One-pot Hydrothermal Synthesis Research Articles

One-Pot Synthesis of Mixed-Phase MoVTeNbOx Catalysts for Selective Oxidation of Propane to Acrylic Acid.

One-pot hydrothermal synthesis assisted by sodium citrate and citric acid is developed to fabricate mixed-phased MoVTeNbOx catalysts with different phase compositions for selective oxidation of propane to acrylic acid. Structures of various catalysts are comprehensively characterized. Interfacial interactions occur among the M1 and M2 phases of mixed-phase MoVTeNbOx catalysts to exert synergistic effects on the selective production of acrylic acid. Various mixed-phase MoVTeNbOx catalysts exhibit the same type of active site on the M1-phase component, with a significantly enhanced ability to adsorb and activate propane. The propane conversion increases linearly with the density of surface site for propane adsorption, while the propene selectivity increases linearly with the density of surface site for propene adsorption. Among the synthesized catalysts, a MoVTeNbOx catalyst composed of 35.3 wt % M1 phase, 19.2 wt % M2 phase, and 45.7 wt % amorphous phase exhibits the largest density of active site and consequently the best catalytic performance with 38.9% propane conversion and 71.2% acrylic acid selectivity at 380 °C.

Novel fluorescent carbon dots derived from shikimic acid for ultra-high sensitive detection and efficient removal of sulfasalazine

The extensive use of sulfasalazine (SSZ) poses potential threats to human health and ecosystems. Therefore, sensitive detection and simultaneous efficient removal of sulfasalazine is greatly desirable. Meanwhile, shikimic acid, a natural product obtained from Chinese star anise is a promising precursor for carbon dots construction due to its unique structure. Taking the above into account, in this work, novel fluorescent carbon dots (SA-CDs) for sensitive detection and highly efficient removal of sulfasalazine have been developed. SA-CDs were facilely obtained from shikimic acid by using one-pot hydrothermal synthesis. The structure and composition of SA-CDs were fully characterized with TEM, PXRD, FT-IR, DLS and XPS tests. Strong fluorescent emission centered at 428 nm was recorded for SA-CDs, enabling the detection of SSZ. Quantitatively speaking, SA-CDs can selectively detection SSZ amount 17 antibiotics with an experimental limit of detection (LOD) of 100 nM and a calculated LOD of 60 pM. Adsorption experiments suggested that chemical monolayer adsorption predominates in the adsorption process, with a maximum adsorption capacity of 22.67 mg/g. Aggregations formed during detection enable the simultaneous removal of SSZ upon centrifugation. Moreover, SA-CDs have been successfully applied to the detection of SSZ in real samples, including river water, soil, tea and eggs.

Mandarin Peels-Derived Carbon Dots: A Multifaceted Fluorescent Probe for Cu(II) Detection in Tap and Drinking Water Samples.

Carbon dots (CDs) derived from mandarin peel biochar (MBC) at different pyrolysis temperatures (200, 400, 600, and 800 °C) have been synthesized and characterized. This high-value transformation of waste materials into fluorescent nanoprobes for environmental monitoring represents a step forward towards a circular economy. In this itinerary, CDs produced via one-pot hydrothermal synthesis were utilized for the detection of copper (II) ions. The study looked at the spectroscopic features of biochar-derived CDs. The selectivity of CDs obtained from biochar following carbonization at 400 °C (MBC400-CDs towards various heavy metal ions resulted in considerable fluorescence quenching with copper (II) ions, showcasing their potential as selective detectors. Transmission electron microscopic (TEM) analysis validated the MBC-CDs' consistent spherical shape, with a particle size of <3 nm. The Plackett-Burman Design (PBD) was used to study three elements that influence the F0/F ratio, with the best ratio obtained with a pH of 10, for 10 min, and an aqueous reaction medium. Cu (II) was detected over a dynamic range of 4.9-197.5 μM and limit of detection (LOD) of 0.01 μM. Validation testing proved the accuracy and precision for evaluating tap and mountain waters with great selectivity and no interference from coexisting metal ions.

One-pot hydrothermal synthesis of 3D garland BiOI, spherical ZnO, and CNFs onto Ni foam: Supercapacitor performance with enhanced electrochemical properties

This study reported one-pot hydrothermal synthesis of 3D garland BiOI, spherical ZnO, and carbon nanofibers (CNFs) onto Ni foam substrate with improved supercapacitor performance and enhanced electrochemical properties. The synthesized nanocomposites exhibited high specific capacitance (SC) of 1073 g−1 at a current density of 1 A/g and excellent cycling stability with 88.6% retention of original capacity after 5000 cycles in 2M KOH aqueous solution. The findings highlight the potential of 3D materials for use as electrode materials in advanced supercapacitor applications due to their high energy storage capabilities.

