Hydrothermal conversion of rice husk ash to faujasite-types and NaA-type of zeolites

The faujasite-type of zeolites (NaX and NaY) and NaA-type of zeolite were synthesized from rice husk ash (RHA) via the hydrothermal conditions. The combustion of rice husk at controlled temperature of 600 °C for an hour in open air produce more than 90% of amorphous silica in the ash which was reactive towards the synthesis of zeolites. The formation of zeolite NaY from RHA is metastable and thus, the seeding and ageing effects in the synthesis of zeolite NaY were investigated to avoid the formation of zeolite A or P as the impurities in zeolite NaY. Zeolites NaX and NaA were also successfully synthesized with high purity, absence of impurities and other phases, and high reproducibility. Thus, the amorphous forms of silica in RHA can be used as a source of silica for the synthesis of faujasite-types and NaA-type of zeolites.     

Preparation of ZSM-12 Zeolite from RHS and Its Application for Synthesis of n-type ZnO Semiconductor Nanoparticles: A Green Chemistry Approach

White rice husk silica (RHS), an agriculture waste, was used as a silica source for ZSM-12 (MTW) zeolite synthesis. The ZSM-12 zeolite derived from RHS was prepared by hydrothermal method at 150 °C in the presence of tetraethylammonium hydroxide. Zinc oxide nanoparticles (NPs) were grown in zeolite substrates using a solid state reaction. The crystallization of ZSM-12 zeolite and ZnO/ZSM-12 nanocomposite (NC) was monitored by XRD, FTIR and SEM, TEM, and BET techniques. It was found that complete crystallization of ZSM-12 zeolite phase was achieved after 6 days. The XRD patterns declared the presence of both ZnO NPs and ZSM-12 zeolite in NC. The SEM image of ZSM-12 and NC demonstrated large spherical aggregates with size diameter of 2.5 µm. The TEM image of ZSM-12 showed formation of ZnO NPs with particle size ~?35 nm on ZSM-12 zeolite. The BET results indicated that pore volume and surface area of ZnO/ZSM-12 NC was bigger than ZSM-12 zeolite. On the basis of the obtained experimental results, it was founded that ZnO NPs were encapsulated into channels of ZSM-12 zeolite.

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Properties of zeolite Y in various forms and utilization as catalysts or supports for cerium oxide in ethanol oxidation

Zeolite Y in sodium form (NaY) was synthesized using silica source from rice husk, transformed to ammonium form (NH₄Y), and calcined to convert to proton form (HY). The direct conversion of NH₄Y to HY resulted in loss of the zeolite crystallinity and lower surface area. Thus, the NH₄Y was further used in the preparation of cerium (Ce) catalysts. The NH₄Y was also treated with a basic solution in an attempt to generate mesopores but only site defects were likely formed. The supported Ce catalysts with good Ce dispersion were prepared by wetness impregnation of Ce precursor solution on NaY, NH₄Y, and base-treated NH₄Y. Upon calcination, the generated catalysts were notated as Ce/NaY, Ce/HY, and Ce/YB. In catalytic testing on ethanol oxidation at varying temperature in a continuous laboratory-scale fixed-bed reactor, all the zeolites gave low ethanol conversion at 100–300 °C. The catalytic activity significantly improved with the presence of Ce. The Ce/YB showed the higher ethanol conversion and CO₂ yield than Ce/NaY and Ce/HY probably because of the presence of more local site defects on the zeolite.     

Co-combustion of coal and biomass in a circulating fluidized bed combustor

In this research, co-combustion of coal and rice husk was studied in a circulating fluidized bed combustor (CFBC). The effects of mixed fuel ratios, primary air and secondary air flow rates on temperature and gas concentration profiles along riser (0.1 m inside diameter and 3.0 m height) were studied. The average particle size of coal from Maetah used in this work was 1,128 mm and bed material was sand. The range of primary air flow rates was 480–920 l/min corresponding to U _g of 1.0–2.0 m/s for coal feed rate at 5.8 kg/h. The recirculation rate through L-valve was 100 kg/hr. It was found that the temperatures along the riser were rather steady at about 800–1,000 degrees Celsius. The introduction of secondary air improved combustion and temperature gradient at the bottom of the riser, particularly at a primary air flow rate below 1.5 m/s. Blending of coal with biomass, rice husk, did improve the combustion efficiency of coal itself even at low concentration of rice husk of 3.5 wt%. In addition, the presence of rice husk in the feed stocks reduced the emission of both NO _x and SO₂.     

