A facile method for production of high-purity silica xerogels from bagasse ash

In this paper, we systematically report the synthesis of mesoporous silica xerogels in high purity from bagasse ash. The bagasse ash was chosen as the raw material due to its availability and low-price, and environmental considerations also were important. Silica was extracted as sodium silicate from bagasse ash using NaOH solution. The sodium silicate was then reacted with HCl to produce silica gel. To produce high-purity silica xerogels, three different purification methods were investigated, i.e., acid treatment, ion exchange treatment, and washing with de-mineralized water. We were able to produce high-purity silica (>99 wt.%) by washing the produced gels with either de-mineralized water or with ion exchange resin. The specific surface area of the prepared silica xerogels ranged from 69 to 152 m² g^?1 and the pore volume ranged from 0.059 to 0.137 cm³ g^?1. The pore radii were 3.2–3.4 nm, which indicated that the silica xerogels was mesoporous. From the adsorption characterization, it was obvious that adsorptive capacity was better for high-purity silica xerogels compared with low-purity. The maximum adsorption capacity by high-purity silica xerogel was 0.18 g-H₂O/g-SiO₂. Finally, we demonstrate the potential of bagasse ash for mesoporous silica production with its excellent adsorptive capacity that makes it beneficial as an environmental solution.     

Preparation of carbon aerogel microspheres by a simple-injection emulsification method

Carbon aerogel microspheres were successfully prepared using a simple-injection emulsification method, employing sol–gel polycondensation of a resorcinol–formaldehyde solution containing sodium carbonate as a catalyst. This process was followed by solvent exchange using acetone, supercritical drying with carbon dioxide and carbonization in a nitrogen atmosphere. The effect of curing time before starting injection, injection rate and agitation rate of continuous phase on the particle size and the porous properties of the carbon aerogel microspheres was investigated. Adsorption of phenol by using the prepared carbon aerogel microspheres was also examined. The diameter of carbon aerogel microspheres was controlled in the range of 20–55 μm by varying injection rate and agitation rate. The mean diameter of carbon aerogel microspheres decreased with increasing the injection rate and the agitation rate, whereas their mean diameter was independent of the curing time. The BET surface area and total pore volume of carbon aerogel microspheres increased with increasing the curing time. In contrast, their BET surface area and total pore volume decreased with increasing the injection rate and the agitation rate. The BET surface area, total pore volume, mesopore volume and micropore volume of the carbon aerogel microspheres with a mean diameter of 45 μm were 903 m²/g, 0.60 cm³/g, 0.31 cm³/g and 0.27 cm³/g, respectively. The phenol-adsorption capacity of these carbon aerogel microspheres was 29.3 mg phenol/g adsorbent.     

A facile method for the production of high-surface-area mesoporous silica gels from geothermal sludge

Mesoporous silica gels were successfully produced from geothermal sludge by alkali extraction followed by acidification. The silica in the geothermal sludge was dissolved by NaOH solution to produce a sodium silicate solution, which was then reacted with HCl or tartaric acid to produce silica gels. The effects of silica concentration and pH on the silica gel properties were investigated. In addition, an improved method was proposed by incorporating two-step aging. The first aging step, which was conducted at pH 10, was used to induce Ostwald ripening to increase the size of the primary particles, and the second step was used to strengthen the gel network. Decreasing the silica concentration by diluting the as-prepared sodium silicate solution tended to increase the surface area and pore volume of the prepared silica gels. The silica gels produced by tartaric acid possessed higher surface area and pore volume than those by HCl. The surface area and pore volume reached approximately 450 m² g⁻¹ and 0.8 cm³ g⁻¹, respectively. When the gelation pH was decreased to 6, the surface area exceeded 600 m² g⁻¹. The first aging process increased the size and uniformity of the primary particles, which in turn increased the surface area of the particles. The pore diameter for all cases was greater than 5 nm, indicating that the silica gels were mesoporous.     

