Synthesis of bimodal mesoporous carbon nanospheres for methyl orange adsorption

Mesoporous materials with bimodal mesopores show advantages in adsorption, energy storage, and catalysis because such unique structures are beneficial to the mass transfer. Here, we describe the synthesis of bimodal mesoporous carbon nanospheres (BMCSs) by using phenolic resin as carbon precursor, triblock copolymer Pluronic F127 as the soft template, and mesoporous silica spheres as hard templates. The BMCSs with uniform spherical morphology, high specific surface area (1489 m² g^??1), large pore volume (0.92 cm³ g^??1), and bimodal mesoporous structure (3.8 and 6.8 nm) exhibit promising properties for adsorption of methyl orange (MO). The maximum adsorption capacity of the BMCSs is 5.5?×?10² ± 0.2?×?10² mg g^??1, which is higher than that of many adsorbents reported. The kinetics studies show a better fit of pseudo-second-order model. Meanwhile, fitting equilibrium data show that the Langmuir model is more suitable to describe the MO adsorption than Freundlich model.     

Synthesis and characterization of mesoporous graphite carbon,and adsorption performance for benzene

In this paper, graphite carbon with a mesoporous structure was synthesized using the template–catalysis procedure with hydrated metal oxide nanoparticle as template and catalyst, phenol and formaldehyde as carbon source. XRD, Raman, BET and TEM analyses were performed to study the effluence of synthetic conditions on the structure of samples. The adsorption performances for benzene vapor were evaluated. The results show that CCo and CFe samples have mesoporous graphitized carbon structures. The molar amount of template to carbon source significantly affects the specific surface area, pore structure and adsorption–desorption performance. The specific surface area of CCo-1, with the best graphite structure, was 287.638 m²/g, the pore size was 19.075 nm, and the adsorption capacity for benzene vapor was 19.615 mmol/g. The synergistic effect between the cobalt element and graphite carbons affects the adsorption capacity of CCo-3, which was 34.643 mmol/g. However, the desorption efficiency was only 89 %, and the adsorption performance of CCo-3 material was degraded greatly after three times run.     

Worm-hole structured mesoporous carbon monoliths synthesized with amphiphilic triblock copolymer

In the present work, mesoporous carbon monoliths with worm-hole structure had been synthesized through hydrothermal reaction by using amphiphilic triblock copolymer F127 and P123 as templates and resole as carbon precursor. Synthesis conditions, carbonization temperature and pore structure were studied by Fourier transform infrared, thermogravimetric analysis, transmission electron microscopy and N₂ adsorption–desorption. The results indicated that the ideal pyrolysis temperature of the template is 450 °C. The organic ingredients were almost removed after further carbonized at 600 °C and the mesoporous carbon monoliths with worm-hole structure were obtained. The mesoporous carbon synthesized with P123 as single template exhibited larger pore size (6.6 nm), higher specific surface area (747 m² g^?1), lower pore ratio (45.9 %) in comparison with the mesoporous carbon synthesized with F127 as single template (with the corresponding value of 4.9 nm, 681 m² g^?1, 49.6 %, respectively), and also exhibited wider pore size distribution and lower structure regularity. Moreover, the higher mass ratio of template P123/resole induced similar pore size, larger specific surface area and lower pore ratio at the same synthesizing condition. It was also found that the textural structure of mesoporous carbon was affect by calcination atmosphere.     

Hydrothermal synthesis of mesoporous carbons for adsorption of two alkaloids

Two mesoporous carbons were synthesized via a hydrothermal treatment approach, characterized and evaluated for adsorption properties of berberine hydrochloride and matrine from water. The mesoporous carbons have BET specific surface areas of 1568.1 and 769.3 m²/g, pore volumes of 1.44 and 0.89 cm³/g, average pore diameters of 3.75 and 8.22 nm, and few O-containing functional groups on the surfaces. Both the mesoporous carbon adsorbents can effectively adsorb berberine hydrochloride and matrine from aqueous solutions, the higher equilibrium adsorption capacities of berberine hydrochloride and matrine at 298 K are 385, and 275 mg/g at 0.10 mg/mL, respectively. Adsorption enthalpy, entropy and free energy of berberine hydrochloride and matrine on the selected mesoporous carbon (with higher BET specific surface area and pore volume) were calculated. The adsorption of berberine hydrochloride and matrine on the selected carbon sample is fast at 298 K, 95% of the adsorption equilibrium could be achieved within 180 and 120 min, respectively. The dynamic adsorption capacities on the selected adsorbent are calculated to be 343.1 and 383.4 mg/g for berberine hydrochloride and matrine, respectively; and 70.8% of the adsorbed berberine hydrochloride and 79.2% of the adsorbed matrine could be desorbed by a 70% alcohol solution. These results provide a reference to the large-scale industrial production and application of mesoporous carbons as potential adsorbents in purification of alkaloids from herbal plant extracts.     

