Hydrothermal Conditions Research Articles

Electron Structure of α‐, β‐Te2MoO7 and Photocatalytic Decomposition of Antibiotics

AbstractTwo modifications of Te2MoO7 oxide have been prepared by different synthetic methods. The crystal structure and composition have been studied by X‐ray diffraction analysis and X‐ray microanalysis. The phase of α‐Te2MoO7 has been synthesized by solid‐state reaction from ammonium salts and characterized by monoclinic structure with P21/c. The β‐Te2MoO7 compound has been formed in hydrothermal conditions and has amorphous nature. The thermal behavior of β‐Te2MoO7 modification is characterized by the phase transition into α‐form, however after melting the amorphous state has restored. The electron structure has been investigated experimentally by X‐ray photoelectron spectroscopy and UV‐vis diffusion reflectance spectra and theoretically by approximation using atomic electronegativity. Despite the same composition, the band gap of β‐Te2MoO7 corresponds to visible light, whereas α‐Te2MoO7 adsorbs light in UV region. The both modifications are able to generate superoxide radicals in vacuum or air and hydroxyl radicals in water under irradiation. The HPLC‐MS analysis has shown the quite deep decomposition of dye and antibiotics by α‐Te2MoO7, whereas amorphous phase almost does not lead to any oxidation.

Hydrothermal carbonization of sugar beet pulp: optimization and characterization

AbstractIn this study, the optimum hydrothermal conditions of sugar beet pulp were investigated by Response Surface Methodology (RSM) based on Central Composite Design (CCD). The hydrochar obtained from sugar beet pulp (SBP) was optimized for maximum yield and carbon content. Process conditions were chosen with reaction temperatures of 200–240 °C, residence time 60–150 min, and biomass to water ratio of 1:3–1:10. The yield and carbon content of the hydrochar varied with the process parameters. In order to obtain hydrochar with the highest yield and carbon content in optimization, the reaction temperature should be 220.74 °C, the biomass to water ratio should be 1:3, and the residence time should be 95.58 min. High heating value, energy and mass yield, and energy densification ratio of sugar beet pulp and hydrochar were also investigated. The products were characterized using FT-IR, SEM, and ultimate analysis techniques. The Coats-Redfern method was used to estimate the kinetic parameters of the combustion processes. The activation energy values of SBP and SBP-HC products were calculated as 13.88 and 11.46 kJ/mol, respectively. The kinetic data were used to determine the thermodynamic parameters (ΔH, ΔG, and ΔS). As a result, the properties of hydrochar produced from sugar beet pulp under optimum conditions have been extensively investigated and the results have shown that hydrochar has potential for use in different areas.

One-Pot Synthesis of Ce-SSZ-39 Zeolite with Performance in the NH3-SCR Reaction.

Cu-SSZ-39 zeolite with 8-membered rings is regarded as a very promising catalyst in the NH3-SCR reaction, but its hydrothermal stability still remains to be improved. One of the solutions to promote hydrothermal stability is the insertion of rare earth elements in the product. Nevertheless, normal ion exchange of rare earth elements limits their contents in the zeolite product due to their large hydrated ionic radius and alkaline environment under hydrothermal conditions. Herein, we for the first time present a new method for the one-pot synthesis of Ce-SSZ-39 zeolite under solvent-free conditions. The key to success is the use of Ce-FAU zeolite as a precursor. The obtained product shows good crystallinity, sheet-like morphology, large BET surface area, and 4-coordinated Al species. Detailed investigations illustrate that Ce species in the Cu/Ce-SSZ-39 zeolite micropore can prevent the dealumination and thus formation of CuAlOx species during hydrothermal aging at 850 °C for 16 h, giving the excellent hydrothermal stability and thus showing the excellent catalytic performance in the NH3-SCR reaction. One-pot synthesis of Ce-SSZ-39 zeolite with excellent catalytic performance might open a new door for developing very efficient selective catalytic reduction (SCR) catalysts in near future.