Facile construction of a novel dual Z-scheme mixed phases BiFeO3 heterojunction: For peroxymonosulfate activation toward efficient photodegradation of 4-nitrophenol and mechanistic insights

This study proposes a novel approach for preparing bismuth ferrite (BiFeO3, BFO) with controlled crystal phase purity and morphology via a one-pot hydrothermal process using specific mineralizers (NaOH or KOH). The effects of these mineralizers on the crystal purity and photocatalytic efficiency of the catalyst were investigated. The XRD results revealed that KOH produced pure BFO, whereas NaOH yielded mixed-phase BFO (m-BFO) with secondary phases, including Bi2O3 and Bi2Fe4O9. SEM analysis revealed that m-BFO exhibited a flake-like structure assembled into cubes, whereas pure BFO consisted of irregularly shaped agglomerated nanoparticles. The photocatalytic efficiency of the two catalysts was evaluated for the degradation of 4-nitrophenol (4-NP). The results showed that m-BFO exhibited outstanding photocatalytic degradation performance (92%) for 4-NP compared with pure BFO (22%). The enhanced photocatalytic efficiency of m-BFO was attributed to the construction of a dual-heterojunction Z-scheme within its structure and the presence of abundant surface oxygen vacancies. This study provides valuable insights into the synthesis of efficient dual-heterojunction Z-scheme photocatalysts via one-pot hydrothermal synthesis.

One-pot hydrothermal synthesis of g-C3N4/BiOBr/Bi2MoO6 as a Z-scheme heterojunction for efficient photocatalytic degradation of ciprofloxacin (CIP) antibiotic and Rhodamine B (RhB) dye

Photocatalytic degradation of toxic organic pollutants using natural sunlight is a rapidly advancing area of research, particularly involving binary or ternary component photocatalysts with Z-type heterojunctions. In this study, ternary g-C3N4/BiOBr/Bi2MoO6 photocatalysts were fabricated using a simple one-pot solvothermal method. The morphology and physicochemical properties of the samples were characterized using various techniques, including X-ray diffraction analysis (XRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS), confirming the presence of BiOBr, Bi2MoO6, and g-C3N4 components. The inclusion of g-C3N4 increased the BET surface area of the composite up to 46 m2/g, compared with BiOBr. In addition, g-C3N4 also enhanced the light absorption capability of the composite into the visible light range, while BiOBr and Bi2MoO6 significantly improved separation of electron-hole pairs, as evidenced by photoluminescence (PL) intensity. Under visible light illumination (LED lamp), the prepared photocatalyst showed high efficiency, achieving 94 % degradation of ciprofloxacin (CIP) antibiotic in 180 min and 92 % degradation of Rhodamine B (RhB) dye in 240 min. Moreover, under natural sunlight irradiation, the photocatalyst achieved degradation efficiencies of approximately 91 % for CIP and 100 % for RhB within 180 minutes. The photodegradation of the pollutants followed first-order kinetics with a Z-scheme type heterojunction. The photogenerated electrons played a crucial role as the main active species involved in detoxification of the organic contaminants. The photocatalyst exhibited excellent structural stability and good cycling ability, maintaining its original photocatalytic performance even after five cycles of use. This work demonstrates a promising strategy for developing sunlight-active ternary heterojunctions for environmental remediation.

Photothermal synergistic catalytic oxidation mechanism of toluene by Ce-doped SrTiO3 via one-pot hydrothermal synthesis

Industrial volatile organic compounds (VOCs) emissions pose significant environmental and human health risks, with photothermal catalysis degradation emerging as a promising VOCs treatment technology. The light response range and catalysis degradation efficiency of photocatalysts, however, need to be improved. This study prepared Ce-doped SrTiO3 perovskite catalysts via a one-pot hydrothermal method. The synergistic photic/thermal degradation mechanism of toluene was uncovered via XPS, Uv–Vis, EPR, and in-situ DRIFTS analysis. It was found that the toluene removal rate and CO2 yield reached their maximums at 200 °C, reaching 95 % and 90 %, respectively, at a Ce doping ratio of 50 %. During the catalytic process, the prerequisite to trigger toluene oxidation, and light promote the generation of reactive oxygen species (·OH and ·O2–), which facilitates the formation of intermediates and thus accelerates the deep oxidation of toluene. The doped Ce increases surface oxygen vacancies while lowering the energy band gap of the catalyst, facilitating the separation of holes and photogenerated electrons. Furthermore, in situ DRIFTS studies demonstrated that toluene undergoes a ring-opening process, producing intermediates such as benzaldehyde and benzoic acid. This study will assist in promoting the use of photothermal synergistic catalytic degradation technology to remove VOCs from industrial sources.

