Preparation and Characterization of Activated Carbons from Palm Nut Shells: Effects of Calcination Temperature on Porosity and Chemical Properties

Activated carbons (ACs) calcined at 400˚C, 500˚C, and 600˚C (AC-400, AC-500, and AC-600) were prepared using palm nut shells from Gabon as raw material and zinc chloride (ZnCl2) as a chemical activating agent. Prepared ACs were characterized by physisorption of nitrogen (N2), determination of diode and methylene blue numbers for studies of porosity and by quantification and determination of surface functional groups and pH at point of zero charge (pHpzc) respectively, for studies of chemical properties of prepared ACs. Then, effects of calcination temperature (Tcal) on porosity and chemical properties of prepared ACs were studied. The results obtained showed that when the calcination temperature increases from 500˚C to 600˚C, the porosity and chemical properties of prepared ACs are modified. Indeed, the methylene blue and iodine numbers determined for activated carbons AC-400 (460 and 7.94 mg·g−1, respectively) and AC-500 (680 and 8.90 mg·g−1, respectively) are higher than those obtained for AC-600 (360 and 5.75 mg·g−1, respectively). Compared to the AC-500 adsorbent, specific surface areas (SBET) and microporous volume losses for AC-600 were estimated to 44.7% and 45.8%, respectively. Moreover, in our experimental conditions, the effect of Tcal on the quantities of acidic and basic functional groups on the surface of the ACs appears negligible. In addition, results of the pHpzc of prepared ACs showed that as Tcal increases, the pH of the adsorbents increases and tends towards neutrality. Indeed, a stronger acidity was determined on AC-400 (pHpzc = 5.60) compared to those on AC-500 and AC-600 (pHpzc = 6.85 and 6.70, respectively). Also according to the results of porosity and chemical characterizations, adsorption being a surface phenomenon, 500˚C appears to be the optimal calcination temperature for the preparation of activated carbons from palm nut shells in our experimental conditions.

Optimization of preparing V_2O_5 by calcination from ammonium metavanadate using response surface methodology

Parameters of technique to prepare vanadium pentoxide by calcination from ammonium metavanadate were optimized using central composite design of response surface methodology. A quadratic equation model for decomposition rate was built and effects of main factors and their corresponding relationships were obtained. The results of the statistical analysis show that the decomposition rate of ammonium metavanadate is significantly affected by calcination temperature and calcination time. The optimized calcination conditions are as follows： calcination temperature 669.71 K, calcination time 35.9 min and sample mass 4.25 g. The decomposition rate of ammonium metavanadate is 99.71%,which coincides well with experimental value of 99.27% under the optimized conditions, suggesting that regressive equation fits the decomposition rates perfectly. XRD reveals that it is feasible to prepare the V2O5 by calcination from ammonium metavanadate using response surface methodology.

Effect of Calcination Temperature on La-Modified Al2O3 Catalysts for Vapor Phase Hydrofluorination of Acetylene to Vinyl Fluoride

A La-modified Al2O3 catalyst was prepared with deposition-precipitation method. The effect of calcination temperature on the reactivity for vapor phase hydrofluorination of acetylene to vinyl fluoride. The catalysts calcined at different temperatures were characterized using NH3-TPD, pyridine-FTIR, X-ray diffraction, and Raman techniques. It was found that the calcination process could not only change the structure of these catalysts but also modify the amount of surface acidity on the catalysts. The catalyst calcined at 400 ℃ exhibited the highest conversion of acetylene （94.6%） and highest selectivity to vinyl fluoride （83.4%） and lower coke deposition selectivity （0.72%）. The highest activity was related to the largest amount of surface acidity on the catalyst, and the coke deposition was also related to the total amount of surface acidic sites.

