Characterization of Microwave and Conventional Heating on the Pyrolysis of Pistachio Shells for the Adsorption of Methylene Blue and Iodine

The production of activated carbon was investigated using the sequential combination of microwave and conventional heating of pistachio shells as the raw precursor with zinc chloride. Several techniques such as thermogravimetric and differential thermal analyses, infrared spectroscopy, scanning electron microscopy, and specific surface area analyses were performed to characterize the samples. The highest specific surface area value for the activated carbon prepared at a microwave power of 200?W with microwave time of 20?min, and flow rate of 50?mL?min^?1 was 1468?m²?g^?1. The methylene blue and iodine adsorption capacities were 331 and 1276?mg?g^?1, respectively. The results were compared to those obtained using physical and chemical activation methods and showed that the sequential combination of microwave and conventional heating reasonably influenced the micropore surface area of the samples as well as the specific surface area.     

Preparation and Characterization of Activated Carbon from Microwave and Conventional Heated Almond Shells Using Phosphoric Acid Activation

Activated carbon production from almond shells using phosphoric acid activation agent was achieved by applying both conventional heating and microwave heating in succession. The morphology and surface properties of activated carbon were studied using thermogravimetric and differential gravimetric analysis, Fourier-transform infrared spectroscopy, scanning electron microscopy, and Brunauer–Emmett–Teller analysis. A surface area of 1128 m²/g was achieved by optimizing the microwave power (500?W), microwave application time (15?minutes), conventional heating time (45?minutes), conventional heating temperature (500?°C), and the phosphoric acid:sample ratio (0.7:1). An adsorption capacity of methylene blue of 148?mg/g and an iodine value of 791?mg/g was obtained for the prepared activated carbon.     

微波辐射在制备竹节活性炭中的应用研究

研究了以竹节废料为原料，采用微波辐射氯化锌法制备优质活性炭的可行性．探讨了微波功率．活化时间及氯化锌浓度对产品各项指标的影响．得到了微波辐射氯化锌法制备活性炭的最佳工艺：微波功率350W、活化时间5min、氯化锌浓度40%．用此工艺制得的活性炭碘吸附值1088．4mg／g、亚甲基蓝脱色力22．0ml/0．1g．得率39．2％．该工艺所需活化时间为传统方法的1／36，产品活性炭亚甲基蓝脱色力为国家一级标准的1．83倍(GB/T13496.10-1999)．微波辐射法所制活性炭比传统方法所制活性炭具有更加发达的孔隙结构，且孔隙的分布更加均匀．     

Adsorption of cationic methylene blue dye using microwave-assisted activated carbon derived from acacia wood: Optimization and batch studies

This study assesses the performance of optimized acacia wood-based activated carbon (AWAC) as an adsorbent for methylene blue (MB) dye removal in aqueous solution. AWAC was prepared via a physicochemical activation process that consists of potassium hydroxide (KOH) treatment, followed by carbon dioxide (CO₂) gasification under microwave heating. By using response surface methodology (RSM), the optimum preparation conditions of radiation power, radiation time, and KOH-impregnation ratio (IR) were determined to be 360 W, 4.50 min, and 0.90 g/g respectively, which resulted in 81.20 mg/g of MB dye removal and 27.96% of AWAC’s yield. Radiation power and IR had a major effect on MB dye removal while radiation power and radiation time caused the greatest impact on AWAC’s yield. BET surface area, mesopore surface area, and pore volume of optimized AWAC were found to be 1045.56 m²/g, 689.77 m²/g, and 0.54 cm³/g, respectively. Adsorption of MB onto AWAC followed Langmuir and pseudo-second order for isotherm and kinetic studies respectively, with a Langmuir monolayer adsorption capacity of 338.29 mg/g. Mechanism studies revealed that the adsorption process was controlled by film diffusion mechanism and indicated to be thermodynamically exothermic in nature.     