Metastable microporous lanthanide silicates – Light emitters capable of 3D-2D-3D transformations

The synthesis of zeolites and porous heteropolyhedral silicates is usually accompanied by crystal phase transformations. Typically, this process is irreversible and characterized by a conversion from a metastable phase to a stable one. Here we demonstrate a reversible transformation between porous (K3LnSi3O9·nH2O) and layered (K3LnSi3O8(OH)2) structures exemplified by a dual synthesis (hydrothermal and solid-state transformation). We discuss structural and photoluminescent properties of the obtained microporous lanthanide silicates MS-4 (Minho-Sofia, solid number 4; K3LnSi3O9·nH2O, Ln = Y, Dy; orthorhombic, Pmc21). These materials are metastable, transforming from 3D porous to a 2D layered structure after prolonged crystallization time at hydrothermal conditions and returning to the same but distorted (≈ 2 % smaller lattice volume) porous 3D framework by calcination of 2D structure. The mechanism of 3D-2D structure transformation is driven by interzeolite-like transformation, while the rearrangement of common structural fragments controls 2D-to-3D conversion. We also show how the avoidance of Dy and preference for Y ions during MS-4 hydrothermal synthesis may be overcome by a 2D-3D conversion, allowing the production of white light emitters with controllable photoluminescence.

Preparation of anion‐uptake powder compact containing layered double oxide and metakaolinite

AbstractA powder compact with anion‐uptake ability was prepared prior to the proceeding of the solid‐state reaction involving layered double hydroxide (LDH) and kaolinite during calcination. LDH features anion‐exchangeable capability, and kaolinite is used as a raw potty material because of the sintering property. In the present study, the solid‐state reaction of LDH with kaolinite did not proceed at 750°C, resulting in the formation of a mixture of layered double oxide (LDO) and metakaolinite. Unlike LDO, which typically undergoes anion‐uptake accompanied by LDH reconstruction, metakaolinite does not revert to kaolinite without the use of hydrothermal conditions. In addition, the powder compact composed of LDO crumbled, whereas the one containing a mixture of LDO and metakaolinite remained intact. When the powder compact of LDO and metakaolinite mixture was immersed in a methyl orange (MO) aqueous solution, an LDH–MO intercalation compound was generated within the compact. By contrast, no such compound was generated when LDO powder was immersed in an MO aqueous solution. These results indicated that the successful preparation of a powder compact with distinct anion‐uptake ability was different from powder, owing to that the solid‐state reaction of LDO with metakaolinite did not proceed at 750°C.

Unlocking Enhanced Electrochemical Performance of MBene-MoB Through Controlled Aluminum Dissipation from MoAlB.

2D transition metal borides, known as MBenes, have attracted considerable attention due to their exceptional properties. This study explores the feasibility of aluminum (Al) etching from MoAlB using environmentally friendly and sustainable fluoride-free dilute acidic/alkaline solutions at room temperature, revealing its thermodynamic and kinetic viability. Furthermore, it is found that complete removal of Al can be achieved in dilute alkaline reagent under hydrothermal conditions, yielding pristine single/few-layered MBene-MoB for the first time, while acidic solutions result in ≈33% etching rates. XRD refinement, which tracks aluminum removal from 0% to 100%, reveals transient metastable phases of MoAl1-xB (x<0.5) in the initial etching stages, evolving into relatively stable pure Mo2AlB2 structures with 50% Al deficiency, serving as a precursor to MBenes. The subsequent loss of Al results in a 2D MBene-MoB structure. DFT calculations confirm excellent conductivity for MoAlB, MoAl1-xB (x=0-1), and MBene-MoB. Remarkably, MBene-MoB exhibits superior supercapacitor performance with a 4025.60mFcm-2/201.28Fg-1 capacitance. Simulations validate rapid electrolyte diffusion in layered MBene-MoB, contributing significantly to enhanced capacitance. Additionally, in the hydrogen evolution reaction (HER), MBene-MoB demonstrates superior catalytic activity compared to the precursor MoAlB and commercial MoB. Calculations suggest the potential for enhancing HER through surface modulation, considering its suboptimal hydrogen adsorption energy.

