The optimization of silica gel synthesis from chemical bottle waste using response surface methodology

To reduce the amount of hazardous chemical bottle waste in the environment, we report the optimization research of silica extraction in chemical bottle waste into silica gel. Alkali fusion and sol–gel process were utilised to prepare silica gel effectively. The alkali fusion process was carried out by adding sodium hydroxide to produce sodium silicate. Afterwards, silica gel was prepared by the sol–gel method using hydrochloric acid. Box-Behnken Design (BBD) was applied to Optimisation factors the poptimiseactors affecting the silica recovery. The factors that optimised mass ratio, particle size, and temperature. The optimum recovery of silica gel was obtained by SiO₂: NaOH mass ratio of 1:3, the particle size of 63–74 µm, and a temperature of 800 °C. The purity of silica gel optimum is 63.74% characterised using X-ray fluorescence. The structure of silica gel is the appearance of amorphous peaks at 2θ 20-30° characterised using an x-ray diffractogram. The silica gel surface was characterises using scanning electron microscopy-energy dispersive x-ray. It showed an irregular surface and characteristic showed that silica gel had a radius of 15.74 nm and a specific surface area of 297.08 m².     

Study of radiation-induced polymerization of vinyl monomers adsorbed on inorganic substances. VII. Effect of pretreatment temperature of silica gel on styrene–silica gel system

To investigate the reaction mechanism of radiation-induced polymerization of styrene adsorbed on silica gel, the effect of pretreatment temperature of silica gel was studied. Preheating of silica gel was carried out at 200, 500, and 800°C. The number of silanol groups of silica gel surface decreased as preheating temperature increased. The rate of polymerization on the silica gel preheated at 500°C was faster than that at 200°C, but the polymerization rate on the silica gel preheated at 800°C was the lowest. These results suggest that rate of polymerization on the silica gel is affected by the conditions of silica gel surface such as the number of silanol groups and the pore size. At the same monomer conversion, percent grafting decreased as preheating temperature of silica gel increased. The GPC spectra of both graft polymers and homopolymers have two peaks at all preheating temperatures. The monomer conversion of low molecular weight peaks of graft polymers decreased as preheating temperature of silica gel increased. This result suggests that there is a probability that the grafting sites of low molecular weight peaks of graft polymers somehow interact with silanol groups.     

Selective separation behavior of silica gel for zirconium in simulated high level radioactive liquid waste

Zirconium in simulated high level radioactive liquid waste (HLLW) was selectively adsorbed and separated by self-made high adsorption activity silica gel. The selective adsorption mechanism was analyzed according to the structure character of self-made silica gel and performance of zirconium in acid simulated HLLW. The results show that the adsorption selectivity of self-made silica gel for zirconium is strong, because zirconium has higher positive charge and zirconium ion hydrolyzes easily. Distribution coefficient of self-made silica gels for zirconium is 53.5 ml/g. There are 6.5 (OH)/nm² on the surface on self-made silica gels which provide more adsorption activity places, thus self-made silica gels have higher adsorption capacity for zirconium (31.4 mg/g). The elution rate of the adsorption of zirconium on self-made silica gel by 0.2 mol/l H₂C₂O₄ is more than 99%. The solubility of the self-made silica gel in nitric acid is low, the chemical stability of self-made silica gel is very strong.     

改性固体表面的吸附作用——甲基化硅胶的热稳定性和吸附性能

本文利用三甲基氯硅烷与硅胶表面羟基反应的方法制备了甲基化硅胶。测定了亲水硅胶和甲基化硅胶的热处理对其自四氯化碳中吸附乙酸的等温线的影响,并配合有热重分析(TG)和红外光谱(IR)的测定。结果表明:(1)甲基化后的硅胶对乙酸的吸附能力大大下降;(2)甲基化硅胶的热处理温度达500℃时吸附能力完全恢复到甲基化前的硅胶的水平,甲基化层明显开始破坏的温度为450℃;(3)甲基化硅胶高温处理后吸附能力得以恢复的主要原因是重新形成表面自由羟基。     