Characteristics of activated carbon prepared from pistachio-nut shell by zinc chloride activation under nitrogen and vacuum conditions

Activated carbons with well-developed pore structures were prepared from pistachio-nut shells by chemical activation using zinc chloride under both nitrogen atmosphere and vacuum conditions. The effects of preparation parameters on the carbon pore structure were studied in order to optimize these parameters. It was found that under vacuum conditions, the characteristics of the activated carbons produced are better than those under nitrogen atmosphere. The impregnation ratio, the activation temperature, and the activation hold time are the important parameters that influence the characteristics of the activated carbons. The optimum experimental conditions for preparing predominantly microporous activated carbons with high pore surface area and micropore volume are an impregnation ratio of 0.75, an activation temperature of 400 degrees C, and a hold time of 1 h. Under these conditions, the BET surface areas of the carbons activated under nitrogen atmosphere and vacuum conditions were 1635.37 and 1647.16 m2/g, respectively. However, at a ZnCl2 impregnation ratio of 1.5, a furnace temperature of 500 degrees C, and a hold time of 2 h, the predominantly mesoporous activated carbon prepared under vacuum condition had a BET surface area of 2527 m2/g. Fourier transform infrared spectra were used to detect changes in the surface functional groups of the samples during the different preparation stages.     

A New Approach for Controlling Mesoporosity in Activated Carbon by the Consecutive Process of Air Oxidation,Thermal Destruction of Surface Functional Groups,and Carbon Activation (the OTA Method)

A new and simple method, based entirely on a physical approach, was proposed to produce activated carbon from longan fruit seed with controlled mesoporosity. This method, referred to as the OTA, consisted of three consecutive steps of (1) air oxidation of initial microporous activated carbon of about 30% char burn-off to introduce oxygen surface functional groups, (2) the thermal destruction of the functional groups by heating the oxidized carbon in a nitrogen atmosphere at a high temperature to increase the surface reactivity due to increased surface defects by bond disruption, and (3) the final reactivation of the resulting carbon in carbon dioxide. The formation of mesopores was achieved through the enlargement of the original micropores after heat treatment via the CO₂ gasification, and at the same time new micropores were also produced, resulting in a larger increase in the percentage of mesopore volume and the total specific surface area, in comparison with the production of activated carbon by the conventional two-step activation method using the same activation time and temperature. For the activation temperatures of 850 and 900 °C and the activation time of up to 240 min, it was found that the porous properties of activated carbon increased with the increase in activation time and temperature for both preparation methods. A maximum volume of mesopores of 0.474 cm³/g, which accounts for 44.1% of the total pore volume, and a maximum BET surface area of 1773 m²/g was achieved using three cycles of the OTA method at the activation temperature of 850 °C and 60 min activation time for each preparation cycle. The two-step activation method yielded activated carbon with a maximum mesopore volume of 0.270 cm³/g (33.0% of total pore volume) and surface area of 1499 m²/g when the activation temperature of 900 °C and a comparable activation time of 240 min were employed. Production of activated carbon by the OTA method is superior to the two-step activation method for better and more precise control of mesopore development.     

Preparation and characterization of activated carbon from pine cone by microwave-induced ZnCl2 activation and its effects on the adsorption of methylene blue

In this work, activated carbon prepared from pine cone (PCAC) with ZnCl₂ as an activation agent under microwave radiation was investigated. The activation step was performed at the microwave input power of 400 W and radiation time of 5 min. The properties of activated carbon were characterized by N₂ adsorption Brunauer–Emmett–Teller (BET), scanning electron microscopy and Fourier transform infrared spectroscopy. Results showed that the BET surface area, Langmuir surface area, and total pore volume of PCAC were 939, 1,486 m²/g and 0.172 cm³/g, respectively. Adsorption capacity was demonstrated by the iodine numbers. The adsorptive property of PCAC was tested using methylene blue dye. Equilibrium data was best fitted by the Langmuir isotherm model, showing a monolayer adsorption capacity of 60.97 mg/g. The pseudo-first- and pseudo-second-order kinetic models were examined to evaluate the kinetic data, and the rate constants were calculated. Adsorption of the dyes followed pseudo-first order kinetics. Thermodynamic parameters such as free energy, enthalpy and entropy of dye adsorption were obtained.     

Preparation of activated carbon from sawdust by zinc chloride activation

A series of activated carbons were prepared from sawdust by zinc chloride activation in different operation conditions. The effects of operation parameters such as impregnation ratio, activation temperature and time on the adsorption properties of activated carbons were measured and analyzed in order to optimize these operation conditions. The experimental results show that under the experimental circumstances studied, both the yield and the adsorption for iodine and methylene blue of activated carbon can reach a relatively higher value in the chemical activation process with the impregnation ratio of 100% ZnCl₂/sawdust in the activation temperature of 500 °C carbonized for 60–90 minutes which are the optimum activation conditions in making wood activated carbon. The most important operation parameter in chemical activation with zinc chloride was found to be the impregnation ratio.     