Zeolites synthesis from phyllosilicates and their performance for CO2 adsorption.

Five phyllosilicates (kaolinite, montmorillonite, saponite, sepiolite and palygorskite) have been selected as starting materials for the synthesis of zeolites. Among them, kaolinite and montmorillonite display the lowest Si/Al molar ratio leading to aluminosilicates with high crystallinity. Thus, the hydrothermal treatment under basic conditions forms 4A zeolite when kaolinite is used as starting material while 13X zeolite is obtained when montmorillonite is used as starting material. The microporosity and CO2-adsorption capacity of the prepared zeolites are directly related to its crystallinity. Thus, in order to improve it, raw phyllosilicates were subjected to a microwave-assisted treatment to remove undesired Mg or Fe-species, which have a negative effect in the assembling of the zeolites by hydrothermal basic conditions in a second step. The highest adsorption value was 3.85mmol/g at 25°C and 760mm of Hg for Mont-A-B sample after the consecutive treatments.

Templated Growth of In2S3 in Ti3C2TX MXene with Enhanced Photocatalytic Properties

The growth of ultrathin semiconductors is advantageous for photocatalysis due to improved photophysical properties and reduced charge recombination. Along these lines, templating the growth of semiconductors in confined spaces can allow control over semiconductor growth while also conferring the properties of the template to provide composite nanomaterial hybrids. Herein, the semiconductor In2S3 is grown in the organically‐modified interlayer space of Ti3C2TX MXene, a versatile 2D material with metallic character and broadband light absorption. The growth of 1–2 nm thick layers of In2S3 in the interlayer of MXene leads to a drastic increase in photocatalytic properties and light‐induced charge generation due to decreased interfacial charge transfer resistance. Interestingly, the hydrothermal conditions of In2S3 growth lead to partial oxidation of Ti3C2TX MXene to form anatase TiO2 nanocrystals, although this effect is strongly limited by increased In2S3 precursors due to passivation of the MXene surface. MXenes serve as effective templates for the confined growth of semiconductors, emphasizing the potential of MXene as a template for 2D material heterostructures. Overall, this work further develops MXene‐based 2D material composites, offering insights into the origins of the enhanced photocatalytic and photoelectrochemical properties, toward improvements in energy production and aqueous phase catalysis.

Two new Zn(ii) coordination polymers incorporating 2-(2,6-dichlorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline: Synthesis and structure

Abstract Based on phenanthroline derivate ligand and Zn(ii), two novel coordination polymers, namely [Zn(L)(hta)] n (1) and {[Zn2(L)2(dhb)2]·H2O} n (2) (L = 2-(2,6-dichlorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, H2hta = heptanedioic acid, and H2dhb = 3,5-dinitro-2-hydroxybenzoic acid), have been synthesized under the hydrothermal condition. For 1, each hta anion bridges two Zn(ii) atoms in a tridentate mode to shape into a chain structure and through different π–π stacking interactions to form a three-dimensional supramolecular structure. The L ligand of 2 connects two neighbouring Zn(ii) atoms to give a 1D chain, which is further extended into the 2D supramolecular layer.

Eu‐based coordination polymer with fluorescence enhancement for Cu2+/prochloraz and quenching for nitrobenzene/pyrimethanil

The detection of pollutants is an important part of environmental protection. A one‐dimensional Eu(III) coordination polymer (CP1), [Eu2(3‐pyia)2(Ac)2 (H2O)4]·(2,2′‐bipy)0.5·4.25H2O, based on 5‐(pyridin‐3‐ylmethoxy) isophthalic acid (3‐H2pyia) and 2,2′‐bipyridine (2,2′‐bipy) was designed and prepared under hydrothermal condition. The structure was characterized as one‐dimensional ladder‐like structure with water and 2,2′‐bipy guest molecules. The excellent luminescence properties of CP1 prompted us to investigate its fluorescence sensing performance for pollutants. It exhibited fluorescence enhancement for Cu2+ and prochloraz, but quenching for nitrobenzene and pyrimethanil, and the fluorescence sensing mechanism has been further investigated by experimental and density functional theory (DFT) calculations. This work expands the exploitation of rare earth coordination polymers for fluorescence sensing and contributes to pollutant detection.