Investigation of the effect of rice husk derived Si/SiC on the morphology and thermal stability of carbon composite aerogels

Highly porous carbon aerogels were prepared by pyrolyzing the novolac–silica aerogels. The silica phase was extracted from rice husk ash (RHA). The polymer aerogel was synthesized via the novel method of sol–gel polymerization in solvent vapor-saturated atmosphere. This method removes the need for supercritical drying and reduces the shrinkage of aerogels during drying stage and also has much lower process time compared to the conventional sol–gel method. In the next step, polymer composite aerogels become carbon/silica and carbon/silica/silicon carbide composites in pyrolysis (800 °C) and carbothermal reduction (1500 °C) stages, respectively. The characterization of the prepared composite aerogels was performed by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) analyses, respectively. Thermal and mechanical properties of the samples were investigated by differential scanning calorimetry (DSC) and compressive strength analysis. The resultant composite aerogels show a nanostructure with high porosity (above 82%) and low density (below 0.3 g cm^− 3). Si mapping images showed the good distribution of silica phase throughout the carbon matrix. Also the rate of oxidation for carbon composites decreased by silica incorporation and oxidation temperature increased about 20% by adding RHA silica. Compressive strength of composite samples increased about 25% by increasing RHA silica phase content.     

Nanoporous carbon synthesized from sol–gel template for adsorbing gibberellic acid in aqueous solution

A novel method, based on dynamic carbonization and silica template formed by sol–gel, was developed to prepare nanoporous carbon materials with tailored pore structures. The effects of the sol–gel reaction and carbonization process on the final nanoporous carbon product were investigated by pore features such as specific surface area, the total pore volume, and pore size distribution, which were systemically characterized by iodine index, transmission electron microscopy, and nitrogen adsorption. The experimental results indicate that the pore structures of the prepared nanoporous carbon are tunable on the nano-scale by controlling the preparation process in the proposed method. The nanoporous carbon prepared under the optimal conditions has a high total pore volume of 1.26 cm³/g, a large specific surface area of 1744 m²/g, and a maximal adsorption capacity of 9.2 mg/g to gibberellic acid in aqueous solution, which is nearly 6 times that of commercial activated carbon.     

Compressive strength and microstructural characteristics of class C fly ash geopolymer

Geopolymers prepared from a class C fly ash (CFA) and a mixed alkali activator of sodium hydroxide and sodium silicate solution were investigated. A high compressive strength was obtained when the modulus of the activator viz., molar ratio of SiO₂/Na₂O was 1.5, and the proper content of this activator as evaluated by the mass proportion of Na₂O to CFA was 10%. The compressive strength of these samples was 63.4 MPa when they were cured at 75 °C for 8 h followed by curing at 23 °C for 28 d. In FTIR spectroscopy, the main peaks at 1036 and 1400 cm^?1 have been attributed to asymmetric stretching of Al–O/Si–O bonds, while those at 747 cm^?1 are due to the Si–O–Si/Si–O–Al bending band. The main geopolymeric gel and calcium silicate hydrate (C–S–H) gel co-exist and bond some remaining unreacted CFA spheres as observed in XRD and SEM–EXDA. The presence of gismondine (zeolite) was also observed in the XRD pattern.     

Rapid synthesis of ordered hexagonal mesoporous silica and their incorporation with Ag nanoparticles by solution plasma

Rapid synthesis of silica with ordered hexagonal mesopore arrangement was obtained using solution plasma process (SPP) by discharging the mixture of P123 triblock copolymer/TEOS in acid solution. SPP, moreover, was utilized for Ag nanoparticles (AgNPs) incorporation in silica framework as one-batch process using silver nitrate (AgNO₃) solution as precursor. The turbid silicate gel was clearly observed after discharge for 1 min and the white precipitate formed at 3 min. The mesopore with hexagonal arrangement and AgNPs were observed in mesoporous silica. Two regions of X-ray diffraction patterns (2θ < 2° and 2θ = 35–90°) corresponded to the mesoporous silica and Ag nanocrystal characteristics. Comparing with mesoporous silica prepared by a conventional sol–gel route, surface area and pore diameter of mesoporous silica prepared by solution plasma were observed to be larger. In addition, the increase in Ag loading resulted in the decrease in surface area with insignificant variation in the pore diameter of mesoporous silica. SPP could be successfully utilized not only to enhance gelation time but also to increase surface area and pore diameter of mesoporous silica.     