微波辐射紫茎泽兰制备优质活性炭的研究

以紫茎泽兰为原料,碳酸钾为活化剂,采用超声波浸渍,微波辐射法制备活性炭.研究了浸渍方式与时间、微波功率、微波辐射时间、剂料比对活性炭吸附性能和得率的影响.得到了本实验条件下的优化工艺条件:超声波浸渍20min、120℃脱水2h,微波功率700W、微波辐射时间12min、剂料比1.25∶1.优化工艺条件下制备的活性炭碘吸附值为1470.27mg/g,亚甲基蓝吸附值为300mL/g,得率为16.35%.浸渍时间极大的缩短,微波辐射时间只有传统法活化时间的1/15左右,活性炭的吸附指标超过了国标GB/T 13803.1-1999和GB/T 13803.2-1999一级品的标准,其中碘吸附值是国家一级标准的1.47倍,亚甲基蓝吸附值是国家一级标准的2.73倍.同时,测定了该活性炭氮吸附,其BET比表面积为1540.97m2/g,总孔容为0.7393mL/g,并通过DFT表征了活性炭的孔径分布,结果表明该活性炭为微孔型活性炭.     

Microwave assisted preparation of efficient activated carbon from grapevine rhytidome for the removal of methyl violet from aqueous solution

Grapevine rhytidome (the outer layer of bark on trunk), as an abundant and low-cost precursor, was used to prepare granular activated carbon with high surface area for the removal of methyl violet from aqueous solution. Microwave heating source was used to reduce the treatment time and energy consumption. To optimize the preparation, the effects of the different parameters, such as phosphoric acid concentration, acid/precursor weight ratio, impregnation time, microwave power, radiation time, and oven heating time on the ability of the samples for removal of methyl violet were studied. The obtained activated carbon was characterized by N₂ adsorption/desorption, SAXS, TEM and SEM methods. The adsorption of methyl violet onto the activated carbon was studied from both equilibrium and kinetic point of view and the results were compared with the commercial granular activated carbon. The rate of adsorption onto the prepared activated carbon was faster than commercial activated carbon. Different kinetic models were used to analyze the experimental kinetic data. The obtained activated carbon showed higher adsorption capacity (more than twice) for the adsorption of methyl violet in comparison with the commercial one. The equilibrium data were analyzed using different isotherm models. Adsorption was found to be maximum in the pH range 7-9.     

Conversion of teak wood waste into microwave-irradiated activated carbon for cationic methylene blue dye removal: Optimization and batch studies

The objective of this study is to find optimum preparation conditions in converting teak wood waste into activated carbon (TWAC) and to evaluate its performance in adsorbing cationic dye of methylene blue (MB). TWAC was produced via physiochemical activation (potassium hydroxide, KOH chemical treatment, and carbon dioxide, CO₂ gasification) and heated through microwave irradiation technique. With the aid of response surface methodology (RSM), optimized TWAC was successfully synthesized at radiation power, radiation time, and impregnation ratio (IR) of 366 W, 5.30 min, and 1.15 g/g, respectively. These preparation conditions produced TWAC with MB adsorption uptakes of 66.69 mg/g and a yield of 38.23%. Characteristics of TWAC in terms of BET surface area, mesopores surface area, total pore volume, and average pore diameter were determined to be 1345.25 m²/g, 878.63 m²/g, 0.6140 cm³/g, and 2.85 nm, respectively. Isotherm studies divulged that the MB-TWAC adsorption system followed the Langmuir model with a maximum monolayer adsorption capacity of 567.52 mg/g. In terms of kinetic studies, this adsorption system fit pseudo-second order model the best whereas Boyd plot confirmed that the adsorption process was controlled by the film diffusion mechanism. Thermodynamic parameters of enthalpy change, ΔH°, entropy change, ΔS°, Gibbs free energy, ΔG° and Arrhenius activation energy, E_a were calculated to be ?4.06 kJ/mol, 0.06 kJ/mol.K, –22.69 kJ/mol and 16.03 kJ/mol, respectively. The activation and microwave heating methods employed succeeded to produce TWAC with excellent adsorption performance in removing MB dye. TWAC was also successfully regenerated for 5 cycles via microwave heating technique.     