不同金属盐改性对硅胶的水蒸气吸附性能影响

用不同的金属盐溶液对中孔硅胶进行了改性,并进行了吸附水蒸气动力学实验.讨论了改性硅胶的吸湿性与离子半径之间的关系及吸附速率与平均孔径的关系.实验结果表明:(1) CaCl2,LiCl,MgCl2,ZnCl2改性硅胶,可以使硅胶的吸湿性能明显增加.其中用CaCl2改性的硅胶的吸湿量最大,其平衡吸湿量是未改性硅胶的3倍;(2) 用CaCl2溶液改性的中孔硅胶其吸湿量已接近微孔硅胶的吸湿量,但其吸附速率明显大于微孔硅胶的吸附速率;(3) 用CaCl2和ZnCl2的混合溶液改性硅胶对其吸湿量的提高没有明显效果.     

变色硅胶吸附脱除模拟柴油中各种碱性氮化物

研究了变色硅胶吸附脱除氮含量为960.56μg/g模拟柴油中的碱性氮化物喹啉、苯胺和吡啶。比较了氧化铝、硅藻土、硅胶及变色硅胶对模拟柴油中喹啉的吸附脱除效果。采用XRD、低温N_2吸附-脱附和NH_3-TPD等方法对硅胶和变色硅胶进行了表征。考察了粒径、吸附温度、吸附时间、剂油质量比及共存芳香化合物(萘、苯或甲苯)对变色硅胶吸附脱除各种碱性氮化物的影响。变色硅胶吸附脱除碱性氮化物的顺序均为苯胺吡啶喹啉。吸附时间对三种氮化物的吸附脱除没有影响;吸附温度、变色硅胶粒径和共存芳香化合物对苯胺和吡啶的吸附脱除效果影响不大,对喹啉的吸附脱除效果影响较为明显;剂油质量比对三种氮化物的吸附脱除影响均较大,尤其是对喹啉影响最大。结果表明,变色硅胶吸附各种氮化物时Co能够与其中的N原子形成配位络合吸附。经焙烧再生,变色硅胶几乎完全恢复了对喹啉和吡啶的吸附脱除能力,并可多次再生,但变色硅胶再生后对苯胺的吸附能力损失较大。     

Radiation effect on polystyrene deposited and grafted on silica gel

The effect of radiation on polystyrene was studied in the presence and absence of silica gel by molecular weight measurement with GPC. Polystyrene crosslinked under vacuum in the absence of silica gel, but it either crosslinked or degraded by radiation, depending on the molecular weight of the polymer in the presence of silica gel. Part of the deposited polymer bonded to silica gel by radiation; the G value for graft-chain formation is in the range of 0.01–0.1. Irradiation of polystyrene grafted on silica gel resulted in degradation of the graft chain because of the transfer of energy from silica gel. The G value for main chain scission was about 2 when graft polymer was irradiated in the absence of homopolymer. The degradation of graft polymer was suppressed when the polymer was irradiated in the presence of homopolymer, and the amount of unextractable polymer from silica gel increased with increasing irradiation. This adds evidence to the estimation that an increase in grafting percent coupled with a slight decrease in molecular weight at a later stage of radiation-induced polymerization of styrene adsorbed on silica gel is due to a secondary effect of radiation on the polymer.     

Synthesis of poly(vinylidene fluoride) (PVdF)/silica hybrids having interpenetrating polymer network structure by using crystallization between PVdF chains

High transparent and homogeneous poly(vinylidene fluoride) (PVdF)/silica hybrids were obtained by using an in‐situ interpenetrating polymer network (IPN) method. The simultaneous formation of PVdF gel resulting from the physical cross‐linking and silica gel from sol–gel process prevented the aggregation of PVdF in silica gel matrix. To form the physical cross‐linking between PVdF chains, the cosolvent system of dimethylformaide (DMF) and γ‐butyrolactone was used. The obtained PVdF/silica hybrids had an entangled combination of physical PVdF gel and silica gel, which was called a “complete‐ IPN” structure. The physical cross‐linking between PVdF chains in silica gel matrix was confirmed by differential scanning calorimetry (DSC) measurements. The miscibility between PVdF and silica phase was examined by scanning electron microscopy (SEM) and tapping mode atomic force microscopy (TM‐AFM) measurements. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 3543–3550, 2005     