Non-hydrothermal synthesis of mesoporous materials using sodium silicate from coal fly ash

Siliceous mesoporous materials with pores of ordered 2-D hexagonal structure were successfully prepared without hydrothermal treatment from condensation–polymerization of various concentration of quaternary ammonium salt as structure directing agents and silica precursor from the supernatant of coal fly ash (CFA) in the presence of catalyst. The synthesized materials had high surface area of ca. 740 m² g⁻¹ and pore volume of ca. 0.42 mL g⁻¹. The synthesized material exhibited a narrow size pore distribution and the mean pore diameter as measured by Dollimore–Heal method was about 2.3 nm. The formation of ammonium salt that act as precipitant during the synthesis enable the hydrolysis and co-condensation of the sodium silicate at room temperature.     

Effect of circulating fluidized bed combustion ash on the properties of roller compacted concrete

Circulating fluidized bed combustion (CFBC) ash, which has such a high content of f-CaO and SO_3, is a waste or by-product of petroleum coke combustion power stations. The purpose of this study is to investigate the effects of CFBC ash on the properties of roller compacted concrete (RCC). CFBC ash was used to replace fine aggregate with various dosages (5%, 10% and 15%) by weight. All mixtures were designed according to ACI 211.3R and prepared for testing. During casting, cylinders were vibrated and compacted with different pressures of 25 g/cm², 50 g/cm² and 75 g/cm², respectively. Test results show that CFBC ash can increase the water absorption and effectively reduce the initial surface absorption. Meanwhile, CFBC ash has a positive effect on compressive strength, splitting tensile strength, and sulphate attack resistance of hardened RCC. SEM revealed that the main hydration products of specimens containing CFBC ash are AFt (ettringite), C–S–H (hydrated calcium silicate) and portlandite. Based on the presented observations and results, RCC with the dosage of 5% CFBC ash as fine aggregate replacement and the roller compaction pressure of 75 g/cm² is recommended.     

Extremely high surface area of ordered mesoporous MCM-41 by atrane route

Silatrane synthesized from inexpensive oxide precursor, silica and TEA was used as the precursor for MCM-41 synthesis at low temperature because of its stability in aqueous solutions. Using cationic surfactant hexadecyltrimethyl ammonium bromide (CTAB) as a template, the resulting meso-structure mimics the liquid crystal phase. Varying the surfactant concentration, ion concentration and temperature of the system, changes the structure of the liquid crystal phase, resulting in different pore structures and surface area. After heat treatment, very high surface area mesoporous silica was obtained and characterized using XRD, BET and TEM. XRD and TEM results show a clear picture of hexagonal structure. The surface area is extraordinarily high, up to more than 2400 m² g⁻¹ at a pore volume of 1.29 cm³ g⁻¹. However, the pore volume is up to 1.72 cm³ g⁻¹ when the surface area is greater than 2100 m² g⁻¹.     

Synthesis of electrically active biopolymer–SiO2 nanocomposite aerogel

Silica nanoparticles encapsulated acacia gum–silica (AgSiO₂) composites were synthesized through sol–gel method using tetraethyl orthosilicate (TEOS) as silica precursor in basic condition. The nanocomposite gels were dried at different temperatures to form aerogels. The incorporation of nanostructured silica will influence the electronic behavior of composite. The composition of silica with acacia gum was tailored to optimize the material having good electronic properties. The resulting material was characterized by FTIR, XRD and AFM. The control curing of the composite resulted to mesoporous material with nanosize silica. At optimum composition, electrical conductivity and ion transference number of hybrid material are found to be 18.3 × 10^− 2 Scm^− 1 and 4.26 × 10² cm² V^− 1 s^− 1 respectively. The electrical conductivity of biopolymeric hybrid is comparable to that of commercially used synthetic conducting polymers. The ion transfer number of AgSiO₂ nanocomposites attributes the superionic character for electrical conduction.     

