Transferring polypropylene into carbon nanotubes via combustion of PP/zeolites (H‐ZSM‐5 or H‐beta)/Ni2O3

In a simple device, two kinds of zeolites were successfully used as synergistic additive to promote formation of the multi‐walled carbon nanotubes (MWNTs) from polypropylene (PP) via combustion. More importantly, this kind of process may potentially act as a new approach for recycling plastic wastes, because it could effectively transfer polyolefin wastes into valuable carbon materials. Experimental results demonstrated that the higher quality of MWNTs can be obtained from the mixture (PP/H‐Beta/Ni₂O₃) than that from the mixture (PP/H‐ZSM‐5/Ni₂O₃). At the same time, the yield of MWNTs from PP/H‐ZSM‐5/Ni₂O₃ system is much lower than that from PP/H‐Beta/Ni₂O₃ under the same condition. The reason for the different effects of both types of zeolites on the morphology and the yield of the MWNTs was analyzed. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Synthesis and characterization of novel core‐shell magnetic nanogels based on 2‐acrylamido‐2‐methylpropane sulfonic acid in aqueous media

Ultrafine well‐dispersed Fe₃O₄ magnetic nanoparticles were directly prepared in aqueous solution using controlled coprecipitation method. The synthesis of Fe₃O₄/poly (2‐acrylamido‐2‐methylpropane sulfonic acid) (PAMPS), Fe₃O₄/poly (acrylamide‐co‐2‐acrylamido‐2‐methylpropane sulfonic acid) poly(AM‐co‐AMPS) and Fe₃O₄/poly (acrylic acid‐co‐2‐acrylamido‐2‐methylpropane sulfonic acid) poly(AA‐co‐AMPS) ‐core/shell nanogels are reported. The nanogels were prepared via crosslinking copolymerization of 2‐acrylamido‐2‐methylpropane sulfonic acid, acrylamide and acrylic acid monomers in the presence of Fe₃O₄ nanoparticles, N,N′‐methylenebisacrylamide (MBA) as a crosslinker, N,N,N′,N′‐tetramethylethylenediamine (TEMED) and potassium peroxydisulfate (KPS) as redox initiator system. The results of FTIR and ¹H‐NMR spectra indicated that the compositions of the prepared nanogels are consistent with the designed structure. X‐ray powder diffraction (XRD) and transmission electron microscope (TEM) measurements were used to determine the size of both magnetite and stabilized polymer coated magnetite nanoparticles. The data showed that the mean particle size of synthesized magnetite (Fe₃O₄) nanoparticles was about 10 nm. The diameter of the stabilized polymer coated Fe₃O₄ nanogels ranged from 50 to 250 nm based on polymer type. TEM micrographs proved that nanogels possess the spherical morphology before and after swelling. These nanogels exhibited pH‐induced phase transition due to protonation of AMPS copolymer chains. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Experimental study on the solvent regeneration of a CO2‐loaded MEA solution using single and hybrid solid acid catalysts

The performance of a hybrid solid acid catalyst consisting of a physical mixture of γ‐Al₂O₃ and H‐ZSM‐5 in terms of the rate and heat duty for solvent regeneration (i.e., CO₂ stripping) of a CO₂‐rich MEA solution was compared with the individual performance of γ‐Al₂O₃, H‐ZSM‐5, and H‐Y solid acid catalysts using MEA (2–7 mol/L), with initial CO₂ loading of 0.5 mol CO₂/mol MEA at 378 K. It was observed that any catalyst significantly decreased the energy required for CO₂ regeneration. The performance of the catalysts investigated ranked as follows: γ‐Al₂O₃/H‐ZSM‐5 = 2/1 > γ‐Al₂O₃ > H‐ZSM‐5 > H‐Y if the process is in the lean CO₂ loading region whereas it was H‐ZSM‐5 > γ‐Al₂O₃/H‐ZSM‐5 = 2/1 > γ‐Al₂O₃ > H‐Y if the process is in the rich CO₂ loading region. These results highlight the joint dependence on Brønsted/Lewis acidity and mesopore surface area of heat duty for solvent regeneration. © 2015 American Institute of Chemical Engineers AIChE J, 62: 753–765, 2016     

Mesoporous H‐ZSM‐5 for the Conversion of Dimethyl Ether to Hydrocarbons

The potential of hierarchical H‐ZSM‐5 zeolites was studied for the conversion of DME to fuel‐compatible hydrocarbons. For this purpose, hierarchical H‐ZSM‐5 zeolites have been prepared from commercial H‐ZSM‐5 by desilication and organosilane‐directed hydrothermal synthesis. The zeolites were characterized by X‐ray diffraction, NH₃‐TPD, DRIFTS, and N₂ physisorption measurements. The catalysts have been tested in a tube reactor (1 bar, 648 K). The results indicate important structural changes in framework and acidic sites, which are significant for the synthesis of gasoline‐range hydrocarbons.     