Effects of activation conditions on the structural and adsorption characteristics of pinecones derived activated carbons

This study was conducted to understand and optimize the activation process for the production of a low-cost activated carbon (AC) using a renewable and plentiful biomass waste, pinecones. This was achieved by tracking the changes in porous structure, surface chemistry and adsorption properties of the AC produced using different activating agents, activation temperatures, holding times and heating rates. Generally, produced ACs were predominantly microporous with small external surface area and were different in terms of H/C and O/C ratios. Study of Pb²⁺ cations adsorption on these samples proved the high affinity of the pinecones derived ACs to this cation. The best adsorption behaviour was recognized in sample prepared by impregnation with H₃PO₄ at weight ratio of 2, then heating at 400?°C for 2?h at 5?°C/min heating rate. This sample possessed the highest BET surface area (1335 m²/g). The adsorption process obeyed the pseudo-first-order and Freundlich model slightly better than the pseudo-second-order kinetics and Langmuir model. The high Langmuir maximum adsorption capacity of 418?mg/g supports the applicability of the produced AC for the removal of Pb²⁺ cations from wastewater.     

Adsorption of methyl orange using activated carbon prepared from lignin by ZnCl2 treatment

Lignocellulosic materials are good and cheap precursors for the production of activated carbon. In this study, activated carbons were prepared from the lignin at different temperatures (200 to 500°C) by ZnCl₂. The effects influencing the surface area of the resulting activated carbon are activation temperature, activation time and impregnation ratio. The optimum condition, are found an impregnation ratio of 2, an activation temperature of 450°C, and an activation time of 2 h. The results showed that the surface area and micropores volume of activated carbon at the experimental conditions are achieved to 587 and 0.23 cm³ g^?1, respectively. The adsorption behavior of methyl orange dye from aqueous solution onto activated lignin was investigated as a function of equilibrium time, pH and concentration. The Langmuir and Freundlich adsorption models were applied to describe the equilibrium isotherms. A maximum adsorption capacity of 300 mg g^?1 of methyl orange by activated carbon was achieved.     

Preparation and characterization of activated carbons from Sterculia alata nutshell by chemical activation with zinc chloride to remove phenol from wastewater

Nutshells of Sterculia alata, a forest waste, were used to prepare activated carbons by zinc chloride activation under four different activation atmospheres, to develop carbons with substantial capability, and to adsorb phenol from wastewater. Experiments were carried out at different chemical ratios (activating agent/precursor). Effect of carbonization temperature and time are the important variables, which had significant effect on the pore structure of carbon. Developed activated carbon was characterized by SEM analysis. Pore volume and surface area were estimated by Hg porosimetry and BET surface area analyses. The carbons showed surface area and micropore volumes of around 712 m²/g and 0.542 cm³/g, respectively. The activated carbon developed shows substantial capability to adsorb phenol from wastewater. The kinetic data were fitted to the models of intraparticle diffusion, pseudo-second order, and Lagergren model and followed more closely the pseudo-second-order chemisorption model. The isotherm equilibrium data were well-fitted by the Langmuir and Freundlich models. The maximum uptake of phenol was found at pH 3.5.     

Preparation and Characterization of Quaternized Chitosan Under Microwave Irradiation

For the first time, N-(2-hydroxyl) propyl-3-trimethyl ammonium chitosan chloride (HTCC) was prepared through a fast, easy and efficient method with the assistance of microwave irradiation, and the quaternized chitosan was also degraded via the microwave irradiation. A comparative study was performed by using the conventional heating method to prepare HTCC. The structure and property of the quaternized chitosan obtained by these two methods were characterized by GPC, XRD, FTIR, NMR, TG and elemental analysis. It was shown that quaternized chitosan was successfully prepared within 50 min via microwave irradiation method, while a much longer time of 6–7 h was needed with the conventional heating method. The substitutions both occurred on the C2 position of chitosan with the two different methods, and their HTCC products had weight average similar molecular weight (Mw), structure and thermal stability. The HTCC prepared by the microwave irradiation method had a little lower degree of substitution (DS) than those prepared via conventional heating with the same mole ratio (6:1) of the intermediate to chitosan. The degradation study showed that the Mw of HTCC decreased rapidly from 4.6 × 10⁵ to 1.1 × 10⁵ in 1 h under microwave irradiation, while it only decreased from 4.6 × 10⁵ to 2.1 × 10⁵in 1 h through conventional heating degradation. These results revealed that microwave irradiation is a more efficient and environment-friendly way to obtain the water-soluble chitosan derivatives and their degraded products.     

