Search Results (8)

For industrial CO₂ utilization, the supply of concentrated CO₂ within a continuous, high-volume stream at high temperatures remains a substantial requirement. Membrane processes offer a simple and efficient method to provide CO₂ in this form. While several organo-silica-based membranes have been developed for CO₂/N₂ separation under these conditions, there is no standardized framework guiding comparability and optimization. Therefore, we present these membranes in a Robeson-like plot across various temperatures. Utilizing a standard 1,2-bis(triethoxysilyl)-ethane (BTESE) precursor and a simplified sol–gel method, we prepared a microporous membrane layer and characterized it for an exemplary comparison. This characterization includes key parameters for mixed-gas applications: (1) temperature-dependent single- and mixed-gas permeances to observe interactions, (2) the impact of the driving forces in mixtures (vacuum and concentration) to distinguish between permselectivity and the separation factor clearly, and (3) influence of the support structure to enable permeability calculations at elevated temperatures. Furthermore, a quick interpretation method for assessing the membrane’s microstructure is presented. A qualitative microstructure assessment can be achieved by analyzing the temperature dependencies of the three major diffusion mechanisms that simultaneously occur—Knudsen, surface, and activated diffusion. Full article

Hydrotalcite exhibits the capability to adsorb CO₂ at elevated temperatures. High surface area and favorable coating properties are essential to harness its potential for practical applications. Stable alcohol-based dispersions are needed for thin film applications of mixed membranes containing hydrotalcite. Currently, producing such dispersions without the need for delamination and dispersing agents is a challenging task. This work introduces, for the first time, a manufacturing approach to overcoming the drawbacks mentioned above. It includes a synthesis of hydrotalcite nanoparticles, followed by agent-free delamination of their layers and final dispersion into alcohol without dispersing agents. Further, the hydrotalcite-derived sorption agent is dispersed in a matrix based on organo-silica gels derived from 1,2-bis(triethoxysilyl)ethane (BTESE). The analytical results indicate that the interconnection between hydrotalcite and BTESE-derived gel occurs via forming a strong hydrogen bonding system between the interlayer species (OH groups, CO₃²⁻) of hydrotalcite and oxygen and silanol active gel centers. These findings lay the foundation for applications involving incorporating hydrotalcite-like compounds into silica matrices, ultimately enabling the development of materials with exceptional mass transfer properties. In part 2 of this study, the gas separation performance of the organo-silica and the hydrotalcite-like materials and their combined form will be investigated. Full article

The separation ability of bis(triethoxysilyl)ethane (BTESE) membranes for hydrogen (H₂) purification from hydrogen (H₂)/toluene (TOL) gas mixtures after a methylcyclohexane (MCH) dehydrogenation process was investigated via one-stage and two-stage membrane processes. This study revealed that BTESE membranes of varied pore sizes (0.4, 0.5, and 0.7 nm) in a one-stage configuration can manage to achieve a H₂ purity ~99.9%. However, the TOL concentrations fell within a wide range, ranging from 280 to 5441 ppm. A primary goal of this research was to lower the TOL concentration in the permeate stream below 200 ppm. Hence, by applying the two-stage membrane, it was demonstrated that the TOL concentration in the permeate stream could be lowered below 200 ppm. Full article

New polysilsesquioxane (PSQ)-based CO₂ separation membranes with succinic anhydride and monoalkylurea units as thermally degradable CO₂-philic units were prepared by the copolymerization of a 1:1 mixture of [3-(triethoxysilyl)propyl]succinic anhydride (TESPS) or [3-(triethoxysilyl)propyl]urea (TESPU) and bis(triethoxysilyl)ethane (BTESE). The succinic anhydride and monoalkylurea units underwent thermal degradation to form ester and dialkylurea units, respectively, with the liberation of small molecules (e.g., CO₂ and NH₃) under N₂ atmosphere. The effects of thermal degradation on the performance of the obtained membranes were investigated. The TESPS-BTESE- and TESPU-BTESE-based membranes calcined at 250 °C and 200 °C exhibited good CO₂/N₂ permselectivities of 20.2 and 14.4, respectively, with CO₂ permeances of 7.7 × 10⁻⁸ and 7.9 × 10⁻⁸ mol m⁻²·s⁻¹·Pa⁻¹, respectively. When the membranes were further calcined at elevated temperatures of 350 °C and 300 °C, respectively, to promote the thermal degradation of the organic units, the CO₂ permeances increased to 1.3 × 10⁻⁷ and 1.2 × 10⁻⁶ mol m⁻²·s⁻¹·Pa⁻¹ (3.9 × 10² and 3.6 × 10³ GPU), although the CO₂/N₂ permselectivities decreased to 19.5 and 8.4, respectively. These data indicate that the controlled thermal degradation of the organic units provides a new methodology for possible tuning of the CO₂ separation performance of PSQ membranes. Full article