N2O Decomposition on Singly and Doubly (K and Li)-Doped Co3O4 Nanocubes─Establishing Key Factors Governing Redox Behavior of Catalysts.

The intimate mechanism of N2O decomposition on bare and redox-tuned Co3O4 nanocubes (achieved by single (Li or K) and double (Li and K) doping) was elucidated. The catalysts synthesized by the hydrothermal method were characterized by X-ray electron absorption fine structure measurements, X-ray diffraction, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy, and Kelvin Probe techniques. TPSR and steady-state isothermal catalytic tests reveal that the N2O turnover frequencies are critically sensitive to the work function of the catalysts, adjusted purposely by doping. For the catalysts obtained by one-pot hydrothermal synthesis, lithiation of the Co3O4 nanocubes leads to the formation of {Li'8a, Co·16d} species, decreasing steadily the work function and the activity, while for the catalysts prepared by postsynthesis impregnation, formation of {Li'8a, Co'16d, Co··16c} species leads to a volcano-type dependence of the catalytic activity and the work function in parallel. The beneficial effect of potassium was discussed in terms of mitigation of surface potential buildup due to the accumulation of ionosorbed oxygen intermediates (surface electrostatics), which hinders the interfacial electron transfer. Analysis of the catalytic activity response to the redox tuning of Co3O4, substantiated by DFT calculations, allowed for a straightforward conceptualization of the redox nature of the N2O decomposition in terms of the lineup of frontier orbitals of the N2O/N2O- and O2-/O2 reactants with the surface DOS structure and the resultant molecular orbital interactions. The positions of the virtual bonding 3πg0(N2O)-α-3dz2 and the occupied 2πg1(O2-)-α-3dz2 states relative to the Fermi energy level play a crucial role in the regulation of the forward and backward interfacial electron transfer events, which drive the redox process.

Green synthesis of CoVS2-MOF@CMS nanocomposite electrode for sustainable approach towards eco-friendly energy storage and dopamine detection

Dopamine, a crucial brain chemical belonging to the catecholamine and phenethylamine chemical families, plays a vital role in promoting a healthy and happy life. Irregular dopamine release has been linked to various neurological disorders and depressive conditions. Therefore, conducting real-time, in vivo monitoring of dopamine levels is essential to gain a comprehensive understanding of its physiological functions. In this research, the hydrothermal technique was employed to synthesize copper‑molybdenum sulfide (Cu2MoS4 (CMS)). Further, we have reported the one-pot hydrothermal synthesis of CoVS2-MOF, using the bioactive chemical as fuel obtained from Euphorbia cognata Boiss. The specific capacity (Qs) of the sample CoVS2-MOF@CMS was calculated to be 820 Cg−1 at 3 mVs−1, a value expressively higher than that of the reference samples. Furthermore, in the supercapattery device, an outstanding Qs of 300 Cg−1 was achieved at 1.5 Ag−1, surpassing the previously observed values. The device demonstrated outstanding performance, including a coulombic efficiency of 89 %, a specific energy of 36.68 Whkg−1, and a power density (Pd) of 2218.53 Wkg−1. Moreover, the sensor typically yielded dopamine (DA) concentrations in human serum ranging from 100.8 % to 102.2 %. The utilization of the multifunctional CoVS2-MOF@CMS nanocomposite electrode material illustrates promising prospects for the fabrication of hybrid devices with applications in biomedical and energy harvesting fields.

Porous Structure Fibers Based on Multi-Element Heterogeneous Components for Optimized Electromagnetic Wave Absorption and Self-Anticorrosion Performance.