Effect of Calcination Temperature on Catalytic Activity and Textual Property of Cu/HMOR Catalysts in Dimethyl Ether Carbonylation Reaction

The effect of calcination temperature on the catalytic activity for the dimethyl ether （DME） carbonylation into methyl acetate （MA） was investigated over mordenite supported copper （Cu/HMOR） prepared by ion-exchange process. The results showed that the catalytic activity was obviously affected by the calcination temperature. The maximal DME conversion of 97.2% and the MA selectivity of 97.9% were obtained over the Cu/HMOR calcined at 430 ℃ under conditions of 210 ℃, 1.5 MPa, and GSHV of 4883 h^-1. The obtained Cu/HMOR catalysts were characterized by powder X-ray diffraction, N2 absorption, NH3 temperature program desorption, CO temperature program desorption, and Raman techniques. Proper calcination temperature was effective to promote copper ions migration and diffusion, and led the support HMOR to possess more acid activity sites, which exhibited the complete decomposing of copper nitrate, large surface area and optimum micropore structure, more amount of CO adsorption site and proper amount of weak acid centers.

A thermodynamic view on the in-situ carbon dioxide reduction by biomass-derived hydrogen during calcium carbonate decomposition

In the carbonate industry,deep decarbonization strategies are necessary to effectively remediate CO_(2).These strategies mainly include both sustainable energy supplies and the conversion of CO_(2)in downstream processes.This study developed a coupled process of biomass chemical looping H2 production and reductive calcination of CaCO_(3).Firstly,a mass and energy balance of the coupled process was established in Aspen Plus.Following this,process optimization and energy integration were implemented to provide optimized operation conditions.Lastly,a life cycle assessment was carried out to assess the carbon footprint of the coupled process.Results reveal that the decomposition temperature of CaCO_(3)in an H_(2)atmosphere can be reduced to 780℃(generally around 900℃),and the conversion of CO_(2)from CaCO_(3)decomposition reached 81.33%with an H2:CO ratio of 2.49 in gaseous products.By optimizing systemic energy through heat integration,an energy efficiency of 86.30%was achieved.Additionally,the carbon footprint analysis revealed that the process with energy integration had a low global warming potential(GWP)of-2.624 kg·kg^(-1)(CO_(2)/CaO).Conclusively,this work performed a systematic analysis of introducing biomass-derived H_(2)into CaCO_(3)calcination and demonstrated the positive role of reductive calcination using green H_(2)in mitigating CO_(2)emissions within the carbonate industry.

Recycling arsenic-containing bio-leaching residue after thermal treatment in cemented paste backfill:Structure modification,binder properties and environmental assessment

The substantial arsenic(As)content present in arsenic-containing bio-leaching residue(ABR)presents noteworthy environ-mental challenges attributable to its inherent instability and susceptibility to leaching.Given its elevated calcium sulfate content,ABR exhibits considerable promise for industrial applications.This study delved into the feasibility of utilizing ABR as a source of sulfates for producing super sulfated cement(SSC),offering an innovative binder for cemented paste backfill(CPB).Thermal treatment at varying temperatures of 150,350,600,and 800℃ was employed to modify ABR’s performance.The investigation encompassed the examination of phase transformations and alterations in the chemical composition of As within ABR.Subsequently,the hydration characteristics of SSC utilizing ABR,with or without thermal treatment,were studied,encompassing reaction kinetics,setting time,strength development,and microstructure.The findings revealed that thermal treatment changed the calcium sulfate structure in ABR,consequently impacting the resultant sample performance.Notably,calcination at 600℃ demonstrated optimal modification effects on both early and long-term strength attributes.This enhanced performance can be attributed to the augmented formation of reaction products and a densified micro-structure.Furthermore,the thermal treatment elicited modifications in the chemical As fractions within ABR,with limited impact on the As immobilization capacity of the prepared binders.