Effect of strip tillage widths on soil moisture, soil temperature and soil structure in northeast China

Strip tillage is an effective tillage technique, which included the strip seedbed tilled area (ST-IR) and the straw-covered area between the seedbeds (ST-BR). However, soil hydrothermal conditions and soil disturbance varies with strip tillage widths, which might affect crop growth and yields. Therefore, this study explored the effect of strip tillage width on the soil hydrothermal conditions and soil structure of ST-IR and ST-BR, to determine the optimal strip tillage width. A field experiment with three replicates was conducted to analyze soil moisture and soil temperature variation and to clarify the difference of soil structure in the IR and BR. Three strip tillage widths, 20 cm (ST20), 30 cm (ST30), and 40 cm (ST40), were examined in this study. Soil temperature in both the ST-IR and ST-BR increased as the strip tillage width increased, and the average soil temperature of ST30-IR and ST40-IR in the seedling stage was 2.11°C and 2.62°C higher than that of ST20-IR, respectively. Moreover, the daily soil temperature range in both the IR and BR was greater for ST40 than for ST20 and ST30 in the seedling stage; soil temperature differences in other crop growth stages were small. No significant difference in soil temperature was observed between ST30-IR and ST40-IR. Conversely, soil moisture was greater in ST20-IR and ST30-IR than in ST40-IR; soil moisture was also greater in ST30-BR and ST40-BR than in ST20-BR during the monitoring period. Soil moisture in ST40-IR and ST20-BR increased and decreased more rapidly during rainfall events than in the other treatments. Moreover, soil temperature was higher in the ST-IR than in the ST-BR for all 3 strip tillage widths, and the opposite results were observed for soil moisture. In addition, strip tillage widths had no significant differences on soil structure. In conclusion, a 30 cm strip tillage width had higher soil temperature and remained more soil moisture than other strip tillage widths, so this strip tillage width is thus recommended for use by farmers in Northeast China.

Fabrication of new in‐situ ternary nano/microcomposite LDH/Ag2O/Bayerite in trimetallic NiAg/Al layered double hydroxides for CO2 capture material

AbstractWe reported new in‐situ ternary nano/microcomposite layered double hydroxides/Ag2O/bayerite in trimetallic NiAg/Al layered double hydroxides (LDH) via hydrothermal technique; and characterization by powder X‐ray diffraction (XRD), Fourier transforms infrared spectroscopy (FT‐IR), field emission scanning electron microscopy (FE‐SEM), energy dispersive spectroscopy (EDS), and N2 adsorption‐desorption. The formation of bayerite and silver oxide species on the LDH nanosheet depended on the excess of Al3+ and Ag+ in the solution under alkaline and hydrothermal conditions. The nitrogen isotherm adsorption profile for all ternary composites exhibited uniformity with mesoporous and lamellar characteristics. The surface area of all the composites ranged from 81.17 to 150.23 m2. g−1, the Barret‐Joyner‐Halenda (BJH) pore volume from 0.22 to 0.27 cm3. g−1, and the average pore diameter ranged from 3.47 to 5.78 nm. All composites show a laminar plate‐like structure covered with elongated pieces. The particle size of the composites ranged from 54.86 to 115.96 nm, indicating the size changed from nano to microcomposite because of the different molar ratios of Ag and Ni in the solid. The ternary composite reveals CO2 capture activity with adsorption capacity ranging from 13.93 to 19.61 mmol g−1. © 2024 Society of Chemical Industry and John Wiley &amp; Sons, Ltd.