The excellent performance of electromagnetic wave absorbers primarily depends on the coordination among components and the rational design of the structure. In this study, a series of porous fibers with carbon nanotubes uniformly distributed in the shape of pine leaves are prepared through electrospinning technique, one-pot hydrothermal synthesis, and high-temperature catalysis method. The impedance matching of the nanofibers with a porous structure is optimized by incorporating melamine into the spinning solution, as it undergoes gas decomposition during high-temperature calcination. Moreover, the electronic structure can be modulated by controlling the NH4F content in the hydrothermal synthesis process. Ultimately, the Ni/Co/CrN/CNTs-CF specimen (P3C NiCrN12) exhibited superior performance, while achieving a minimum reflection loss (RLmin) of -56.18dB at a thickness of 2.2mm and a maximum absorption bandwidth (EABmax) of 5.76GHz at a thickness of 2.1mm. This study presents an innovative approach to fabricating lightweight, thin materials with exceptional absorption properties and wide bandwidth by optimizing the three key factors influencing electromagnetic wave absorption performance.

A one-pot hydrothermal synthesis of morphologically controllable yolk-shell structured CoFe glycerate spheres for oxygen evolution reaction

CoFe-based catalysts are efficient electrocatalysts for the oxygen evolution reaction (OER) in alkaline media. Here, we present a simple one-pot hydrothermal method for synthesizing a series of CoFe glycerates with controllable surface morphologies and investigate their potential as highly efficient catalysts for the OER in alkaline media. These CoFe glycerates exhibit a unique yolk-shell microsphere structure assembled from ultrathin nanosheets. The adjustment of the surface nanosheet size is achieved by varying the CoFe ratio, ensuring a more efficient electrocatalytic system for the OER process. Due to the abundant active sites provided by the yolk-shell structure and interleaved ultrathin nanosheets, Co3Fe1 glycerate (Co3Fe1 gly) demonstrates a low overpotential (283 mV) and a small Tafel slope (44.61 mV dec−1) at 10 mA cm−2. Additionally, Co3Fe1 gly exhibits excellent durability in alkaline electrolytes. Moreover, a series of characterizations demonstrate that the active sites of Co3Fe1 gly are the high-valence Co species generated during the OER process. This study opens a promising avenue for utilizing efficient and low-cost electrocatalysts to enhance OER performance.

Fabrication of iron manganese oxide-reduced graphene oxide nanocomposite: A highly effective synergistic electrocatalyst for sensitive metronidazole detection

Efficient 2D-inorganic spinel perovskites nanostructure materials are used as potential candidates for highly sensitive detection of harmful substances present in the environment. In this regard, a facile one-pot hydrothermal synthesis was employed to fabricate nanocomposite material containing iron manganese oxide (FeMn2O4) decorated with reduced graphene oxide (rGO) which is used as an electrochemical detection of metronidazole (MTZ). The crystalline nature and structural insights of the as-synthesized FeMn2O4-rGO nanocomposite were established using various spectroscopic and electrochemical techniques. Distinctively FeMn2O4-rGO nanocomposite fashioned glassy carbon electrode (GCE) showed excellent linear range (0.01–512.2 μM), sensitivity (71.4 μA mM−1 cm−2), limit of detection (0.0129 μM), reproducibility, stability and resist-interference capability towards metronidazole (MTZ) antibiotic drug. In addition, the fabricated FeMn2O4-rGO/GCE electrochemical sensor exhibited a remarkable MTZ detection in spiked water as well as urine samples with better recovery percentages supporting its facile and feasible nature for environmental applications. The present work established the fabrication of FeMn2O4-rGO/GCE nanocomposite for effective determination of antibiotic drugs in real sample analysis.

One-pot hydrothermal synthesis of transition metal sulfides-decorated CuS microflower-like structures for electrochemical CO2 reduction to CO

Electrochemical CO2 reduction (ECR) to value-added products is regarded as a sustainable strategy to mitigate global warming and energy crisis, and designing highly efficient and robust catalysts is essential. In this work, transition metal sulfides (TMS)-decorated CuS microflower-like structures were prepared via the one-pot hydrothermal synthesis method for ECR to CO, and the influence of TMS doping on ECR performance was demonstrated. Characterization of the catalysts was performed using XRD, FESEM-EDS, N2 physisorption, and XPS, revealing the successful loading of TMS, the formation of microflower-like architectures and the generation of sulfur vacancies. Electrochemical tests demonstrated that doping ZnS, Bi2S3, CdS and MoS2 improved the intrinsic CO2 reduction activity of the CuS catalyst. Particularly, the MoS2-CuS composite catalyst with imperfect petal-like structure showed uniform distribution of edge Mo sites, which worked synergistically with the formed grain boundaries (GBs) and undercoordinated S vacancy sites in promoting CO2 activation, stabilizing *COOH adsorption, facilitating *CO desorption, and lowering the energy barrier of the potential-limiting step for improved CO selectivity. The MoS2-CuS catalyst achieved a maximum CO selectivity of 83.2% at –0.6 V versus the reversible hydrogen electrode (RHE) and a high CO cathodic energetic efficiency of 100%. At this potential, the catalyst maintained stable catalytic activity and CO selectivity during a 333-min electrolysis process. The findings will offer a promising avenue for the development of efficient and stable catalysts for CO production from ECR.

