Composite Water Sorbents of the Salt in Silica Gel Pores Type: The Effect of the Interaction between the Salt and the Silica Gel Surface on the Chemical and Phase Compositions and Sorption Properties

The influence of the inorganic salt-silica gel surface interaction on the chemical and phase compositions and sorption properties of composites of the salt in silica gel pores type is studied. Two possible interaction mechanisms are considered: (1) the ion-exchange adsorption of metal cations on the silica gel surface from a solution of a salt (CaCl₂, CuSO₄, MgSO₄, Na₂SO₄, and LiBr) and (2) the solid-phase spreading of a salt (CaCl₂) over the silica gel surface. The adsorption of metal cations on the silica gel surface in the impregnation step affords ≡Si-OM ⁿ⁺¹ surface complexes in the composites. As a result, two salt phases are formed in silica gel pores at the composite drying stage, namely, an amorphous phase on the surface and a crystalline phase in the bulk. The sorption equilibrium between the CaCl₂/SiO₂ system and water vapor depends on the ratio of the crystalline phase to the amorphous phase in the composite.     

Retention Behavior of Proteins on Glutamic Acid-Boned Silica Stationary Phase

A glutamic acid-bonded silica (Glu-silica) stationary phase with cation-exchange properties was synthesized using l-glutamic acid as ligand and silica gel as matrix. The effects of solution pH value, salt concentration and metal ion on the retention of proteins were examined. The standard protein mixture was separated with a prepared chromatographic column and an iminodiacetic acid column, and compared. The influence of the binding capacity of an immobilized metal ion on the complexation of metal chelate column was studied. The results indicate that the obtained column displays cation-exchange characteristic and better separation ability for proteins. As fixing metal ion on the Glu-silica column, retention of proteins on the column is a cooperative interaction of metal chelate and cation-exchange. The stationary phase shows the typical metal chelate properties with the increase of the sorption capacity of immobilized metal ion.     

Proton conductivity and interphase interaction in CsH2PO4-SrZrO3 composites

Microstructure, transport, and thermal properties of the composites of (1 ? x)CsH₂PO₄/xSrZrO₃ (x = 0.01–0.2) are studied. Introduction of highly dispersed strontium zirconate results in an increase in low-temperature conductivity by 1–3 orders of magnitude as depedent on the composition, leveling, and disappearance of a superionic phase transition in CsH₂PO₄. The methods of differential scanning calorimetry and thermogravimetry were used to show that a significant change in thermodynamic properties of CsH₂PO₄ in composites at x = 0.1–0.2 is observed due to salt amorphization. According to the data of X-ray phase analysis, there is no chemical interaction between the components and no new compounds are formed. An increase in conductivity is caused by salt disordering due to the interphase surface interaction.     

Magnetic Sorbent with a Mesoporous Shell for the Simultaneous Preconcentration of Ecotoxicants of Different Nature

A magnetic sorbent with a multilayer shell of the composition Fe₃O₄@TEOS@CTAB@TEOS + MPTEOS designed for the simultaneous or sequential preconcentration of components of various nature is obtained. The conditions of microwave synthesis and modification of a new magnetic sorption material are described; its composition and particle sizes are characterized. The sorption capacity of the sorbent is provided by creating a mesoporous silica layer filled with cetyltrimethylammonium bromide (CTAB) micelles and additionally modified with an S-containing polymer (MPTEOS) on the surface of the magnetic carrier. The properties of the obtained material with respect to the regulated substances from two groups of priority pollutants are studied: phenols of various structures and heavy metals. The main sorption characteristics (effect of pH, phase contact time, nature of eluent, V: m, salt background) are studied and the conditions for extracting ecotoxicants at their concentration in the solution at a level of μg/L are optimized. The data obtained under the conditions of separate and simultaneous extraction of analytes of different nature confirmed a possibility of the quantitative determination of various types of natural water pollutants at the levels significantly lower than the MPC using a single sorption material. In using HPLC methods and electrothermal atomic absorption spectrometry, a complete analysis of a single sample takes 40?50 min and of a series of samples, 2–3 h. Such characteristics, combined with the simplicity of material preparation make it promising for routine analytical studies.     

Determination of molybdenum using 1,5-diphenylcarbazone immobilized on silica

The sorption of 1,5-diphenylcarbazone on highly dispersed silica from toluene and acetone-hexane (1:4) solutions was studied. The nature of the bonding of the reagent with the surface of silica gel was studied by absorption spectrometry. A solid-phase reagent is proposed for the sorption-diffuse-reflection and visual test determinations of down to 0.025 and 0.05 μg/L molybdenum(VI), respectively. The procedures were used for the determination of molybdenum in sea salt and a medicinal preparation.     