Chemical Textures on Rare Earth Carbonates: An Experimental Approach to Mimic the Formation of Bastnäsite

AbstractThe interaction between multi‐component rare earth element (REE) aqueous solutions and carbonate grains (dolomite, aragonite, and calcite) are studied at hydrothermal conditions (21–210 °C). The effect of ionic radii of five REEs (La, Ce, Pr, Nd, Dy) on solid formation are analyzed using two solution types: equal REE concentrations and concentrations normalized to Post Archean Australian Shale Standard (PAAS). The interaction replaces the host Ca–Mg carbonate grains with a series of REE minerals (lanthanite → kozoite → bastnäsite → cerianite). At 165 °C, equal concentration solutions promote kozoite crystallization, maintaining similar REE ratios in solids and solution. PAAS solutions result in zoned REE‐bearing crystals with heterogeneous elemental distributions and discreet REE phases (e.g., cerianite). Chemical signatures indicate metastable REE‐bearing phases transforming into more stable polymorphs, along with symplectite textures formed by adjacent phase reactions. Overall, experiments highlight the dependence of polymorph selection, crystallization pathway, mineral formation kinetics, and chemical texture on REE concentrations, ionic radii, temperature, time, and host grain solubility.

Experimental characterization and numerical prediction for mechanical aging of epoxy and its carbon fiber‐reinforced composite under hydrothermal conditions

AbstractThe Aqueous environment impairs the mechanical performance of carbon fiber‐reinforced polymers (CFRPs) and decreases the durability of engineering structures made of CFRPs primarily by degrading the resin matrix. Hence, the objective of this study is to investigate and accurately predict the influence of hydrothermal aging on the epoxy and its carbon fiber reinforced polymer (CFRP). Particularly, this work developed a modeling method that combined Fick's model, empirical aging model and elastoplastic constitutive model to predict the mechanical behavior of hydrothermally aged epoxy matrix. After the experimental characterization, this epoxy modeling method demonstrated its predictive capability on the mechanical response of the deteriorated epoxy under different hydro‐thermal‐salt conditions, with the mean absolute percent error (MAPE) of approximately 4.61%. Furthermore, the transverse compressive behavior of unidirectional (UD) CFRPs could be predicted by using the representative volume element (RVE) model with the degraded matrix behavior predicted via this epoxy modeling method. Integrated with this CFRP modeling, results from mechanical tests and fracture analysis further demonstrated that the hydrothermal aging effect on the transverse compressive performance of the UD CFRPs was dominated by the deterioration of their resin matrix. Therefore, this study demonstrates the feasibility of the finite element analysis (FEA) for mechanical aging of the epoxy matrix and its CFRP under hydrothermal conditions via employing the proposed integrated modeling method.Highlights Degradation of epoxy polymer under hydro‐thermal‐salt aging conditions. Integrated model to predict mechanical response of hydrothermally aged epoxy. RVE model to predict the mechanical behavior of hydrothermally aged CFRP. Hydrothermal aging on the transverse compressive behavior of UD CFRP.

Metal Organic Framework Derived Spinel Nickel‐Ferrites Employing Reduced Graphene Oxide Template for Supercapacitor and Photocatalytic Dye Degradation

AbstractSpinel oxides from transition metals are the most crucial components for producing supercapacitive electrodes and photocatalytic semiconductor materials. However poor electrical conductivity and restricted specific energy of these materials are two main drawbacks for energy storage applications. This investigation used reduced graphene oxide templated spinel nickel ferrites nanoparticles (RGO@SNFs), synthesized using Fe2Ni MIL‐88 MOF via hydrothermal conditions followed by a pyrolysis process. The structural properties and morphology of the hybrid are characterized through several methods, including XRD, FTIR, BET‐PSD, and FESEM. Superconducting electrochemical studies such as Galvano static charge‐discharge, impedance spectroscopy and cyclic voltammetry are carried out on a hybrid electrode to examine the impact of the RGO template on SNF nanoparticles. This electrode may be an alluring choice for supercapacitor applications because of its capacitance 115 F/g and retention rate of approximately 95 % following 2000 cycles. Additionally, a model dye degradation process utilizing Rhodamine B (RhB) was used to examine the photodegradation action of these materials. The designed catalyst also represents excellent photo‐degradation activity toward RhB, and seventy‐five minutes of sun light were enough to destroy about 99 % of the dye.