Iron incorporated rice husk silica as a sorbent for hexavalent chromium attenuation in aqueous system

An environmentally benign metal oxide, Fe, was incorporated into silica derived from rice husk via the sol gel route and the physiognomies of both the modified (IRS) and raw rice husk derived silica (RHS) were studied via FTIR and XRD analysis and pH_PZC and surface area determinations. The stability of the Fe incorporated into the silica matrix, determined via the toxicity characteristic leaching procedure, showed that the integrity of the sorbent was intact only in basic medium but got vitiated in acidic medium. The sorption process conformed to the pseudo second order model than reversible first order and pseudo first order kinetic models and the rate of sorption of Cr(VI) onto either sorbents was determined by film diffusion. Process variables optimization showed that the amount of Cr(VI) removed per gram of sorbent reduced with increase in initial solution pH and the negative impact of the anionic interference was more in the presence of SO₃²⁻ than NO₃²⁻ and Cl⁻. The predicted Langmuir monolayer sorption capacity (mg/g) of the IRS (63.69) was higher than that of the RHS (61.35). The value of the mean free energy (kJ/mol) of sorption, obtained for IRS (267.26) and RHS (100.00), and the significant changes in the peak positions of specific functional groups on the Cr(VI) laden sorbents showed that chemisorption was the dominant mechanism of Cr(VI) uptake.     

Microwave Versus Conventional-Hydrothermal Synthesis of NaY Zeolite

This paper focuses on the synthesis of NaY zeolite crystals by using microwave-hydrothermal (M-H) processing. NaY zeolites were synthesized from colloidal silica, sodium aluminate, sodium hydroxide and deionized water at 100°C, and some properties were studied. NaY zeolite crystals with high surface area, in the range of 439 to 716 m²/g, have been prepared at 100°C for 1 to 3 hrs. Compared to the formation of NaY zeolite via conventional-hydrothermal (C-H) treatment, the M-H treatment led to increased rate of formation by 3 to 4 times.     

稻壳制备活性炭联产二氧化硅工艺

采用物理法将稻壳炭化,炭化料用酸碱处理,固体残渣经高温水蒸汽活化制备活性炭,脱灰液体采用沉淀法制备SiO2. 结果表明,用2.5 mol/L NaOH溶液按液固比10 mL/g脱灰的炭化料所制活性炭比表面积为961.8 m2/g,比不脱灰炭化料所制活性炭增加136%,总孔容积增加103.8%,对碘和亚甲基蓝的吸附容量分别为1270和300 mg/g. 在10% HCl、煅烧温度600℃条件下所制SiO2粒径为40~60 nm,为无定型结构,比表面积达330 m2/g,纯度达99.84%.     

球磨法制备超细稻壳二氧化硅

将稻壳用10％(体积分数)的盐酸处理后在600℃焚烧得到稻壳二氧化硅,再利用球磨法进行研磨,得到平均粒径为5.01 μm、分散度为1.31的超细稻壳二氧化硅粉体.研究了研磨时间、球料比和磨球直径对粉体粒径的影响,并对研磨前后粉体的性质、红外光谱(FTIR)及X-衍射图谱(XRD)进行了比较.结果表明:合适的球料比、磨球...     

Characteristics of natural rubber hybrid composites based on marble sludge/carbon black and marble sludge/rice husk derived silica

This paper discusses an extensive overview of characterization of marble sludge (MS) with carbon black (CB) and rice husk derived silica (RHS) in hybrid natural rubber (NR) composite. Cure characteristics, mechanical and swelling properties of MS/CB and MS/RHS hybrid NR composite were investigated. As CB and RHS content increases in weight ratio of MS/CB and MS/RHS a decrease in scorch and cure time and increase in the torque, tensile, tear, modulus, hardness, crosslink density were observed, while elongation at break and swelling coefficient decreased. The aging behavior of corresponding hybrid composite materials was also evaluated at two different temperatures.     

Single-step process without organic template for the formation of zeolite A from RHA

Dice-shaped zeolite A (NaA) was prepared via direct dissolution of rice husk ash (96.5% SiO₂) in the presence of NaOH and sodium aluminate solution by autoclave process at 90°C/6 h without using any templating agent. The prepared particles were characterized by DTA/TG, XRD, FTIR, N₂ adsorption-desorption physisorption analysis, FESEM, and TEM. XRD results confirmed crystallization of pure NaA zeolite phase. FTIR study shows the characteristic bands at 554 cm⁻¹ for double 4 membered ring (D4R) of NaA zeolite. The total BET surface area of the product was found to be 31.6 m² g⁻¹. FESEM and TEM images show dice shaped NaA particles of size around 1 μm which is formed via oriented crystalline aggregation of primary particles (30-40 nm). A tentative mechanism was proposed for the formation of NaA crystals through direct dissolution of rice husk ash. The synthesized NaA zeolite could be used for purification of alcohol and separation of toxic and radioactive ions from waste water via a cost-effective process.     