Effect of Na_(2)CO_(3)Roasting Activation on Acid Leaching Property of Fly Ash

By using high-alumina fly ash as raw material,a process was proposed for activating the fly ash with Na_(2)CO_(3)calcination and extracting aluminum from activated clinker with sulfuric acid leaching.The feasibility of roasting process of activated fly ash by Na_(2)CO_(3)was discussed based on thermodynamic analysis.The experimental results showed that Na_(2)CO_(3)gradually reactes with mullite over 700 K to produce NaAlSiO_(4).The optimal process conditions for the activation stage are:a material ratio of 1:1 between sodium carbonate and fly ash,a calcination temperature of 900℃,and a calcination time of 2.5 hours.Under these conditions,the leaching rate of aluminum is 90.3%.By comparing the SEM and XRD analysis of raw and clinker materials,it could be concluded that the mullite phase of fly ash is almost completely destroyed and transformed into sodium aluminosilicate with good acid solubility.

Controllable synthesis of CuAlO_(2) via solid-phase method and its catalytic performance for methanol steam reforming to hydrogen

This study explores the controllable synthesis of CuAlO_(2) using copper hydroxide and pseudo-boehmite powders as raw materials via a simple solid-phase ball milling method,along with its catalytic performance investigation in methanol steam reforming(MSR).Various catalysts were prepared under different conditions,such as calcination temperature,calcination atmosphere,and heating rate.Characterization techniques including BET,XRD,XPS,SEM and H2-TPR were employed to analyze the samples.The results revealed significant effects of calcination temperature on the phase compositions,specific surface area,reduction performance,and surface properties of the CA-T catalysts.Based on the findings,a synthesis route of CuAlO_(2) via the solid-phase method was proposed,highlighting the importance of high calcination temperature,nitrogen atmosphere,and low heating rate for CuAlO_(2) formation.Catalytic evaluation data demonstrated that CuAlO_(2) could catalyze MSR without pre-reduction,with the catalytic performance of CA-T catalysts being notably influenced by calcination temperature.Among the prepared catalysts,the CA-1100 catalyst exhibited the highest catalytic activity and stability.The findings of this study might be useful for the further study of the catalytic material for sustained release catalysis,including the synthesis of catalytic materials and the regulation of sustained release catalytic performance.

Model of limestone calcination / sulfation under oxy-fuel fluidized bed combustion

The characteristics of the simultaneous calcination/ sulfation of limestone under oxy-fuel fluidized bed combustion were studied and compared with those of the sulfation of precalcined CaO. During the calcination stage, SO2 can react with product CaO and slow down the CaCO3 decomposition rate by the covering effect of the CaSO4 product. The sulfation rate of simultaneous calcinatiort/sulfation is slower than that of precalcined CaO, but with a long enough sulfation time, the calcium conversion of simultaneous calcination/sulfation is higher than that of the precalcined CaO. A grain-micrograin model is established to describe the simultaneous calcination, sintering and sulfation of limestone. The graln-micrograln model can reflect the true reaction process of the calcination and sulfation of limestone in oxy-fuel fluidized bed combustion.

Solvent-free selective oxidation of cyclohexane with molecular oxygen over manganese oxides:Effect of the calcination temperature

The effects of calcination temperature on the physicochemical properties of manganese oxide catalysts prepared by a precipitation method were assessed by X-ray diffraction,N2 adsorption-desorption,X-ray photoelectron spectroscopy,H2 temperature-programmed reduction,O2 temperature-programmed desorption,and thermogravimetry-differential analysis.The catalytic performance of each of these materials during the selective oxidation of cyclohexane with oxygen in a solvent-free system was subsequently examined.It was found that the MnOx-500 catalyst,calcined at 500 °C,consisted of a Mn2O3 phase in addition to Mn5O8 and Mn3O4 phases and possessed a low surface area.Unlike MnOx-500,the MnOx-400 catalyst prepared at 400 °C was composed solely of Mn3O4 and Mn5O8 and had a higher surface area.The pronounced catalytic activity of this latter material for the oxidation of cyclohexene was determined to result from numerous factors,including a higher concentration of surface adsorbed oxygen,greater quantities of the surface Mn4＋ ions that promote oxygen mobility and the extent of O2 adsorption and reducibility on the catalyst.The effects of various reaction conditions on the activity of the MnOx-400 during the oxidation of cyclohexane were also evaluated,such as the reaction temperature,reaction time,and initial oxygen pressure.Following a 4 h reaction at an initial O2 pressure of 0.5 MPa and 140 °C,an 8.0% cyclohexane conversion and 5.0% yield of cyclohexanol and cyclohexanone were achieved over the MnOx-400 catalyst.In contrast,employing MnOx-500 resulted in a 6.1% conversion of cyclohexane and 75% selectivity for cyclohexanol and cyclohexanone.After being recycled through 10 replicate uses,the catalytic activity of the MnOx-400 catalyst was unchanged,demonstrating its good stability.