Preparation and characterization of silica aerogels from oil shale ash

The silica aerogels were successfully synthesized using oil shale ash which is a by-product of oil shale processing via ambient pressure drying. The physical and textural properties of the silica aerogels have been investigated and discussed. The results showed that the organic modification of hydrogels was a crucial step during the processing which preserved mesopores in ambient pressure drying. The unmodified hydrogel underwent tremendous shrinkage during the drying and yielded microporous silica aerogel. Using this novel route, it could produce silica aerogel with low tapping density of 0.074 g/cm³, high specific surface (909 m²/g) and cumulative pore volume of 2.54 cm³/g. From the industrial point of view, the present process is quite suitable for a large scale production of powdered silica aerogel. Furthermore, it provides a new way to solve the problem of oil shale ash pollution.     

Synthesis of low-density silica gel at ambient pressure: Effect of heat treatment

A silica gel with the density of 0.2 g/cm³ and porosity of 90% was synthesized. The silica wet gel was dried and heat-treated under the ambient pressure after modification of the surface by TMCS. The specific surface area and total pore volume of the dried gel increased with increasing heat treatment temperature and represented the maximum value of 1050 m²/g and 3.2 cm³/g, respectively, under 350 °C. The surface characteristic of the gel was hydrophobic when heat-treated in nitrogen and converted to hydrophilic after heat-treatment in air. As the result of pore characteristics, and microstructure of gel, the properties of the gel were considered to be similar to those of conventional aerogel.     

Synthesis and surface characteristics of nanosilica produced from alkali-extracted rice husk ash

Rice husk is a form of agricultural biomass that provides an abundant silicon source. This study used rice husk as a raw material to prepare nanosilica without adding an extra surfactant. This work investigated a dissolution-precipitation technique as a function of acid treatment, sodium silicate concentration, gelation pH, aging temperature, and aging time to establish optimum conditions for preparing silica nanoparticles. Experimental results showed that silica produced by hydrochloric acid possesses higher surface area than that of sulfuric, oxalic, and citric acids. Surface characteristics of the sample depend mainly upon gelation pH. The highest surface area and pore volume of silica samples were 634 m²/g and 0.811 cm³/g. Pore diameters were controllable from 3 to 9 nm by adjusting the solution pH value. Particles had a uniform size of 5-30 nm. The objective of this study was to develop a method of nanosilica preparation that enhances the economic benefits of re-using rice husk waste.     

Aramid fibers reinforced silica aerogel composites with low thermal conductivity and improved mechanical performance

Aramid fibers reinforced silica aerogel composites (AF/aerogels) for thermal insulation were prepared successfully under ambient pressure drying. The microstructure showed that the aramid fibers were inlaid in the aerogel matrix, acting as the supporting skeletons, to strengthen the aerogel matrix. FTIR revealed AF/aerogels was physical combination between aramid fibers and aerogel matrix without chemical bonds. The as prepared AF/aerogels possessed extremely low thermal conductivity of 0.0227 ± 0.0007 W m⁻¹ K⁻¹ with the fiber content ranging from 1.5% to 6.6%. Due to the softness, low density and remarkable mechanical strength of aramid fibers and the layered structure of the fiber distribution, the AF/aerogels presented nice elasticity and flexibility. TG–DSC indicated the thermal stability reaching approximately 290 °C, can meet the general usage conditions, which was mainly depended on the pure silica aerogels. From mentioned above, AF/aerogels present huge application prospects in heat preservation field, especially in piping insulation.     

High surface area sol–gel nano silica as a novel drug carrier substrate for sustained drug release

Among various carrier materials for drug delivery, silica has been found to be significant for loading and sustained release of the drug. In the present study, the antibiotic gentamicin was incorporated in various amounts on to a silica matrix, using a sol–gel subcritical drying route. Crack free silica rods with a length of 1–1.5 cm, diameter of 0.5 cm and density of 1.35 g/cm³ incorporated with gentamicin were obtained. The incorporation of gentamicin into the silica matrix was revealed by FTIR. The adsorption–desorption isotherms and pore size distribution were studied in detail. The drug elution patterns were analysed and show a biphasic mode of release. After the initial burst release, a constant release pattern is observed. A release value above the minimum inhibitory concentration (MIC) is always maintained. The amount of drug released is higher than that of many other bioactive ceramic materials. An attempt has been made to correlate the functional properties with the porosity features.     