P2O5‐Fe2O3‐CaO‐SiO2 ferromagnetic glass‐ceramics for hyperthermia

Ferromagnetic glass‐ceramics are an important kind of thermoseed material for hyperthermia treatments. In order to investigate the applications of glass‐ceramics in magnetic hyperthermia, P₂O₅‐Fe₂O₃‐CaO‐SiO₂ (PFCS) glass‐ceramics with different compositions were prepared by the sol‐gel method. The crystal phase, magnetic properties, induction heating ability, and cytotoxicity of the as‐prepared glass‐ceramics were investigated. The results show that all the samples exhibit low cytotoxicity and good induction heating ability. Moreover, it was found that the phosphorus content affected the crystal phase component of the sample, and thus influenced the induction heating ability. Results of the magnetic hyperthermia experiments showed that the PFCS glass‐ceramic samples induced significant cell death of the LoVo cancer cells. The highest cell death rate for sample B2P7 was more than 95%, which suggests good application prospects in the field of hyperthermia therapy.     

Synthesis of ZSM‐5 by hydrothermal method with pre‐mixing in a stirred‐tank reactor

This work proposed a synthesis route of ZSM‐5 via the hydrothermal method with premixing in a stirred tank reactor (STR). Effects of various operating conditions, including pre‐mixing time, molar ratio of SiO₂/Al₂O₃, TPAOH (organic template agents) concentration, NaCl (alkali metal cations) concentration, crystallization temperature, and crystallization reaction time, on the average particle size (PS) and particle size distribution (PSD) were investigated. It was found that the pre‐mixing time in the STR significantly affect the formation of proto‐nuclei in premixing process and crystal growth in hydrothermal reaction process, and consequently influence the PS and PSD of the prepared ZSM‐5. ZSM‐5 with good thermal stability, a PS of 380 nm, PSD of 0.17–0.9 µm, pore diameter of 2.31 nm, pore volume of 0.19 cm³ · g^?1 and specific surface area of 337.25 m² · g^?1 were obtained under the optimal conditions of a crystallization reaction time of 24 h, a crystallization temperature of 130 °C, a molar ratio of SiO₂/Al₂O₃ of 200, a TPAOH concentration of 3.5 mol · L^?1, NaCl concentration of 0.3 mol · L^?1, and a pre‐mixing time of 5 h. This work indicated that the operating conditions including premixing time have a significant effect on its PS and PSD.     

Ethanol perm‐selective B‐ZSM‐5 zeolite membranes from dilute solutions

Boron‐substituted MFI (B‐ZSM‐5) zeolite membranes with high pervaporation (PV) performance were prepared onto seeded inexpensive macroporous α‐Al₂O₃ supports from dilute solution and explored for the separation of ethanol/water mixtures by PV. The effects of several parameters on microstructures and PV performance of the B‐ZSM‐5 membranes were examined systematically, including the seed size, synthesis temperature, crystallization time, B/Si ratio, H₂O/SiO₂ ratio and silica source. A continuous and compact B‐ZSM‐5 membrane was fabricated from solution containing 1 tetraethyl orthosilicate/0.2 tetrapropylammonium hydroxide/0.06 boric acid/600 H₂O at 448 K for 24 h, showing a separation factor of 55 and a flux of 2.6 kg/m² h along with high reproducibility for a 5 wt % ethanol/water mixture at 333 K. It was demonstrated that the incorporation of boron into mobile five (MFI) structure could increase the hydrophobicity of B‐ZSM‐5 membrane evidenced by the improved contact angle and amount of the adsorbed ethanol, and thus enhance the PV property for ethanol/water mixtures. © 2016 American Institute of Chemical Engineers AIChE J, 62: 2447–2458, 2016     

Low Temperature Synthesis of Needle‐like α‐FeOOH and Their Conversion into α‐Fe2O3 Nanorods for Humidity Sensing Application