Effect of Calcination Temperature on Surface Oxygen Vacancies and Catalytic Performance Towards CO Oxidation of Co3O4 Nanoparticles Supported on SiO2

Co3O4/SiO2 catalysts for CO oxidation were prepared by conventional incipient wetness impregnation followed by calcination at various temperatures. Their structures were char- acterized with X-ray diffraction （XRD）, laser Raman spectroscopy, X-ray photoelectron spectroscopy （XPS）, temperature-programmed reduction （TPR） and X-ray absorption fine structure （XAFS） spectroscopy. Both XRD and Raman spectroscopy only detect the existence of Co3O4 crystallites in all catalysts. However, XPS results indicate that excess Co2＋ ions are present on the surface of Co3O4 in Co3O4（200）/Si02 as compared with bulk Co3O4. Meanwhile, TPR results suggest the presence of surface oxygen vacancies on Co3O4 in Co3O4（200）/SiO2, and XAFS results demonstrate that Co3O4 in Co3O4（200）/SIO2 contains excess Co2＋. Increasing calcination temperature results in oxidation of excess Co2＋ and the decrease of the concentration of surface oxygen vacancies, consequently the for- mation of stoichiometric Co3O4 on supported catalysts. Among all Co3O4/SiO2 catalysts, Co3O4（200）/SiO2 exhibits the best catalytic performance towards CO oxidation, demonstrating that excess Co2＋ and surface oxygen vacancies can enhance the catalytic activity of Co3O4 towards CO oxidation. These results nicely demonstrate the effect of calcination temperature on the structure and catalytic performance towards CO oxidation of silicasupported Co3O4 catalysts and highlight the important role of surface oxygen vacancies on Co3O4.

Modified calcination conditions of rare alkali metal Rb-containing muscovite(KAl_2[AlSi_3O_(10)](OH)_2)

Muscovite mineral was roasted in different conditions.Rubidium leaching rate was a standard to examine the impact of various factors on calcination effect,including the agent types,roasting time,mass ratio,and roasting temperature.The results indicate that the best agent is the combination of sodium chloride and calcium chloride,and its mass ratio of muscovite/NaCl/CaCl2is1.00:0.25:0.25.Calcined at 850℃ for 30 min,the rubidium leaching rate is up to 90.12%.The reaction of muscovite ore with the chlorinating agent CaCl2was studied by TG/DSC,and the surface morphology before and after leaching was characterized by SEM.Rubidium chloride products can be obtained using t-BAMBP extraction,hydrochloric acid re-extraction,and purification.

Effect of calcination temperatures on photocatalytic H_(2)O_(2)-production activity of ZnO nanorods

Photocatalytic hydrogen peroxide(H_(2)O_(2))production from O_(2) and H2O is an ideal process for solar‐to‐chemical energy conversion.Herein,ZnO nanorods are prepared via a simple hydrothermal method for photocatalytic H_(2)O_(2) production.The ZnO nanorods exhibit varied performance with different calcination temperatures.Benefiting from calcination,the separation efficiency of photo‐induced carriers is significantly improved,leading to the superior photocatalytic activity for H_(2)O_(2) production.The H_(2)O_(2) produced by ZnO calcined at 300℃ is 285μmol L^(−1),which is over 5 times larger than that produced by untreated ZnO.This work provides an insight into photocatalytic H2O2 production mechanism by ZnO nanorods,and presents a promising strategy to H2O2 production.