Composite sorbents based on synthetic manganese oxide and carbon fiber

Manganese oxides have been prepared on the surface of carbon fiber by simple methods: coprecipitation of manganese salts of different valence in the presence of fiber as a support or electrodeposition from Mn(II) salt solution on a carbon fiber cathode, in the presence of chitosan including, under oxidation with air oxygen conditions. The obtained samples have been characterized by scanning electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy. Sorption properties of the composites toward As(V) have been studied. The relationships between sorption properties, structure, Mn valence, and manganese oxide surface morphology have been discussed.     

Fabrication of NiO coated SiO2 and SiO2 coated NiO for the removal of Pb2＋ ions

We have prepared silica,SiO2coated NiO and NiO coated SiO2by sol-gel method.The physicochemical properties of the desired materials were investigated by surface charge properties,scanning electron microscopy（SEM）,energy dispersive X-ray（EDX） spectroscopy,surface area measurements and X-ray diffraction（XRD） analyses.The point of zero charge（PZC） of the solid was determined by the salt addition method.In coated materials,two PZC values were noted representing the surface charge of their counterparts.The SEM image of SiO2coated NiO displays a uniform coating of silica on the surface of NiO whereas in case of NiO coated SiO2,a honeycomb like appearance was observed with highly porous structures.In the diffractograms of NiO,the characteristic peaks were suppressed in NiO coated silica however,no diffraction peak could be seen in SiO2coated NiO.Batch adsorption technique was applied for the removal of Pb2＋ions from aqueous solution.The sorption trend for Pb2＋ions was observed in the order of NiO coated SiO2〉 SiO2coated NiO 〉 NiO 〉 SiO2.This trend confirms that the coated materials have more sorption capacities than their parent counterparts.     

Effect of Temperature on Thermal Treatment of Silica Coated Magnetic Nanoparticles

In the quest for developing a catalyst with as many desired characteristics, a facile synthetic route was designed for the preparation of mesoporous silica coated magnetic nanoparticles(MSMNP) employing a colloid mill reactor. The composite particles were characterized by the techniques, such as nitrogen adsorption-desorption isotherms, scanning electron microscopy(SEM), transmission electron microscopy(TEM), X-ray diffraction patterns (XRD), thermo-gravimetric analysis(TGA), Fourier transform infrared spectroscopy(FTIR) and vibrating sample magnetometer(VSM), etc. The analysis showed that the resulted MSMNP composites were composed of silica shell layers with open pores connecting channels and NiFe₂O₄ with spinel structure, so the thermal treatment temperature did not show significant effect on pore textural properties, and its specific surface areas were in the range of 443-474 m²/g, while pore volume of about 0.8 cm³/g with an average pore size of around 9.5 nm. The composites with super paramagnetic nature were encapsulated entirely with amorphous silica layers contributing to optimum porosity and abundant surface hydroxyl groups.     

Surface modification of silica nanoparticles by a polyoxyethylene sorbitan and silane coupling agent to prepare high-performance rubber composites

The interfacial interaction between nano-silica and rubber matrix is very important for the preparation of high-performance rubber composites. In this paper, we first proposed the use of TWEEN-20 as a new silica modifier, it has four long arms consisting of three polyether chains with terminal hydroxyl group and a fatty chain. The oxygen on the polyether can form a hydrogen bond with the silanol groups on silica surface, and the terminal hydroxyl groups can chemically react with the silanol groups without any VOCs. Moreover, the long fatty chain can weaken silica polarity to obtain a better compatibility with rubber, so that silica modified by TWEEN-20 with chemical reaction and physical absorption can homogeneously disperses in rubber matrix. Nextly, we prepared high-performance natural rubber (NR) composites by adjusting the ratio of TWEEN-20 to TESPT to adjust the physical and chemical interaction between nano-silica and rubber molecular chains. The results indicated that the performances, including the filler dispersion, static mechanical properties, and dynamic heating (viscoelastic self-heating), were optimal when the ratio of TESPT to TWEEN-20 was 2:1. In addition, one-third of TESPT was replaced by TWEEN-20 to prepare silica/rubber composites, which can reduce one-third of VOCs, improve “scorchy”, and achieve high dispersion of silica.     