Zinc cations incorporated in Silicalite-1 zeolite assist in anchoring atomically dispersed platinum catalyst for boosted and robust propane dehydrogenation

The utilization of Pt-based catalysts in the catalytic conversion of propane to propylene (PDH) remains pivotal in industrial processes. However, the scarcity of Pt and its high cost necessitates innovative strategies to enhance Pt dispersion and catalytic performance. In this study, we present an approach involving the in-situ incorporation of Zn cations into Silicalite-1 (S-1) zeolite through one-pot hydrothermal synthesis, which facilitates the anchoring of atomically dispersed Pt atoms. The synthesized 0.5Pt/Zn@S-1 catalyst exhibits the dehydrogenation performance of 25 % propane for approximately 34.2 % propane conversion and 95.1 % propylene selectivity (propylene turnover rate of 14.2 s−1), coupled with robust stability of up to 60 h without distinct deactivation under a WHSV of 49.1 h−1. Comprehensive characterizations reveal the formation of atomically dispersed Pt-Zn catalytic sites. The Pt atoms are incorporated with the Zn cations and dense silanol nests. This unique configuration facilitates a synergistic effect between Pt and Zn for dehydrogenation.

One-pot hydrothermal synthesis of silicon, nitrogen co-doped carbon dots for enhancing enzyme activity of acid phosphatase (ACP) to dopamine and for cell imaging

Developing water-soluble nanomaterials with high photoluminescence emission and high yield for biological analysis and imaging is urgently needed. Herein, water-soluble blue emitting silicon and nitrogen co-doped carbon dots (abbreviated as Si-CDs) of a high photoluminescence quantum yield of 80 % were effectively prepared with high yield rate (59.1 %) via one-step hydrothermal treatment of N-[3-(trimethoxysilyl)propyl]ethylenediamine (DAMO) and trans-aconitic acid. Furthermore, the Si-CDs demonstrate environmental robustness, photo-stability and biocompatibility. Given the importance of the potentially abnormal levels of acid phosphatase (ACP) in cancer diagnosis, developing a reliable and sensitive ACP measurement method is of significance for clinical research. The Si-CDs unexpectedly promote the catalytic oxidation of ACP on dopamine (DA) to polydopamine under acidic conditions through the produced reactive oxygen species (ROS). Correspondingly, a fluorescence response strategy using Si-CDs as the dual functions of probes and promoting enzyme activity of ACP on catalyzing DA was constructed to sensitively determine ACP. The quantitative analysis of ACP displayed a linear range of 0.1–60 U/L with a detection limit of 0.056 U/L. The accurate detection of ACP was successfully achieved in human serum through recovery tests. As a satisfactory fluorescent probe, Si-CDs were successfully applied to fluorescent imaging of A549 cells in cytoplasmic with long-term and safe staining. The Si-CDs have the dual properties of outstanding fluorescent probes and auxiliary oxidase activity, indicating their great potential in multifunctional applications.

One-pot Hydrothermal Synthesis of Bifunctional Co/Mo-rGO efficient Electrocatalyst for HER/OER in Water Splitting

One-pot Hydrothermal Synthesis of Bifunctional Co/Mo-rGO efficient Electrocatalyst for HER/OER in Water Splitting

IrSn Bimetallic Clusters Confined in MFI Zeolites for CO Selective Catalytic Reduction of NOx in the Presence of Excess O2.

We developed a simple strategy for preparing IrSn bimetallic clusters encapsulated in pure silicon zeolites via a one-pot hydrothermal synthesis by using diethylamine as a stabilizing agent. A series of investigations verified that metal species have been confined successfully in the inner of MFI zeolites. IrSn bimetallic cluster catalysts were efficient for the CO selective catalytic reduction of NOx in the presence of excess O2. Furthermore, the 13CO temperature-programmed surface reaction results demonstrated that NO2 and N2O could form when most of the CO was transformed into CO2 and that Sn modification could passivate CO oxidation on the IrSn bimetallic clusters, leading to more reductants that could be used for NOx reduction at high temperatures. Furthermore, SO2 can also influence the NOx conversion by inhibiting the oxidation of CO. This study provides a new strategy for preparing efficient environmental catalysts with a high dispersion of metal species.

