS) and transmission electron microscopy (TEM). Such results indicate that the formed magnetic silica-pillared clay keeps the ordered layered structure and uniform gallery pore size, and the magnetic nanoparticles generated onto the silica-pillared clay host is mainly composed of Fe3O4. Magnetic measurements reveal that these composites possess super paramagnetic properties at 300K, and the saturation magnetization increases with increasing Fe ratio loaded. These magnetic silica-pillared clays show sustained release profiles with acetylsalicylic acid as the model drug. The magnetic silica-pillared clay samples show higher release rate with respect to the general silica-pillared clay.

Synthesis of mesoporous iron-incorporated silica-pillared clay and catalytic performance for phenol hydroxylation

Fe-incorporated silica-pillared clays (Fe-SPCs) with ordered interlayer mesoporous structure have been synthesized through a new two-step procedure including the modification of the silica nano-pillars with potassium ferricyanide (K3Fe(CN)6) and successive calcination. X-ray diffraction, nitrogen adsorption–desorption, Fourier transform infrared spectra, X-ray fluorescence analyses, diffuse reflectance UV–vis spectra and X-ray absorption near-edge structure spectra were used to characterize the structures and the synthesizing mechanism of Fe-SPCs. Results show that all iron species were tetrahedrally coordinated with the interlayer silica nano-pillars, and the cationic surfactant molecule plays an important role in the intercalation of tetraethoxysilane and the introduction of iron into the intragallery silica framework. Moreover, the structural parameters of Fe-SPC can be adjusted by controlling the concentration of K3Fe(CN)6, as the concentration of K3Fe(CN)6 increases from 1M to 2M, the gallery height of Fe-SPC increases from 2.51 to 2.66nm, while the Brunauer–Emmett–Teller (BET) surface area, pore volume and Barrett–Joyner–Halenda (BJH) pore size decrease from 856 to 794m2/g, 0.75 to 0.69cm3/g, and 2.2 to 2.0nm, respectively. The Fe-SPCs show good catalytic activity in phenol hydroxylation using H2O2 as oxidant (phenol:H2O2=1:1, water), specifically, the phenol conversion is 46.2%, and the selectivity of dihydroxybenzenes is 70.6% at 343K.