Activated carbon from bacterial cellulose as an effective adsorbent for removing dye from aqueous solution

ABSTRACT

Novel activated carbon (AC) derived from bacterial cellulose (BC-AC) was produced by phosphoric acid activation at a carbonization temperature of 500 °C. BC-AC possesses mesoporous structures of 2.3 nm in diameter, porosity of 1.0 cm³/g and surface area of 1734 m²/g with high thermal stability between 100 and 500 °C. BC-AC could be used as an effective adsorbent for removing methylene blue (MB) from aqueous solutions with the maximum adsorption capacity of 505.8 mg/g. BC-AC presented physisorption and the adsorption of MB was most likely to be a monolayer adsorption. The Redlich–Peterson model displayed the best fit with the experimental data.     

PRODUCTION AND CHARACTERIZATION OF POROUS CARBON FROM DATE PALM SEEDS BY CHEMICAL ACTIVATION WITH H3PO4: PROCESS OPTIMIZATION FOR MAXIMIZING ADSORPTION OF METHYLENE BLUE

The potential of date palm pits to be a suitable precursor for preparation of porous carbon was explored in the present work, utilizing phosphoric acid as the activating agent. Experimental methods reported in the literature were chosen with certain modifications in order to simplify the process. Process optimization was performed using the popular response surface methodology (RSM) adopting a Box-Behnken design. Process optimization was intended to maximize the porous carbon yield and the methylene blue (MB) adsorption capacity, with the process variables being the activation temperature, impregnation ratio (IR), and activation time. The structural characteristics were assessed based on nitrogen adsorption isotherms, SEM, and FT-IR, while the adsorption capacity was estimated using MB adsorption. The optimized experimental conditions were identified to be an activation temperature of 400°C, IR of 3, and activation time of 58 min, with the resultant porous carbon having a yield of 44% and MB adsorption capacity of 345 mg/g. The structural characteristics of the porous carbon reveal the BET surface area to be 725 m²/g, with pore volume of 1.26 cc/g, an average pore diameter of 2.91 nm, and total micropore volume of 0.391 cc/g. The popular Langmuir and Freundlich adsorption isotherm models were tested, and a maximum monolayer adsorption capacity of MB was estimated to be 455 mg/g, which compares with the highest for MB reported in literature, evidencing the suitability of porous carbon for adsorption of macromolecular compounds. The low activation temperature and activation time with highest yield render the process technically and economically attractive for commercial use.     

Hierarchical porous nitrogen-doped carbon materials derived from one-step carbonization of polyimide for efficient CO<Subscript>2</Subscript> adsorption and separation

Hierarchical porous nitrogen-doped carbon (HPNC) materials are synthesized through one-step carbonization of polyimide using triblock copolymer P123 as mesoporous template. The microstructure, chemical composition and CO₂ adsorption behaviors are investigated in detail. The results show that HPNC materials have hierarchical micro-/mesopore structures, high specific surface area of 579 m²/g, large pore volume of 0.34 cm³/g, and nitrogen functional groups (5.2 %). HPNC materials exhibit high CO₂ uptake of 5.56 mmol/g at 25 °C and 1 bar, which is higher than those of previously reported nitrogen-doped porous carbon materials. After 5 cycles the value of CO₂ adsorption uptakes is 5.28 mmol/g, which is approximately 95 % of the original adsorption capacity. The estimated CO₂/N₂ selectivity of HPNC materials is 17, revealing great promise for practical CO₂ adsorption and separation applications. The efficient CO₂ uptake and enhanced CO₂/N₂ selectivity are due to the combination of nitrogen-doped and hierarchical porous structures of HPNC materials.     

Removal of perfluorooctanoic acid from water by adsorption on high surface area mesoporous materials