A one-pot hydrothermal synthesis of Bi/Bi2O2CO3/Bi2WO6 catalyst with enhanced photocatalytic activity to tetracycline

BackgroundThe abuse and irrational discharge of tetracycline (TC) have threatened the surroundings of human beings. Semiconductor photocatalytic oxidation technology is an emerging green environmental remediation technology, which can be widely applied in wastewater treatment. MethodsThis work is the first attempt to prepare Z-scheme heterojunction Bi/Bi2O2CO3/Bi2WO6 ternary material through one-step hydrothermal synthesis method. Significant findingsAbout 95.5 % tetracycline (10 mg·L−1) have been degraded by Bi/Bi2O2CO3/Bi2WO6 ternary material after 120 min of simulated sunlight exposure. The degradation efficiency of TC was 2.04 and 3.01 times than those of Bi2WO6 and Bi2O2CO3, respectively. Radical trapping experiments and ESR analysis showed that h+, ·O2−, and ·OH played a joint role in the degradation of tetracycline. Based on liquid chromatography-mass spectrometry analysis, energy band analysis and theoretical calculations, the degradation mechanisms were identified. The excellence photocatalytic activity is mainly attributed to two aspects: (1) The generation of Z-scheme heterojunctions provided channels for carrier transfer, accelerated interface charge separation and suppressed the rapid recombination of photo generated carriers and holes; (2) The surface plasmon resonance effect of metallic Bi intensifies photon absorption and boost photocatalytic activity. This work offers a viable method for improving the photocatalytic activity of semiconductors made of bismuth on antibiotics.

Towards an agglomeration free Ca(OH)2/CaO thermochemical energy storage loop via nanofabricated hollow CaO microspheres with highly porous shells

The Ca(OH)₂/CaO loop offers a promising solution for seasonal thermochemical heat storage, vital for decarbonizing the heating sector thanks to its high energy density and abundant raw materials. However, cyclic hydration/dehydration of limestone-derived CaO (r-CaO) faces challenges like agglomeration and high-volume expansion, limiting its expected performances. This study focuses on fabricating hollow CaO microspheres (h-CaO) with porous shells via a facile one-pot hydrothermal synthesis method, without doping materials. These microspheres exhibit superior cyclic performance compared to r-CaO, with SEM-EDS confirming successful fabrication. Over 30 cycles in the temperature range of 400–550 °C, h-CaO achieves an average storage density of 1755 kJ/kg, peaking at 1835 kJ/kg, with kinetics twice as high as r-CaO. Most importantly, the hollow microstructure reduces dramatically the apparent volumetric expansion from 250 % to as little as 32 %, offering a potential solution to agglomeration at the reactor level and advan44cing the commercial viability of the Ca(OH)2/CaO thermochemical storage technology.

Preparation of Fe-HMOR with a Preferential Iron Location in the 12-MR Channels for Dimethyl Ether Carbonylation.

As the Brønsted acid sites in the 8-membered ring (8-MR) of mordenite (MOR) are reported to be the active center for dimethyl ether (DME) carbonylation reaction, it is of great importance to selectively increase the Brønsted acid amount in the 8-MR. Herein, a series of Fe-HMOR was prepared through one-pot hydrothermal synthesis by adding the EDTA-Fe complex into the gel. By combining XRD, FTIR, UV-Vis, Raman and XPS, it was found that the Fe atoms selectively substituted for the Al atoms in the 12-MR channels because of the large size of the EDTA-Fe complex. The NH3-TPD and Py-IR results showed that with the increase in Fe addition from Fe/Si = 0 to 0.02, the Brønsted acid sites derived from Si-OH-Al in the 8-MR first increased and then decreased, with the maximum at Fe/Si = 0.01. The Fe-modified MOR with Fe/Si = 0.01 showed the highest activity in DME carbonylation, which was three times that of HMOR. The TG/DTG results indicated that the carbon deposition and heavy coke formation in the spent Fe-HMOR catalysts were inhibited due to Fe addition. This work provides a practical way to design a catalyst with enhanced catalytic performance.