Frictional Stability of Laumontite Under Hydrothermal Conditions and Implications for Injection‐Induced Seismicity in the Gonghe Geothermal Reservoir, Northwest China

AbstractLaumontite is a common and potentially frictionally unstable hydrothermal alteration product present in deep faults of the Gonghe EGS reservoir. We characterize the friction‐stability characteristics of synthetic laumontite gouge under in situ reservoir conditions. The pure laumontite gouge is frictionally strong (μ = 0.73–0.98) and the quartz/laumontite mixture (1:1) is generally less strong (μ = 0.73–0.78) under experimental conditions (Pc = 95 MPa, T = 90–250°C, Pf = 0–90 MPa). The shear velocity was stepped between 6.1, 0.61, then 0.061 μm/s for our experiments. For both gouges, the friction coefficient is independent of temperature and increases with elevated pore pressures. The pure gouge and mixture are strongly velocity‐weakening over a broad range in temperatures (∼90–220°C) and excess pore pressures (0–90 MPa) relevant to the Gonghe stimulation. Microearthquakes (MEQs) observed during stimulation are confined to within the broad depth range of inferred frictional instability—although fluid overpressures are also limited to this region. The observation that laumontite mixtures are frictionally unstable over a broad range of pressures and especially temperatures representative of EGS reservoirs and insensitive to the presence of the coexisting mineral phase (quartz) suggests its presence is a strong indicator of potential seismic hazard.

Investigation of a liquid-mediated defect-healing treatment in zeolite beta

We report the application of a liquid-mediated defect-healing treatment based on tetraethylammonium (TEA+) hydroxide and ammonium fluoride, and variants thereof, to the H+ form of zeolite beta. Through comparison between H-beta of high (730) and lower (28.6) SiO2: Al2O3 ratios, and characterisation of the treated samples before and after calcination, insights into the interaction of TEA+ and F− with H-beta under hydrothermal conditions were gained. In general, the treatments resulted in the loss of crystallinity and the generation of relatively large mesopores in the more siliceous samples, but improvements in long-range order and the development of relatively small mesopores in the less siliceous samples. The healing of silanol defects was observed for most of the treatments. A partial mechanism is proposed to explain the action of defect-healing treatments based on pore-occupying cations and F−; fluorine may be essential in some cases because it balances the charge of the organic cations, preventing the “trapping” of silanol groups as charge-balancing silanolate groups which resist healing.

Laboratory characterization of hydrothermally processed oligopeptides in ice grains emitted by Enceladus and Europa.

The Cassini mission provided evidence for a global subsurface ocean and ongoing hydrothermal activity on Enceladus, based on results from Cassini's mass spectrometers. Laboratory simulations of hydrothermal conditions on icy moons are needed to further constrain the composition of ejected ice grains containing hydrothermally altered organic material. Here, we present results from our newly established facility to simulate the processing of ocean material within the temperature range 80-150°C and the pressure range 80-130 bar, representing conditions suggested for the water-rock interface on Enceladus. With this new facility, we investigate the hydrothermal processing of triglycine (GGG) peptide and, for the first time, analyse the extracted samples using laser-induced liquid beam ion desorption (LILBID) mass spectrometry, a laboratory analogue for impact ionization mass spectrometry of ice grains in space. We outline an approach to elucidate hydrothermally processed GGG in ice grains ejected from icy moons based on characteristic differences between GGG anion and cation mass spectra. These differences are linked to hydrothermal processing and thus provide a fingerprint of hydrothermal activity on extraterrestrial bodies. These results will serve as important guidelines for biosignatures potentially obtained by a future Enceladus mission and the SUrface Dust Analyzer (SUDA) instrument onboard Europa Clipper. This article is part of the theme issue 'Dust in the Solar System and beyond'.