Preparation of silica fibers and non-woven cloth by electrospinning

Silica fibers, which can potentially be used as filters and media for catalysts immobilization, were successfully spun via electrospinning process with precursor prepared through the sol–gel synthesis. Spinnable sols can be obtained only when the molar ratio of water to TEOS is less than 2 which is consistent with the retrospective results derived for other spinning methods. It was confirmed for the first time that the reaction time can be drastically reduced by introducing humidified air, controlled by KCl saturated aqueous solution, during sol–gel process. The size of obtained silica fibers is about 4.5 μm and has a certain degree of flexibility and mechanical strength. Although the specific surface area of as spun fiber was 7.7 m²/g, which is apparently small comparing to generic silica, treatment by boiling water only for 5 min could increase the specific surface area to be about 500 m²/g.     

Spectroscopic properties of Tm3+/Al3+ co-doped sol–gel silica glass

Tm³⁺/Al³⁺ co-doped silica glass was prepared by sol–gel method combined with high temperature sintering. Glasses with compositions of xTm₂O₃–15xAl₂O₃–(100 − 16x) SiO₂ (in mol%, x = 0.1, 0.3, 0.5, 0.8 and 1.0) were prepared. The high thulium doped silica glass was realized. Their spectroscopic parameters were calculated and analyzed by Judd–Ofelt theory. Large absorption cross section (4.65 × 10⁻²¹ cm² at 1668 nm) and stimulated emission cross section (6.00 × 10⁻²¹ cm² at 1812 nm), as well as low hydroxyl content (0.180 cm⁻¹), long fluorescence lifetime (834 μs at 1800 nm), large σ_em × τ_rad (30.05 × 10⁻²¹ cm² ms) and large relative intensity ratio of the 1.8 μm (³F₄ → ³H₆) to 1.46 (³H₄ → ³F₄) emissions (90.33) are achieved in this Tm³⁺/Al³⁺ co-doped silica glasses. According to emission characteristics, the optimum thulium doping concentration is around 0.8 mol%. The cross relaxation (CR) between ground and excited states of Tm³⁺ ions was used to explain the optimum thulium doping concentration. These results suggest that the sol–gel method is an effective way to prepare Tm³⁺ doped silica glass with high Tm³⁺ doping and prospective spectroscopic properties.     

The effects of a hydrochloric acid pre-treatment on the physicochemical properties and pozzolanic performance of rice husk ash

This paper investigates the effects of acid normality (0.01–6 N HCl) and combustion retention time (0.25–16 hours) on the pozzolanic properties of pre-combustion acid-treated rice husk ash. The pozzolanic reactivity was quantified by adding ground ash to saturated Ca(OH)₂ solutions and monitoring the time-dependent electrical conductivity and pH of the solutions. Also, the strength activity of ashes from different processes was measured by testing the compressive strength of mortars. It was observed that acid treatment results in ashes with higher SiO₂ content, lower alkali and unburned carbon content, better grindability, and smaller particle size, in comparison with ash from non-acid treated husks. Acid leaching increased the lime reactivity of the ashes and decreased their sensitivity to prolonged combustion times. Further, acid treatment with 0.01 N HCl was found to be sufficient, as the use of stronger acids did not considerably improve the pozzolanic reactivity of rice husk ash.     

Recovery of high surface area mesoporous silica from waste hexafluorosilicic acid (H2SiF6) of fertilizer industry

In this article we report recovery of mesoporous silica from the waste material (hexafluorosilicic acid) of phosphate fertilizer industry. The process involves the reaction of hexafluorosilicic acid (50 ml, 24 wt% H₂SiF₆) and 100 ml, 0.297 M Na₂CO₃ to generate the alkaline aqueous slurry. Silica was separated from the slurry by filtration and the sodium fluoride was extracted from the aqueous solution by evaporation method. The obtained mesoporous silica was characterized by N₂ absorption/desorption (BET), thermogravimetric analysis (TGA), X-ray diffraction (XRD), scanning electron microscope (SEM), and EDS. The results confirm that the separation of silica and NaF was successful and the final products have high purity. The silica product was found to have an average pore diameter of 4.14 nm and a high surface area (up to 800 m²/g). The process reported in this study may significantly reduce the release of hazardous materials into the environment and it might confer economic benefits to the responsible industries.