Suspension calcination and alkali leaching of low-grade high-sulfur bauxite:Desulfurization, mineralogical evolution and desilication

To enable the utilization of low-grade and high-sulfur bauxite, the suspension calcination was used to remove the sulfur and the activate silica minerals, and the calcinated bauxite was subjected to a desilication process in Na OH solution under atmospheric pressure. The desulfurization and desilication properties and mineralogical evolution were studied by X-ray diffraction, thermogravimetry–differential thermal analysis, scanning electron microscopy, and FactSage methods. The results demonstrate that the suspension calcination method is efficient for sulfur removal: 84.21% of S was removed after calcination at 1000°C for 2 min. During the calcination process, diaspore and pyrite were transferred to α-Al2O3, magnetite, and hematite. The phase transformation of pyrite follows the order FeS2 → Fe3O4 → Fe2O3, and the iron oxides and silica were converted into iron silicate. In the alkali-soluble desilication process, the optimum condition was an alkali solution concentration of 110 g/L, a reaction time of 20 min, and a reaction temperature of 95°C. The corresponding desilication ratio and alumina loss ratio were 44.9% and 2.4%, respectively, and the alumina-to-silica mass ratio of the concentrate was 7.9. The Al2O3·2SiO2, SiO2, and Al2O3 formed during the calcination process could react with Na OH solution, and their activity decreased in the order of Al2O3·2 SiO2, SiO2, and Al2O3.

Effects of Calcination Temperature on the Acidity and Catalytic Performances of HZSM-5 Zeolite Catalysts for the Catalytic Cracking of n-Butane

The acidic modulations of a series of HZSM-5 catalysts were successfully made by calcination at different treatment temperatures, i.e. 500, 600, 650, 700 and 800 ℃, respectively. The results indicated that the total acid amounts, their density and the amount of B-type acid of HZSM-5 catalysts rapidly decreased, while the amounts of L-type acid had almost no change and thus the ratio of L/B was obviously enhanced with the increase of calcination temperature （excluding 800 ℃）. The catalytic performances of modified HZSM-5 catalysts for the cracking of n-butane were also investigated. The main properties of these catalysts were characterized by means of XRD, N2 adsorption at low temperature, NH3-TPD, FTIR of pyridine adsorption and BET surface area measurements. The results showed that HZSM-5 zeolite pretreated at 800 ℃ had very low catalytic activity for n-butane cracking. In the calcination temperature range of 500-700 ℃, the total selectivity to olefins, propylene and butene were increased with the increase of calcination temperature, while, the selectivity for arene decreased with the calcination temperature. The HZSM-5 zeolite calcined at 700 ℃ produced light olefins with high yield, at the reaction temperature of 650 ℃ the yields of total olefins and ethylene were 52.8% and 29.4%, respectively. Besides, the more important role is that high calcination temperature treatment improved the duration stability of HZSM-5 zeolites. The effect of calcination temperature on the physico-chemical properties and catalytic performance of HZSM-5 for cracking of n-butane was explored. It was found that the calcination temperature had large effects on the surface area, crystallinity and acid properties of HZSM-5 catalyst, which further affected the catalytic performance for n-butane cracking.

Comparative catalytic study on butene/isobutane alkylation over LaX and CeX zeolites: The influence of calcination atmosphere

Lanthanum-containing(LaX)and cerium-containing X zeolites(CeX)were prepared by a doubleexchange,double-calcination method.By changing the calcination atmospheres between nitrogen and air,the Ce^(IV) contents in CeX zeolites were adjusted and their impacts on physicochemical properties and catalytic performance in isobutane alkylation were established.The crystallinity of CeX zeolite was found to be negatively correlated with the Ce^(IV) content.This i s believed to be due to the water formed during the oxidation of Ce^(III),which facilitates the framework dealumination.As a consequence,calcining in air resulted in a great elimination of strong Brønsted acid sites while under nitrogen protection,this phenomenon was mostly hindered and the sample’s acidity was preserved.When tested in a continuously flowed slurry reactor,the catalyst lifetime for isobutane alkylation was found to be linearly related to the strong Brønsted acid concentration.In addition,Ce^(3+)was found more benefit for the hydride transfer compared with La^(3+),which is ascribed to the stronger polarization effect on the CH bond of isobutane.Moreover,the decline of hydride transfer activity can be slowed down by the catalytic cracking of the bulky molecules.Based on the product distribution,a new catalytic cycle of dimethylhexanes(DMHs)involving a direct formation of isobutene rather than tert-butyl carbocation was proposed in isobutane alkylation.