Removal of perfluorinated alkylated substances (PFAS) such as perfluorooctanoic acid (PFOA) from aqueous solution is an actual topic in light of their widespread diffusion and their persistence in the environment. The process of adsorption has been identified as an effective technique to eliminate PFAS in water, however the process efficiency strongly depends on the adsorbents employed (silica, alumina, activated carbon, layer doubled hydroxides). In this work three nanostructured mesoporous silica materials of similar pore diameter (~4 nm) featuring high surface area (~900 m²/g) and high pore volume (0.7–1.0 mL/g) were evaluated in PFOA removal: calcined MCM-41 (MCM-41c), calcined hexagonal mesoporous silica (HMSc) and HMSe obtained after ethanol extraction of the amine templates from HMS. Sorption kinetics and isotherms were performed at PFOA concentrations from 10 µg/L to 10 mg/L. It appeared that HMSe showed much faster and higher adsorption capacity for PFOA than the other tested adsorbents (MCM-41c and HMSc) whatever the pH of the solution (5 < pH < 9). Thermogravimetric analysis of HMSe evidenced that the ethanol extraction of the templating amines was not complete (70 %) and HMSe possessed some remaining hexadecylamine (HDA) (0.08 mol amine per mol SiO₂) on the surface conferring some hydrophobic properties to the adsorbent and also some probable complex formation between anionic PFOA^? and protonated HDA. Indeed, the incomplete amine extraction is surely due to the presence of protonated HDA in strong electrostatic interactions with SiO^? avoiding their removal by simple ethanol extraction as for H-bonding amine with Si–OH groups. Considering both adsorption isotherms and adsorption kinetics, PFOA could be efficiently removed from contaminated water in a wide range of concentration by an environmental friendly adsorbent as HMSe.     

A novel carbon aerogel prepared for adsorption of copper(II) ion in water

A novel carbon aerogel with network pore and surface group of hydroxyl was prepared from cellulose colloid, through sol-gel reaction, freeze-drying and carbonization. Surfactant like isooctyl alcohol ether phosphate was taken as structure inducer in sol-gel reaction, for construction of porous network in the prepared samples. Characteristic of a specific area about 725.12 m²/g and total pore volume about 0.64 cm³/g, the prepared cellulose-based carbon aerogel of CCA₂, has a maximum capacity about 55.25 mg/g for Cu²⁺ in neutral aqueous solution. Its adsorption equilibrium can be reached within 10 min in an aqueous solution of pH7.0 at 25?°C, while desorption of Cu²⁺ need about 1 h eluted by HCl or HNO₃ solution of 0.01 M. And regeneration of the carbon aerogel in adsorption of Cu²⁺ can be repeated for five times, remaining 96% adsorption capacity. It is also found in adsorption process the kinetics nicely follows pseudo-second-order rate expression, and the isotherm fits Langmuir model.     

Ordered mesoporous carbon prepared from triblock copolymer/novolac composites

Ordered mesoporous carbon is synthesized by the organic–organic self-assembly method with novolac as carbon precursor and two kinds of triblock copolymers (Pluronic F127 and P123) as template. The hexagonal structure and a worm-hole structure are observed by TEM. The carbonization temperature is determined by TG and FT-IR. Characterization of physical properties of mesoporous carbon is executed by N₂ absorption–desorption isotherms and XRD. The mass ratios of carbon precursor/template affect the textural properties of mesoporous carbon. The mesoporous carbon with F127/PF of 1/1 has lager surface area (670 m² g^?1), pore size (3.2 nm), pore volume (0.40 cm³ g^?1), smaller microporous surface area (368 m² g^?1) and wall thickness (3.7 nm) compare to that with F127/PF of 0.5/1 (576 m² g^?1, 2.7 nm, 0.29 cm³ g^?1, 409 m² g^?1 and 4.3 nm, respectively). The mesoporous carbon prepared by carbonization at high temperature (700 °C) exhibits lager surface area, lower pore size and pore volume than the corresponding one obtained at 500 °C. The structure and order of the resulting materials are notably affected with types of templates. The mesoporous carbon with P123 as template exhibits worm-hole structure compare to that with F127 as template with hexagonal structure. In general, the pore size of mesoporous carbon with novolac as precursor is smaller than that with resorcinol–formaldehyde as precursor.     

Preparation of Activated Carbons from Tobacco Stems by Potassium Hydroxide Activation and Phosphine Adsorption

Activated carbon preparation from tobacco stems by KOH activation at different activation temperatures and KOH/char mass ratios were investigated in this study. The effects of preparation parameters on activated carbon pore structure, morphometrics, microcrystallinities, and surface functional groups were characterized by N₂ adsorption, SEM, XRD, and FTIR technologies, respectively. The optimum preparation condition of activated carbon was activation temperature of 850°C, and KOH/char mass ratio of 2. Under this condition, the BET surface area of 2215 m²/g, and the pore volume of 1.343 cm³/g can be obtained. Prepared activated carbon showed clearly honeycomb holes, and a predominated amorphous structure. With increase of activation temperature and KOH/char mass ratio, decrease of surface oxygen functional group, and aromatization of the carbon structure was found. The activated carbon was subject to PH₃ purification, and the maximum PH₃ adsorption capacity of 253 mg/g can be realized based on well prepared KOH-AC with modification of 2.5% Cu. It seems that the activated carbon produced from chemical activation of tobacco stem would be an effective and alternative adsorbent for PH₃ adsorption because of its high surface area, adsorption capacity, and low cost.     