KOH活化木屑生物炭制备活性炭及其表征

以木屑热裂解的生物质炭为原料,氢氧化钾为活化剂,采用化学活化法制备活性炭,探讨了碱炭比、活化温度和活化时间对活性炭吸附亚甲基蓝吸附值的影响。 利用N2吸附实验、XRD和FTIR等实验技术,对原料与制备活性炭的结构与性能进行了表征。 结果表明,在碱炭质量比为1.5、活化温度750 ℃、活化时间2 h的条件下,所制备的活性炭对亚甲基蓝吸附值为255 mg/g,BET总比表面积为1514 m2/g,中孔比表面积为110 m2/g,吸附总孔容为0.821 cm3/g,中孔孔容为0.117 cm3/g,吸附平均孔径为2.170 nm。     

Single-stage microwave assisted coconut shell based activated carbon for removal of Zn(II) ions from aqueous solution – Optimization and batch studies

Health and environmental issues associated with heavy metal ions have received serious attention from communities worldwide. This work explores the potential of coconut shell as activated carbon (CSAC), in adsorbing zinc, Zn(II) ions. This adsorbent was prepared via a single-stage microwave irradiation technique under the flow of carbon dioxide, CO₂ gas. CSAC posed BET surface area of 625.61 m²/g, 513.25 m²/g of mesopores surface area, total pore volume of 0.42 cm³/g, and average pore diameter of 4.55 nm. Zeta potential distribution on CSAC was found to be ?21 mV. Response surface methodology (RSM) had suggested that the optimum values of variables were 450 W and 3.17 min for radiation power and radiation time respectively, which resulted in 69.65% of Zn(II) removal and 44.32% of CSAC’s yield. Based on F-value, radiation power (473.62) and radiation time (140.50) posed major and moderate effects on Zn(II) removal, respectively. Meanwhile, CSAC’s removal was significantly affected by radiation power (78.84) and less affected by radiation time (7.06). In a batch study, when the initial concentration of Zn(II) was increased, Zn(II) uptakes increased as well. On contrary, Zn(II) removal percentage decreased with the increase of Zn(II)’s initial concentration. Multilayer adsorption of Zn(II) onto CSAC had occurred since this adsorption system followed Freundlich isotherm the best, and the monolayer adsorption capacity, Q_m for Zn(II) was revealed to be 7.87 mg/g. The kinetic data of the Zn(II)-CSAC adsorption system was best described by pseudo-first-order (PFO) which indicated the role of physisorption. In the regeneration study, CSAC’s mass and Zn(II) adsorption uptakes had reduced from 100% to 37% and 77%, respectively, after 6 regeneration cycles.     

微波辐射活性炭负载磷钨酸催化合成季戊四醇双缩酮(醛)

在微波辐射下，以活性炭负载磷钨酸为催化剂，不用溶剂，合成了8种季戊四醇双缩酮（醛），以环己酮与季戊四缩的缩合为模型反应进行优化，其优化反应条件为：季戊四醇2．0g，催化剂0．3g，环己酮4．0mL，微波输出功率600W，辐射时间3min，产率达95．4％，该条件下的反应速度是常规加热反应速度的30倍，所得产物经元素分析，IR和1H NMR表征。     

Surface structural characterization of highly porous activated carbon prepared from corn grain

A novel corn grain precursor was used for the preparation of activated carbon by chemical activation. The detailed investigation of the porosity development in the prepared activated carbon was done by altering the various activation conditions such as the activation temperature, activation time and ratio between the powdered form of carbonized corn grain char and KOH. The surface characteristics including the surface roughness of all the activated carbon samples were evaluated from the analysis of nitrogen (N₂) adsorption isotherm data. At the maximum of 2978 m²/g, a super surface area having the corn grain‐based activated carbon (CG‐AC) was synthesized by using the following conditions: 1/4 ratio of powdered form of carbonized corn grain char/KOH; 800 °C; and 4 h. The possibility of preparing highly porous activated carbons with controlled porosity by varying different activation conditions was found from the pore size distribution results. In particular, the domination of the ratio between the powdered form of carbonized corn grain char and KOH on the porosity development was high compared to the activation temperature and activation time. In addition, the surface roughness calculated from the surface fractal dimension indicates the decrease of surface roughness with increasing activation conditions. Copyright © 2009 John Wiley & Sons, Ltd.