Bioactive assessment of bioactive glass nanostructures synthesized using synthetic and natural silica resources

The sol-gel route of synthesizing bioactive glasses of composition 45S5 has shown higher compatibility than the melt casting method. In bioactive glass synthesis, a major silica source is derived from the synthetic tetraethyl orthosilicate precursor. This work demonstrates the sol–gel-derived bioactive glass prepared from rice husk and TEOS as silica sources. In this study, the effect of crystallization with respect to the silica source in bioactive glass composition was investigated to gain further understanding on the processes involved in the fabrication of bioglass. The in vitro biodegradation and apatite formation of the bioactive glass in simulated body fluid was investigated by spectroscopic and morphological studies. Both the bioactive glasses show a change in morphology toward nanostructured apatite formation after in vitro immersion studies. Further, the hemocompatibility of bioactive glass prepared using rice husk is similar to bioactive glass prepared from organic silica sources. This promises the possibility of synthesizing low cost and biocompatible bioactive glass 45S5 system for tissue engineering applications.     

Synthesis of Silicon Carbide from Rice Husk in a dc Arc Plasma Reactor

SiC particles have been synthesized in the α-phase from a mixture of boiler-burnt rice husk and graphite powder in a dc extended arc plasma reactor on a 200–250 g scale. A SiC yield as high as 72% was achieved at a 3.03:1 carbon-to-silica ratio. 21R polytypism, which is rare to grow, was observed in the SiC. About 90% of the SiC particles produced were found to lie under 163 μm, 50% under 90 μm, and 10% under 28 μm size. Very fine particles under 10 μm size occurred to the extent of 3%. XRD and SEM characterizations were carried out to study the phase and morphology of the particles. Heterogeneous gas-phase reactions seem to be responsible for intermediate-size SiC particle growth in the multitemperature zone dc extended arc plasma reactor.     

Phase transition of mesoporous SiO<Subscript>2</Subscript> impregnated with an organic templating agent by post-synthetic microwave heating

Mesoporous silica SBA-15 samples were subjected to microwave heating for 10–40 min at 393 and 443 K after dry-impregnation with TPAOH (tetrapropylammonium hydroxide) to prepare a mesoporous material with zeolytically ordered pore walls. Physicochemical properties of the materials prepared were characterized by XRD, N₂ adsorption at 77 K, SEM, TEM, UV–vis and FT-IR spectroscopies. These investigations revealed that selective transformation of amorphous pore walls of SBA-15 to crystalline zeolytic phase is difficult to be achieved and a mixed phase of mesoporous silica/zeolite composite material was obtained, instead. Microwave heating time, temperature, TPAOH concentration, and hydrothermal stability of the mesoporous host materials tested (MCM-41, HMS, and SBA-15) were important factors to maintain the mesopore structure of the host materials during the post-synthetic microwave heating treatment.     

Synthesis of silica nanoparticles from Vietnamese rice husk by sol–gel method

Silica powder at nanoscale was obtained by heat treatment of Vietnamese rice husk following the sol–gel method. The rice husk ash (RHA) is synthesized using rice husk which was thermally treated at optimal condition at 600°C for 4 h. The silica from RHA was extracted using sodium hydroxide solution to produce a sodium silicate solution and then precipitated by adding H₂SO₄ at pH = 4 in the mixture of water/butanol with cationic presence. In order to identify the optimal condition for producing the homogenous silica nanoparticles, the effects of surfactant surface coverage, aging temperature, and aging time were investigated. By analysis of X-ray diffraction, scanning electron microscopy, and transmission electron microscopy, the silica product obtained was amorphous and the uniformity of the nanosized sample was observed at an average size of 3 nm, and the BET result showed that the highest specific surface of the sample was about 340 m²/g. The results obtained in the mentioned method prove that the rice husk from agricultural wastes can be used for the production of silica nanoparticles.     

稻壳一次煅烧水热合成P型分子筛

稻壳经稀盐酸煮沸后,用去离子水洗涤至中性,干燥后粉碎并与一定质量的Na2CO3和Al(OH)3粉末混合均匀置于马弗炉中煅烧,煅烧产物采用水热合成法合成P型分子筛.研究发现(SiO2占干燥酸洗稻壳质量分数的20％)当煅烧温度为850℃,煅烧时间为8h,Na2 O/SiO2＝1.2,SiO2/Al2 O3＝4.0,H2 O...     