Magnetically-separable hierarchically porous carbon monoliths with partially graphitized structures as excellent adsorbents for dyes

Magnetically-separable hierarchically porous carbon monoliths with partially graphitized structures were synthesized through confinement self-assembly in polyurethane (PU) foam associated with a direct carbonization process from triblock copolymer F127, phenolic resol and ferric nitrate. It was observed that the magnetic Fe nanoparticles were embedded in the walls of graphitic porous carbon matrix, and the resulting materials exhibited hierarchically porous structure with macropores of 100–450 μm, mesopore size of 4.8 nm, BET surface area of 723 m²/g, pore volume of 0.46 cm³/g, and saturation magnetization of 3.1 emu/g. Using methylene blue as model dye pollutant in water, the carbon monolith materials showed high adsorption capacity of 190 mg/g, exhibiting excellent adsorption characteristics desirable for the application in adsorption of dyes and easy separation under an external magnetic field.     

Removal of methyl orange from aqueous solutions with poly(acrylic acid-co-acrylamide) superabsorbent resin

Poly(acrylic acid-co-acrylamide) (P(AA-co-AM) superabsorbent resin was prepared by solution polymerization of acrylic acid (AA) and acrylamide (AM) using ammonium persulfate (APS) as an initiator and N,N′-methylenebisacrylamide (MBA) as a cross linker. P(AA-co-AM) was used for the removal methyl orange (MO) from aqueous solutions. Factors influencing the adsorption capacity, such as adsorption time, initial concentration of MO, dosage of the superabsorbent resin, pH value and ionic strength, were investigated in detail. It was found that P(AA-co-AM) was effective to remove MO from its aqueous solutions. The equilibrium adsorption capacity was 394.6 mg/g at room temperature as the initial concentration of MO was 3000 mg/L. The mechanism of the adsorption process was also speculated. Study on the equilibrium adsorption isotherms showed that the adsorption was in accordance with both Langmuir and Freundlich model. Further study of the adsorption kinetics showed that the adsorption process was consistent with the Pseudo second-order kinetic model.     

Characterization of graphene oxide supported porous silica for effectively enhancing adsorption of dyes

ABSTRACT

This paper reported the synthesis of graphene oxide (GO)/mesoporous SBA-15 nanocomposite with excellent adsorption properties. The samples were characterized by XRD, FESEM, TEM, FTIR, Raman spectrometer, and surface area analyzer. The adsorption study implied that incorporating GO into SBA-15 frameworks displayed much higher adsorption capacity levels than did pure SBA-15. The composite displayed uniform pore size (6.50 nm), large pore volume (1.035 cm³/g), and high surface area (891 m²/g). The adsorption capacity of samples decreased with increasing sample dosage and adsorption temperature, and increasing initial concentration of dye. The maximum adsorption capacity of the composite for methylene blue was found to be 242 mg/g. The removal efficiency reached 100%. The proposed method was simple and suitable for mass production.     

Adsorptive removal of methyl orange using mesoporous maghemite

In this work, mesoporous maghemite (γ-Fe₂O₃) was prepared by the thermal decomposition of [Fe(CON₂H₄)₆](NO₃)₃ with the aid of cetyltrimethyl ammonium bromide (CTAB), and its adsorption ability for the removal of methyl orange (MO) from wastewater was investigated. X-Ray powder diffraction (XRD) together with nitrogen adsorption–desorption measurements show the formation of mesoporous γ-Fe₂O₃ with an average pore size of 3.5 nm and a specific surface area of 93.0 m²/g. Magnetic measurements show that the mesoporous γ-Fe₂O₃ exhibits ferrimagnetic characteristics with the coercivity of 141.5 Oe and remanent magnetization of 7.3 emu/g and has the maximum saturation magnetization of 55.2 emu/g. The adsorption of MO on the mesoporous γ-Fe₂O₃ reaches the maximum adsorbed percentage of ca. 90% within a few minutes, showing that most of MO can be removed in a short time when the mesoporous γ-Fe₂O₃ is used as an adsorbent. When the pH of MO solution is varied from 3 to 11, the adsorbed percentage of MO decreases from ca. 90 to ca. 81%, showing that the adsorption is slightly influenced by solution pH. The adsorption data for MO fit well with either Langmuir or Freundlich adsorption models. The maximum adsorption capacity of the mesoporous γ-Fe₂O₃ for MO is determined to be 385 mg/g, which suggests that the material could be an excellent magnetic adsorbent for MO.     