A 40 cm length Bis(triethoxysilyl)ethane (BTESE) membrane having different pore sizes was successfully prepared by changing the number of coating times for gas permeation (GP) and organic solvent reverse osmosis (OSRO) separation study. It was found that BTESE-6 membranes prepared through six-time coating consisted of small-sized pores in the range 0.56 to 0.64 nm estimated using modified Gas Translation (mGT) method and 0.59 to 0.67 nm estimated by nanopermporometry (NPP) method, respectively. These membranes demonstrated a high DMF rejection, R_DMF > 95% with total flux, J_{v total} > 5 kg m⁻² h⁻¹ at operating condition feed pressure, P_f: 8 MPa; feed temperature, T_f : 50 °C; and feed flowrate, Q_f : 30 mL/min; and they exhibited a high degree selectivity of He/SF₆ in the range of ~ 260–3400 at a permeation temperature 200 °C. On the other hand, the larger pore sizes of the BTESE-4 membranes (pore size estimates > 0.76 nm to 1.02 nm) exhibited low DMF rejection and a low degree selectivity of He/SF₆ around ~30% and 25, respectively, at the same operating condition as BTESE-6. Both GT and NPP methods can be considered as an indicator of the measurement membrane pore size. From this study, it was found that He and SF₆ gases can be some of the potential predictors for water and DMF permeance. Furthermore, by comparing our OSRO membrane with other PV membranes for DMF/H₂O separation, our BTESE-6 membranes still exhibited high flux in the range of 3–6 kg m⁻² h⁻¹ with a separation factor H₂O/DMF in the range of 80–120. Full article

A new polyhedral oligomeric silsesquioxane (POSS) designed with eight –(CH₂)₃–NH–(CH₂)₂–NH₂ groups (PNEN) at its apexes was used as nanocomposite uploading into 1,2-bis(triethoxysilyl)ethane (BTESE)-derived organosilica to prepare mixed matrix membranes (MMMs) for gas separation. The mixtures of BTESE-PNEN were uniform with particle size of around 31 nm, which is larger than that of pure BTESE sols. The characterization of thermogravimetric (TG) and gas permeance indicates good thermal stability. A similar amine-contained material of 3-aminopropyltriethoxysilane (APTES) was doped into BTESE to prepare hybrid membranes through a copolymerized strategy as comparison. The pore size of the BTESE-PNEN membrane evaluated through a modified gas-translation model was larger than that of the BTESE-APTES hybrid membrane at the same concentration of additions, which resulted in different separation performance. The low values of E_p(CO₂)-E_p(N₂) and E_p(N₂) for the BTESE-PNEN membrane at a low concentration of PNEN were close to those of copolymerized BTESE-APTES-related hybrid membranes, which illustrates a potential CO₂ separation performance by using a mixed matrix membrane strategy with multiple amine POSS as particles. Full article

Microporous organosilica membranes based on 1,2-bis(triethoxylsilyl)ethane (BTESE) were fabricated via an acid-catalyzed sol-gel technique. In the preparation process, the calcination temperature plays a significant role in structural and surface properties of the organosilica networks. With an increase in calcination temperature, the surface hydrophilicity decreased due to the enhanced condensation of Si-OH groups in the networks. N₂ adsorption results suggest that the pore structures of BTESE membranes was clearly dependent on the calcination temperature. The pore sizes of the membranes were quantitatively determined by using the Normalized Knudsen-based permeance (NKP) model. In pervaporation tests, the membranes with higher calcination temperatures showed higher salt rejections and lower water permeances, which was attributed to the changes in pore size and surface chemistry of pore walls. The BTESE membranes calcined at 200 °C exhibited superior hydrothermal stability in temperature cycles up to 70 °C and high reproducibility in concentration cycles with NaCl concentrations of 0.2–13 wt%, showing great promise for desalination applications of high-salinity water. Full article

Solvents purification mainly used in pharmaceutical field such as acetone and methyl ethyl ketone (MEK) were performed through hybrid silica membranes and from binary and multi-components mixtures. Two hybrid silica membranes—zirconia doped bis(triethoxysilyl)methane and bis(triethoxysilyl)ethane (BTESE)—were studied. Flux, permeance, and separation factor were evaluated depending on temperature, composition, and number of organic compounds in the feed. Dehydration tests of acetone were operated at 30 and 45 °C following by acetone and MEK purification at 50 °C from multi-components hydro-organic mixtures where hydrophilic compounds (water, methanol) but also hydrophobic (dichloromethane (DCM) and/or toluene) were present. Results showed that the presence of Zr nanoparticles affected flux and improved selectivity in the case of dehydration. Experiments related to acetone and MEK purification, revealed a mass transfer alteration and a decrease of performance, from 99 to 97 wt% and from 98 to 95 wt% respectively, when the number of compounds in the initial feed grown up and more precisely, in the presence of DCM and toluene thus highlighting a possible coupling effect. Full article