In this study, we report template and surfactant‐free, low temperature (70°C) synthesis of needle‐like α‐FeOOH and its conversion at 400°C into α‐Fe₂O₃ nanorods using Fe(+2) and Fe(+3) chlorides and urea as a hydrolysis‐controlling agent. The isolated needle‐like α‐FeOOH indicates asparagus‐type growth pattern having length ca. 600 nm with 80 nm diameter at base and apex diameter of around 10 nm. The sample on heating (α‐Fe₂O₃) shows nanorod‐like morphology. The samples were characterized using various physicochemical characterization techniques such as XRD, Raman spectroscopy, UV‐Vis spectroscopy, particle size distribution analysis, Field Emission Scanning Electron Microscopy (FE‐SEM), and humidity sensing performance. The humidity sensing behavior of both α‐FeOOH and α‐Fe₂O₃ was studied. The α‐FeOOH shows quicker (10 s) and higher response toward change in humidity from 20%RH to 90%RH as compared with α‐Fe₂O₃ (60 s). Their typical morphology and crystalline structure plays an important role in humidity sensing behavior.     

High performance ZSM‐5 membranes on coarse macroporous α‐Al2O3 supports for dehydration of alcohols

High‐performance ZSM‐5 membranes with a low Si/Al ratio of 10.3 were prepared on cheap coarse macroporous α‐Al₂O₃ tubes by fluoride route without organic template. The effects of crystallization time and aluminum source on the growth, morphology and pervaporation (PV) performances of the as‐synthesized membranes were investigated. The feasibility of preparing ZSM‐5 membranes with different Si/Al ratio which was implemented by using different Al₂(SO₄)₃·18H₂O content in synthesis gel were discussed. It was found that the aluminum source had significant effect on the synthesis of membranes. The ZSM‐5 membranes prepared by using Al₂(SO₄)₃·18H₂O as an aluminum source from synthetic gel with composition of 1SiO₂/0.05Al₂O₃/0.17Na₂O/0.9NaF/45H₂O showed high reproducibility and high PV performance with flux of 3.85 kg/(m²·h) and separation factor of higher than 10,000 in dehydration of 90 wt % i‐PrOH/H₂O at 348 K. Moreover, the ZSM‐5 membranes exhibited high water perm‐selectivity performance for dehydration of 90 wt % n‐PrOH/H₂O, n‐BtOH/H₂O, and i‐BtOH/H₂O mixtures, respectively. © 2016 American Institute of Chemical Engineers AIChE J, 62: 2813–2824, 2016     

Synthesis of modified catalyst and stabilization of CuO/NH4‐ZSM‐5 for conversion of methanol to gasoline

In this article, the catalytic conversion of methanol to gasoline range hydrocarbons has been studied over CuO/ NH₄‐ZSM‐5(3,5,7,9%) catalysts prepared via sono‐chemistry methods. In order to improve, copper oxide can be used as a booster on NH₄‐ZSM‐5 this catalyst property. Accordingly, the conversion process of Methanol to Gasoline (MTG) was conducted under a pressure of 1 atm and temperature of 400°C by a fixed‐bed reactor on copper oxide catalysts which were prepared based on synthetic NH₄‐ZSM‐5. The synthetic catalyst was investigated by such analyses as BET, XRD, FT‐IR, and SEM. Formation of copper oxide phase and proper distribution of copper oxide were proven on the basic level of using XRD analysis. BET analysis showed the reduction in catalyst level and SEM images depicted the proper distribution of particles. The present investigation is to study the effect of CuO loading on NH4‐ZSM‐5 support for conversion of methanol to gasoline range hydrocarbons. A series of CuO/ NH4‐ZSM‐5 catalysts were prepared, characterized, and experimented for their performance on methanol conversion and hydrocarbon yield.     

The effect of Fe2+ state in electrical property variations of Sn‐doped hematite powders

The structural, electrical, and chemical properties of Sn‐doped Fe₂O₃ powders were investigated. Various quantities of Sn‐doped Fe₂O₃ powders were synthesized using solid‐state reactions. Rietveld analysis for the powders that were doped below 2% revealed a phase‐pure Sn‐doped Fe₂O₃ structure (i.e., identical to Fe₂O₃ structure). Alternatively, the analysis for the powders that were doped more than 3% exhibited secondary phase. The unit cell volume and electrical conductivity of the phase‐pure samples increased with an increase in the doping concentration. X‐ray photoelectron spectroscopy measurements showed an increased Fe²⁺ state with the increase in Sn doping concentration. Therefore, the improved electrical conductivity and unit cell volume with the increase in doping concentration of the phase‐pure powders might be related to the increased Fe²⁺ state.     