Study on the Synthesis of Nano Zinc Oxide Particles under Supercritical Hydrothermal Conditions.

The supercritical hydrothermal synthesis of nanomaterials has gained significant attention due to its straightforward operation and the excellent performance of the resulting products. In this study, the supercritical hydrothermal method was used with Zn(CH3COO)2·2H2O as the precursor and deionized water and ethanol as the solvent. Nano-ZnO was synthesized under different reaction temperatures (300~500 °C), reaction times (5~15 min), reaction pressures (22~30 MPa), precursor concentrations (0.1~0.5 mol/L), and ratios of precursor to organic solvent (C2H5OH) (2:1~1:4). The effects of synthesis conditions on the morphology and size of ZnO were studied. It was found that properly increasing hydrothermal temperature and pressure and extending the hydrothermal time are conducive to the more regular morphology and smaller size of ZnO particles, which is mainly achieved through the change of reaction conditions affecting the hydrothermal reaction rate. Moreover, the addition of ethanol makes the morphology of nano-zno more regular and significantly inhibits the agglomeration phenomenon. In addition to the change in physical properties of the solvent, this may also be related to the chemical bond established between ethanol and ZnO. The results show that the optimum synthesis conditions of ZnO are 450 °C, 26 MPa, 0.3 mol/L, 10 min, and the molar ratio of precursor to ethanol is 1:3.

Synthesis, structure and photoluminescence properties of heterometallic-based coordination polymers of trimesic acid.

Reacting trimesic acid (H3TMA, C9H6O6) with CaCl2 and MCl2 at 110 °C under hydrothermal conditions gave the isostructural heterobimetallic coordination polymers (CPs) catena-poly[[tetraaquazinc(II)]-μ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-μ-5-carboxybenzene-1,3-dicarboxylato], [CaZn(HTMA)2(H2O)8]n, 1, and catena-poly[[tetraaquacobalt(II)]-μ-5-carboxybenzene-1,3-dicarboxylato-[tetraaquacalcium(II)]-μ-5-carboxybenzene-1,3-dicarboxylato], [CaCo(HTMA)2(H2O)8]n, 2. Compounds 1 and 2 crystallize in the monoclinic space group C2/c. The solid-state structures consist of eight-coordinate CaII ions and six-coordinate MII ions. These ions are connected by a doubly deprotonated HTMA2- ligand to create a one-dimensional (1D) zigzag chain. Poly[[decaaquabis(μ3-benzene-1,3,5-tricarboxylato)calcium(II)dizinc(II)] dihydrate], {[CaZn2(TMA)2(H2O)10]·2H2O}n, 3, was found incidentally as a minor by-product during the synthesis of 1 at a temperature of 140 °C. It forms crystals in the orthorhombic space group Ccce. The structure of 3 consists of a two-dimensional (2D) layer composed of [Zn(TMA)] chains that are interconnected by CaII ions. The presence of aromatic carboxylic acid ligands and water molecules, which can form numerous hydrogen bonds and π-π interactions, increases the stability of the three-dimensional (3D) supramolecular architecture of these CPs. Compounds 1 and 2 exhibit thermal stability up to 420 °C, as indicated by the thermogravimetric analysis (TGA) curves. The powder X-ray diffraction (PXRD) data reveal the formation of unidentified phases in methanol and dimethyl sulfoxide, while 1 exhibits chemical stability in a wide range of solvents. The luminescence properties of 1 dispersed in various low molecular weight organic solvents was also examined. The results demonstrate excellent selectivity, sensitivity and recyclability for detecting acetone molecules in aqueous media. Additionally, a possible sensing mechanism is also outlined.