Low‐Temperature Synthesis of Mesoporous SiC Hollow Spheres by Magnesiothermic Reduction

Mesoporous silicon carbide hollow spheres (SiC‐HS) with a large specific surface area (690.2 m² g^?1) are synthesized at a relatively low temperature of 650°C by magnesiothermic reduction using the template of carbon‐coated mesoporous silica hollow spheres and molten salt as the heat absorbent and solvent. The mesoporous SiC‐HS comprising many small primary crystals (2–4 nm) with a well‐maintained microstructure have good thermal stability and adsorption ability, and are promising as adsorbents to remove organic pollution from water. The synthesis technique can be extended to other nanostructured carbide ceramic materials.     

Preparation of High Surface Area Mesoporous Activated Carbon: Kinetics and Equilibrium Isotherm

Activated carbon prepared from palm shell by phosphoric acid impregnation, at significantly favorable experimental conditions is characterized for the porous nature and adsorption of methylene blue dye molecules. The activation is carried out using a 2-stage activation process with the activation in a self-generated atmosphere. An activation temperature of 500°C, with an activation time of 75 minutes using a phosphoric acid impregnation ratio of 3 has yielded an activated carbon having unique characteristics. An activated carbon with a yield of 48%, total pore volume of 1.9 cm³/g, surface area of 1956 m²/g, an average pore diameter of 3.8 nm, with the ratio of the mesopore to the total surface area in excess of 75% has been prepared. The activated carbon exhibits a high methylene blue equilibrium adsorption capacity of 438 mg/g with the adsorption isotherm increasing with an increase in the adsorption temperature. Among the various adsorption isotherm models, the Langmuir model is able to explain the adsorption process well, evidenced by the proximity of the model with the experimental data. Among the different kinetic models tested with the experimental kinetic data, a pseudo-second-order model is found to fit the experimental data with close proximity.     

Magnetic mesoporous carbon material with strong ciprofloxacin adsorption removal property fabricated through the calcination of mixed valence Fe based metal-organic framework

As an efficient and low cost adsorbent to remove fluoroquinolones antibiotics (such as ciprofloxacin and norfloxacin) in waste water, magnetic mesoporous carbon material has attracted increasing concern all over the world. Here, a convenient strategy to fabricate magnetic mesoporous carbon material has been explored with Fe containing metal-organic framework (MOF) as precursor. With this method, a magnetic mesoporous carbon material, Fe₃O₄/C , which possesses high surface area, is obtained through the calcination of a mixed valence Fe based MOF. For Fe₃O₄/C, its ciprofloxacin adsorption capacity reaches as high as 868.6 mg/g. Magnetic measurement reveals its ferromagnetic feature of Fe₃O₄/C with magnetization saturation 22.81 emu g^?1 and this guarantees its excellent magnetic separation performance. Furthermore, Fe₃O₄/C also exhibits outstanding stability during ciprofloxacin containing waste water treatment.     

Synthesis and characterization of monolithic carbon/silicon carbide composite aerogels

Resorcinol–formaldehyde/silica composite (RF/SiO₂) aerogels were synthesized using sol–gel process followed by supercritical CO₂ drying. Monolithic carbon/silicon carbide composite (C/SiC) aerogels were formed from RF/SiO₂ aerogels after carbothermal reduction. X-ray diffraction and transmission electron microscopy demonstrate that β-SiC was obtained after carbothermal reduction. Scanning electron microscopy and nitrogen adsorption/desorption reveal that the as-prepared C/SiC aerogels are typical mesoporous materials. The pore structural properties were measured by nitrogen adsorption/desorption analysis. The resulting C/SiC aerogels possess a BET surface area of 564 m²/g, a porosity of 95.1 % and a pore volume of 2.59 cm³/g. The mass fraction of SiC in C/SiC aerogels is 31 %.     

中孑L分布活性炭的制备与表征

以酚醛树脂为前驱体,纳米SiO2为模板剂,采用模板炭化和钾碱活化工艺研制中孔率较高、比表面积较大的中孔炭（Mesoporous carbon,MC）,考察了活化温度、活化时间、树脂模板比等工艺参数对活性炭孔结构的影响。测试了活性炭N2的吸附等温线、孔径分布、比表面积,并通过扫描电子显微镜观察其微观结构。结果表明,较优工艺条件为：树脂模板比为2：1、活化温度850℃、活化时间3h,该条件下所得中孔炭中孔率达91．4％,比表面积为1501m^2·g^-1,总孔孔容1．38m^2·g^-1,为理想的窄孔径分布活性炭。