高岭土原位晶化中物料迁移研究

原位晶化工艺就是利用偏高岭土和高岭土中具有化学反应活性的SiO₂和Al₂O₃,作为合成NaY分子筛的硅源和铝源,在碱性条件下水热合成Y型分子筛。通过对碱抽提高岭土组分特性变化的研究,对原位晶化过程中的物料迁移进行了探讨。研究表明,晶化开始时,固相中的活性SiO₂和Al₂O₃快速向液相中迁移,但氧化钠却由液相向固相迁移;随着晶化时间的延长,液相中的硅、铝和钠逐渐减少。     

Synthesis of ZSM-5 zeolite and silicalite from rice husk ash

Local rice husk was precleaned and properly heat treated to produce high purity amorphous SiO₂ for use in the synthesis of ZSM-5 zeolite and silicalite by hydrothermal treatment (150 °C) of the precursor gels (pH 11) under autogenous pressure in a short reaction time (4–24 h). A wide range of SiO₂/Al₂O₃ molar ratios (30–2075) and a small template content were employed to fully exploit the potential of rice husk ash (RHA). The mineralogical phases, morphology, specific surface area and pore volume of the synthesized products were investigated by XRD, FT-IR, SEM and BET analyses, respectively. Under the employed conditions, it was found that the gels with a low range of SiO₂/Al₂O₃ molar ratios (<80) produced an amorphous phase to poorly crystalline ZSM-5 zeolite; those with a medium range (80–200) favored well crystalline ZSM-5 zeolite production with a large surface area; whilst those with a high range of SiO₂/Al₂O₃ molar ratios (>200) yielded silicalite. The increase in Na₂O content, which was derived from the addition of NaAlO₂ to attain the desired SiO₂/Al₂O₃ molar ratio of the gel, did not significantly enhance the crystallization rate, crystallinity, or yield of products. On the contrary, these properties were greatly affected by the increase in the SiO₂/Al₂O₃ molar ratio.     

A study on the thermal behavior of low silica X-type zeolite ion-exchanged with alkaline earth cations

Pure and high crystalline low silica X-type zeolite with Si/Al ratio of 1 was synthesized under specific hydrothermal conditions. After preparation and characterization of Na form of the zeolite (Na-LSX) from the synthesized zeolite, Na cations were exchanged by three alkaline earth cations. The amount of the exchanged cations per 1 g of the zeolite for each cation was determined by wet chemical method. Among the various prepared samples, those containing approximately equal amount of different cations were selected and characterized by XRD, IR, and XRF techniques. TGA/DTG/DTA and XRD techniques were employed to investigate thermal behavior of the cation exchanged zeolites.     

The role of solvents in the imbibition of ascorbic acid by zeolites

Ascorbic acid is commonly used as an antioxidant agent in form of a powder. This allows the immediate availability of the molecule but cannot avoid the rapid inactivation of the excess. Sodium zeolites have frequently been proposed as agents for the controlled release of absorbed molecules. In order to prepare controlled release antioxidant agents, we treated sodium X and Y zeolites with ascorbic acid dissolved in organic solvents in order to establish how much acid they were able to retain and understand the retention and release mechanism. We found that the acid: (i) undergoes a dissociation and H⁺/Na⁺ exchange with zeolite; (ii) is retained as sodium salt while the zeolite is protonated; (iii) is released as a function of the sodium salt solubility into the solvent used. Thus, the imbibition was function of the nature of the solvent and, in aqueous-organic solvent mixtures, it was a direct function of the water concentration in the range 0–1% and an inverse function in the range 1–11%. It follows from above that, when sodium zeolite is used as a support for ascorbic acid, water percent in the range 0–11% may control the release as the ascorbate salt into aqueous–organic solvent mixtures.     

Adsorption of carbon dioxide using polyethyleneimine modified silica gel

To find an ideal adsorbent for carbon dioxide capture, a new polyethyleneimine modified silica gel material was synthesized with a simple procedure. Three silica gel materials with various particle sizes (15, 25 and 40–63 μm) were prepared and functionalized with polyethyleneimine. The carbon dioxide adsorption amounts of modified silica gel and non-modified silica gel were calculated using a mass balance equation at three different temperatures (298.15, 308.15 and 318.15 K), respectively, and the influence of gas pressure and particle size on adsorption was discussed. Experimental data showed that the carbon dioxide adsorption capacity of modified silica gel was better than non-modified silica gel, and the adsorption capacity gradually decreased with increasing particle size. The smaller particle size (15 μm) PEI modified silica gel had the largest adsorption capacity, at 298.15 K, and the adsorption amounts of various particle sizes of PEI-silica better fit the Langmuir isotherm model.