Design of an X‐Ray Powder Diffraction Probe for Multi‐Channel Application: Proof of Principle

The design of an X‐ray powder diffraction probe and its integration with a multi‐channel reactor system for potential application in high‐throughput experimentation is presented. The working principle of the apparatus is exemplified by measurements of corundum and of the phase change observed when oxidizing vanadium(III) oxide (V₂O₃) in air during heating up to 450 °C. The phase transformations of the parent material were monitored by phase identification of the crystalline intermediate vanadium(IV) oxide (VO₂) and the final product vanadium(V) oxide (V₂O₅).     

Synthesis,structure, and thermo‐physical properties of Fe2O3.Al2O3 and polyethylene nanocomposites

In this study, Fe₂O₃.Al₂O₃/polyethylene composites were prepared using a two‐step process. In the first step, PE is synthesized using titanium based metallocene catalyst system. While the synthesized PE was subsequently purified, hydrated alumina filled PE (MHFP) composites was formed by the hydrolysis of methylaluminoxane (MAO). In the second step, Fe₂O₃.Al₂O₃/PE was prepared via thermal decomposition of ferric formate in a high temperature solution of MHFP composite. The structure, morphology, and thermal properties of the composites were characterized using the XRD, FTIR, SEM‐EDX, TGA, and DSC analytical techniques. Results showed that the incorporation of a suitable amount of Fe₂O₃.Al₂O₃ into the composites enhances the thermal stability. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Preparation and Characterization of Fe2O3/Ammonium Perchlorate (AP) Nanocomposites through Ceramic Membrane Anti‐Solvent Crystallization

A novel ceramic membrane anti‐solvent crystallization (CMASC) method was proposed to prepare Fe₂O₃/AP nanocomposites with core‐shell structure. For the preparation of Fe₂O₃/AP nanocomposites, several key advantages of the CMASC method are as follows. Firstly, both well‐dispersed Fe₂O₃ nanoparticles and the superfine AP preparation can be achieved at one step. Secondly, no non‐component of solid propellant was involved in this composite process. Thirdly, the size and morphology of Fe₂O₃/AP nanocomposites can be effectively controlled by using the ceramic membrane with regular pore structure as feeding template. The morphology and structure of Fe₂O₃/AP nanocomposites were characterized by inductively coupled plasma spectrophotometry (ICP), IR spectroscopy, SEM, and HRTEM. The results verified that the size and morphology of Fe₂O₃/AP nanocomposites are controllable, and the dispersion of Fe₂O₃ nanoparticles is greatly improved in Fe₂O₃/AP nanocomposites. Moreover, the thermal decomposition of the as‐prepared Fe₂O₃/AP nanocomposites was measured with TG‐DSC. The results showed that the Fe₂O₃ nanoparticles in Fe₂O₃/AP nanocomposites exhibit better catalytic activity on the thermal decomposition of AP. In addition, the mechanism was also discussed.     

Synthesis of Nano‐γ‐Ferric Oxide by Thermolysis of the 2‐Mercapto‐5‐Methylpyridine‐N‐Oxide‐Iron(III) Complex via Factorial Design

2‐Mercapto‐5‐methylpyridine‐N‐oxide (MMPNO) and its sodium salt (NaMMPNO) were synthesized. The reaction of the latter with Fe³⁺ generates Fe(MMPNO)₃ chelate. The thermolysis of this chelate at 350 °C yielded highly pure reddish‐brown γ‐Fe₂O₃ nanocrystallites with an average particle size of 6.2 nm, a particle size range of 4.2 to 14.8 nm, and a specific surface area of 51.5 m²g^–1. The thermolysis process was optimized using the 2² fractional design. Quantitative tests and characterization of products were carried out by UV‐vis spectroscopy, XRD, LLS, SEM, TGA, BET, TEM, FT‐IR, elemental microanalysis, and classical analytical measurements.     

Al2O3/Yttria‐Stabilized Zirconia Hollow‐Fiber Membrane Incorporated with Iron Oxide for Pb(II) Removal

Removal by absorptive ceramic membranes can simultaneously absorb and separate metal ions from water. Alumina/yttria‐stabilized zirconia (Al₂O₃/YSZ) hollow‐fiber membranes, fabricated using phase inversion and sintering process, were deposited with iron oxide by an in‐situ hydrothermal process. The results showed that α‐Fe₂O₃ was produced and incorporated across the membranes. A reduction in flux was recorded with the deposition of α‐Fe₂O_3. However, it improved the adsorption capacity for heavy metal adsorption. The adsorption‐separation test demonstrated that the optimized membrane is able to completely remove Pb(II) ions after two hours.     