Hydroxyapatite modified with silica used for sorption of copper(II)

This paper aims to increase the sorption capacity of hydroxyapatite and to find the best apatite-based material for metal ions sorption. The sorption process of copper ions from water solutions by HAP and structurally modified HAP was carried out in this work. Structural modifications of HAP were realized in the preparation phase by an addition of sodium silica into the reaction medium. The prepared materials were characterized by physical-chemical methods: IR, electron-microscopy and X-ray diffraction. The composites characterized were tested in kinetic studies regarding ion exchange and adsorption of Cu²⁺. It was revealed that the silica content, particle size and initial copper ion concentration influence the process rate. Presented at the 8th Conference on Solid State Chemistry, Bratislava, Slovakia, 6–11 July 2008.     

Grafting of silica with a hydrophilic triol acrylamide polymer via surface-initiated "grafting from" method for hydrophilic-interaction chromatography

A novel hydrophilic polymer-coated silica sorbent has been prepared using the radical "grafting from" polymerization method through surface-bound azo initiators for hydrophilic-interaction chromatography (HILIC). The azo groups were introduced to the surface of silica gel through the reaction with amino groups on the surface of silica gel with 4,4'-azobis(4-cyanopentanoic acid chloride) (ACVC). The resultant azo-immobilized silica gel served as surface initiator to polymerize hydrophilic triol acrylamide monomer N-acryloyltris(hydroxymethyl) aminomethane (NA) in methanol to get hydrophilic polymer-coated silica sorbent. The obtained poly(NA)-coated silica (pNA-sil) was characterized by Fourier transform infrared spectroscopy (FT-IR), elemental analysis (EA), and nitrogen sorption porosimetry (NSP). Then the pNA-sil was packed into the stainless-steel column and evaluated in high-performance liquid chromatography (HPLC). Good chromatographic performance for the separation of peptides and nucleosides was obtained under HILIC mode. The results indicated that the pNA-sil stationary phase behaved as mixed-mode retention mechanisms of hydrophilic and ionic interactions. Furthermore, the pNA-sil phase was used to separate tryptic digest of β-casein and our results showed that more than 12 peptides peaks were resolved and well distributed within the elution window. Finally, the pNA-sil stationary phase was demonstrated to possess remarkable reproducibility and stability. Taken together, the pNA-sil stationary phase prepared in the current study offers a potential application in proteomics study.     

Sorption of Anionic Polysaccharides and Bovine Serum Albumin on a Macroporous Glass

Concentration and time dependences of the sorption of alginic acid and -carrageenan on an MPS-1000 macroporous glass were studied. The character of pH effect on the sorption of these polysaccharides was established. For a number of sorbents prepared by the preliminary adsorption of polysaccharides on an MPS-1000 glass, the dependence of the sorption of bovine serum albumin (BSA) on the surface content of alginic acid and -carrageenan was studied. The model of adsorption in the silica–polysaccharide–protein system accounting for the interaction between polysaccharide ionic groups and active sites at the sorbent surface and protein molecules was proposed. Acid-base properties of silica modified with polysaccharides were investigated by the potentiometric titration, and the results supporting the validity of the proposed model were obtained.     

Preparation of porous TiO2/silica composites without any surfactants

TiO₂-SiO₂ composites, with high specific surface area (up to 308 m²/g), large pore volume, and narrow distribution with average pore sizes of 3.2 nm, have been synthesized from wollastonite and titanium sulfate in the absence of any surfactants. Calcium sulfate, a microsolubility salt, plays an important role in the formation of pores in this porous TiO₂/silica composite. The microstructure and chemical composition of composite were characterized by X-ray diffractometry (XRD), transmission electron microscopy (TEM) equipped with energy-dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectrometer (XPS) and N₂ adsorption and desorption analysis. The as-prepared porous titanium dioxide-silicon dioxide composites with high specific surface area and well-crystallized anatase contents were used as an efficient photocatalyst.     

块状石英纤维/Al_2O_3气凝胶复合材料的非超临界干燥法制备及表征

采用溶胶-凝胶法和常压干燥法以N,N′-二甲基甲酰胺(DMF)作为干燥控制化学添加剂制备了低密度石英纤维增强Al2O3气凝胶复合材料.通过氮气吸附-脱附实验比较研究了石英纤维对氧化铝气凝胶孔结构参数的影响;采用X射线衍射技术表征了在升温过程中石英纤维/Al2O3气凝胶复合材料的相结构变化;利用扫描电子显微镜和透射电子显微镜观察了Al2O3气凝胶基体及其石英纤维复合材料的微观形貌;初步探讨了DMF对Al2O3气凝胶形貌和密度的影响.研究结果表明石英纤维/Al2O3气凝胶复合材料成块性好,纤维与气凝胶基体结合紧密,石英纤维提高了Al2O3相转变温度,适量的DMF有利于形成均匀凝胶网络结构,减小干燥收缩压力.     