CO oxidation over Co_3O_4/SiO_2 catalysts:Effects of porous structure of silica and catalyst calcination temperature

The catalytic performances of Co3O4/SiO2 catalysts prepared by incipient wetness impregnation for CO oxidation were investigated using three kinds of silica as carriers with different pore sizes of 7.7,14.0 and 27.0 nm.The effects of calcination temperature on the catalyst surface and micro structure properties as well as catalytic performance for the oxidation of carbon monoxide were also studied.All catalysts were characterized by N2 adsorption-desorption,XRD,XPS,FTIR,H2-TPR and O2-TPD.It was found that the properties and crystal size of cobalt-containing species strongly depended on the pore size of silica carrier.While the silica pore size increased from 7.7 to 27.0 nm,the Co3O4 crystal size increased from 8.5 to 13.5 nm.Moreover,it was demonstrated that if the spinel crystal structure of Co3O4 was obtained at a calcination temperature as low as 150℃,the catalyst sample would have a high Co3O4 surface dispersion and an increase of surface active species,and thus exhibit a high activity for the oxidation of carbon monoxide.

Influence of acid leaching and calcination on iron removal of coal kaolin

Calcination and acid leaching of coal kaolin were studied to determine an effective and economical preparation method of calcined kaolin. Thermogravimetric-differential thermal analysis （TG-DTA） and X-ray diffraction （XRD） demonstrated that 900＆#176;C was the suitable temperature for the calcination. Leaching tests showed that hydrochloric acid was more effective for iron dissolution from raw coal kaolin （RCK）, whereas oxalic acid was more effective on iron dissolution from calcined coal kaolin （CCK）. The iron dissolution from CCK was 28.78wt%, which is far less effective than the 54.86wt% of RCK under their respective optimal conditions. Through analysis by using M？ssbauer spectroscopy, it is detected that nearly all of the structural ferrous ions in RCK were removed by hydrochloric acid. However, iron sites in CCK changed slightly by oxalic acid leaching because nearly all ferrous ions were transformed into ferric species after firing at 900＆#176;C. It can be concluded that it is difficult to remove the structural ferric ions and ferric oxides evolved from the structural ferrous ions. Thus, iron removal by acids should be conducted prior to calcination.

THERMAL DECOMPOSITION BEHAVIOUR OF NATURAL BASTNASITE CRYSTAL IN CALCINATION

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Effect of calcination temperature on microstructure and photocatalytic activity of BiOX(X=Cl,Br)

A series of BiOX(X=Cl,Br) were prepared by simple hydrolysis and then calcined at various temperatures and they were characterized by XRD,Raman,SEM,DSC-TGA,BET and UV-Vis.The photocatalytic activity was evaluated by photocatalytic degradation of methyl orange(MO) solution under simulated solar light irradiation.The results show that the phase structure,crystallite size,morphology,specific surface area,porous structure,and the absorption band-edges are related to the calcination temperature.For BiOBr,it has completely transformed to Bi24O31Br10 at 600℃ and begins to transform to Bi2 O3 at 800℃.As for BiOCl,it begins to transform to Bi24O31Cl10 at 600℃ and completely transforms to Bi24O31Cl10 at 800℃.Finally,the photocatalytic activity of BiOCl decreases with the temperature increasing owing to decrease of the specific surface areas and pore size,while the photocatalytic activity of BiOBr increases in the first stage and then decreases,which is related to good crystallization and three-dimensional structure.