High‐Performance Small‐Amount Fe2O3‐Doped (K,Na)NbO3‐Based Lead‐Free Piezoceramics with Irregular Phase Evolution

[(K_0.43Na_0.57)_0.94Li_0.06][(Nb_0.94Sb_0.06)_0.95Ta_0.05]O₃ + x mol% Fe₂O₃ (KNLNST + x Fe, x = 0~0.60) lead‐free piezoelectric ceramics were prepared by conventional solid‐state reaction processing. The effects of small‐amount Fe₂O₃ doping on the microstructure and electrical properties of the KNLNST ceramics were systematically investigated. With increasing Fe³⁺ content, the orthorhombic‐tetragonal polymorphic phase transition temperature (T_O‐T) of KNLNST + x Fe ceramics presented an obvious “V” type variation trend, and T_O‐T was successfully shifted to near room temperature without changing T_C (T_C = 315°C) via doping Fe₂O₃ around 0.25 mol%. Electrical properties were significantly enhanced due to the coexistence of both orthorhombic and tetragonal ferroelectric phases at room temperature. The ceramics doped with 0.20 mol% Fe₂O₃ possessed optimal piezoelectric and dielectric properties of d₃₃ = 306 pC/N, k_p = 47.0%, = 1483 and tan δ = 0.023. It was revealed that the strong internal stress in the KNLNST + x Fe ceramics with higher Fe³⁺ contents (x = 0.40, 0.60) stabilized the orthorhombic phase, leading to the irregular “V” type rather than the usually observed monotonic phase transition with composition change in the ceramics.     

High‐Energy Pollen‐Like Porous Fe2O3/Al Thermite: Synthesis and Properties

A pollen‐like porous Fe₂O₃/Al thermite was prepared by a templated method, with aluminium nanoparticles (Al‐NPs) embedded in the porous channels. The thermite prepared by reduced pressure released the largest exothermic heat during DSC testing period compared with Fe₂O₃/Al thermites prepared by ultrasonic mixing and physical mixing. The exothermic heats in the range of 773 K to 1273 K are 3742.3 J g⁻¹, 2279.0 J g⁻¹, 1981.1 J g⁻¹, and 2621.0 J g⁻¹ for pollen‐like Fe₂O₃/Al by reduced pressure, pollen‐like Fe₂O₃/Al by ultrasonic mixing, pollen‐like Fe₂O₃/Al by physical mixing, and commercial Fe₂O₃/Al by ultrasonic mixing, respectively. The reactivity between Fe₂O₃ and Al‐NPs was efficiently improved, corresponding to its enlarged contact surface area between Al‐NPs and the porous pollen‐like Fe₂O₃, and the reduced pre‐combustion sintering. Furthermore, pollen‐like Fe₂O₃/Al has good compatibility with both RDX and HMX and it is not compatible with Cl‐20 and GAP.     

Kinetics of Liquid‐Phase Hydrogenation of Iso‐valeraldehyde to Iso‐amyl Alcohol Over A Ru/Al2O3 Catalyst

The liquid‐phase catalytic hydrogenation of iso‐valeraldehyde to iso‐amyl alcohol was studied in a slurry reactor. The kinetics of liquid‐phase hydrogenation of iso‐valeraldehyde over a 5% Ru/Al₂O₃ catalyst was studied in the range of temperature 373‐393 K and H₂ pressure 0.68‐2.72 MPa using 2‐propanol as the solvent. The selectivity to iso‐amyl alcohol was 100%. The kinetic data were analyzed using a simple power law model. A single site Langmuir‐Hinshelwood type model suggesting dissociative adsorption of hydrogen and surface reaction as the rate‐controlling step provided the best fit of the experimental data. The catalyst could be reused thrice without any loss in activity.     

Catalytic combustion of chlorinated ethylenes over H‐zeolites

Several H‐zeolites (H‐Y, H‐ZSM‐5 and H‐MOR) were investigated for the catalytic combustion of chlorinated ethylenes, namely 1,1‐dichloroethylene and trichloroethylene. Conversion was inversely related to the chlorine content of the feed molecule. H‐ZSM‐5 zeolite was the most active catalyst in 1,1‐dichloroethylene combustion whereas H‐MOR was the most effective zeolite for trichloroethylene destruction. Temperature‐programmed desorption of ammonia and diffuse reflectance FT‐IR measurements of adsorbed pyridine revealed that strong Brønsted acidity plays an important role in controlling the activity of H‐zeolites. The main combustion products were CO, CO₂, HCl, and Cl₂. Additionally, small amounts of highly chlorinated by‐products were also detected, namely trichloroethylene and tetrachloroethylene. H‐zeolites showed a great selectivity to HCl formation. © 2002 Society of Chemical Industry