Structure and thermal properties of stearic acid/silica composites as form-stable phase change materials

In this study, stearic acid/silica phase change composites were prepared by the sol-gel method using stearic acid as phase change materials (PCMs). The effects of mass fraction of stearic acid were comprehensively investigated. The structures and thermal properties of the obtained composites were characterized by various methods, including scanning electron microscopy (SEM), differential scanning calorimetry (DSC), leakage tests, and thermogravimetry analysis (TG). The results indicated that composite containing 76% stearic acid had the best thermal properties and low mass leakage, making 76% stearic acid as the maximum content that silica matrix could protect in the composites. The latter was further confirmed by morphological analyses of the silica matrix. Silica matrix exhibited spherical particle clusters, following big–small–big–small size pattern as stearic acid rose. The composite with 76% stearic acid was at the key point of change in particle size. These findings look promising for future to prepare silica-based phase change composites with good thermal properties easily.

Open image in new window

     

Experimental and numerical study on water sorption over modified mesoporous silica

–SO₃H modified mesoporous silica adsorbent with water sorption capacity and fast desorption kinetics for water sorption was synthesized and studied via a combined experimental and numerical approach. Mesoporous silica was synthesized using sol–gel method in H₂SO₄ medium. The water adsorption isotherms and kinetics over the silica were evaluated by a dynamic water vapor sorption analyzer. Mesoporous silica was modeled using annealing simulation with CVFF forcefield. –SO₃H modified mesoporous silica was modeled by the attachment of –SO₃H to the surface hydroxyl groups and validated. Simulation results show water sorption capacity at low relative humidity (RH) increases with –SO₃H loading on mesoporous silica. Energy distribution of intermolecular interaction and micro-view of water sorption over –SO₃H modified mesoporous silica reveal that although strong interaction (intermolecular interaction of ?40 to ?20 kcal/mol) between hydrophilic groups (–SO₃H) with water can increase water sorption capacity at low RH, weak H₂O–H₂O interaction (intermolecular interaction of ?20 to ?10 kcal/mol) dominated water sorption capacity at both low and high RH.     

Surface properties of the Ni-silica gel catalyst precursors for the vegetable oil hydrogenation process: N2 sorption and XPS studies

The effect of the type of the silica gel pore structure on the surface properties of the Ni-silica gel catalyst precursors for the vegetable oil hydrogenation process has been examined applying N₂ sorption and X-ray photoelectron spectroscopy techniques. The nickel catalyst precursors with identical composition (SiO₂/Ni = 1.0) has been synthesized by precipitation of Ni(NO₃)₂ · 6H₂O solution with Na₂CO₃ solution on the three types of silica gel with different pore structures. It is shown that the usage of the silica gel supports with different texture as source of SiO₂ causes different location of Ni-species into the support pores and on the external surface area. The XPS data confirm the formation of surface species with different strength of interaction and different dispersion. These surface characteristics of the precursors will predetermine the formation of the active nickel metallic phase as well as the mass transfer of the reactants and products to and from the catalytic sites.     

平衡溶胀法研究谷氨酸二硫代氨基甲酸镧对SBR/SiO2复合材料界面作用的影响

通过合成一种含有二硫代羧基,羧基和镧离子的新型稀土促进剂——谷氨酸二硫代氨基甲酸镧(简称La-GDTC),并利用平衡溶胀法研究了La-GDTC对丁苯橡胶(SBR)/SiO2复合材料界面作用的影响.交联密度测试表明,SiO2的加入能够有效提高SBR/La-GDTC/SiO2复合材料的交联密度;而SBR/La-GDTC/S...     

Effect of sepiolite fiber on the structure and properties of the sepiolite/silica aerogel composite

Sepiolite fiber-reinforced silica aerogel composites for thermal insulators were prepared by dispersing sepiolite fiber in silica sol, aging, solvent exchanging, and drying in supercritical fluid. The surface treated sepiolite fiber and sepiolite/silica aerogel composite were characterized by scanning electron microscope; transmission electron microscope and Fourier transform infrared spectroscopy. The influence of surface treated sepiolite fiber on the mechanical and thermal properties of the aerogel composite was studied. The results indicate the hydroxyl groups on silica sol particles surface able to condense with the hydroxyls of sepiolite fibers with forming Si–O–Si between sepiolite fibers and aerogel matrix in the sol–gel process, which achieves excellent interfacial interaction in the sepiolite/silica aerogel composite, so the mechanical properties of the aerogel composite have been improved effectively without sacrificing much thermal insulating performance.