Separation of carbohydrates by liquid chromatography on silica gel,adding adsorption modificators to the eluent

Summary For the separation of carbohydrates by liquid chromatography, utilizing the intermolecular interaction with amino groups on the surface of the adsorbent, two types of adsorbents were used: silica gel modified by adding to the eluent a diamine, and a chemically bonded phase prepared by the reaction of -aminopropyl triethoxy silane with silica gel. Mono- di- and trisaccharides could be separated on silica gel modified by the adsorption of piperazin and ethylene diamine from the eluent. The separation capacity of columns packed with silica gel with bonded NH₂ groups and with silica gel having diamines adsorbed on its surface is similar. The retention volumes of 15 carbohydrates were measured on columns containing silica gel with hydroxylated surface and on silica gel modified with piperazin from the eluent consisting of acetone-water. Comparison of acetone-water and acetonitrile-water as the eluent showed that the former is also suitable for the analysis of carbohydrates.     

The Thermal Stability and Adsorbability of the Mechylated Silica Gel

The methylated silica gel has been produced by the reaction between the surface silanol groups and Clsi(CH3)3 vapor.The adsorption isotherms of acetic acid from carbon tetrachloride onto silica gel and emthylated silica gel heated at various temperatures have been determined at 25℃,and the above mentioned silica gels have been studied by TC and IR.The results indicate:(1) The adsorption of acetic acid from carbon tetrachloried onto methylated silica gel decreased greatly,probably because the concentration of the free hydroxyl groups for methylated silica gel decreased greatly as the IR shows.(2) As the methylated surface was destroyed at 450℃,the adsorption ability was restored when the methylated silica gel treated at>500℃.(3) So long as the methylated silica gel was treated at high temperature,the adsorption ability could be restored owing to that surface free hydroxyl groups were reproduced.     

Vibrational spectra of a ferrocenyl phosphine derivative chemisorbed on 3-aminopropylsilyl modified silica gel

Samples of silica gel dried at different temperatures, silica gel modified with 3-aminopropylsilyl (APS) and silica gel modified with APS and further with a ferrocenyl phosphine derivative were investigated by DRIFT, transmission FTIR and MicroRaman spectroscopy. The reaction between 3-aminopropyltrimethoxysilane (APTMS) and silica gel was mainly identified by the diminishing or vanishing intensity of the stretching band of the free OH groups in the silica gel. Further chemical reaction of the APS groups with a ferrocenyl phosphine derivative (suitable as ligand in homogeneous catalysis) was identified in the IR spectra by the appearance of the CN stretching band of the formed Schiff base, and diminishing intensity of the δ(NH₂) modes. According to the IR spectra the reaction of the ferrocenyl phosphine derivative with the APS-modified silica gel is almost quantitative. From the recorded IR and Raman spectra, conclusions concerning the substitution of APTMS methoxy groups during the chemisorption on silica gel were derived. Through deconvolution of the complex Raman band in the siloxy stretching region of the APS-modified silica gel, the newly formed siloxy bond was identified.     

Solid Phase Extraction of Neutral Analytes through Silica Gel Coated with Layers of Au Nanoparticles Self‐Assembled with Alkanethiols

In this study, we used Au nanoparticle (NP)‐coated silica gel as a solid phase extraction sorbent for the preconcentration of neutral analytes (steroid drugs). The sorbent was fabricated using two alkanethiol self‐assembly processes: one to deposit the Au NPs onto a 3‐aminopropyltrimethoxysilane‐modified silica gel and the other to functionalize the surfaces of the Au NPs. A large volume of the steroid solution was passed through the silica gel to facilitate adsorption mediated by hydrophobic interactions between the steroids and the hydrophobic moieties on the silica gel surface. Extraction of the steroids was accomplished by flushing the silica gel with a low‐polarity solvent. In this preliminary study, we found that the particle size of the silica gel and the number of layers of Au NPs coated on the silica gel both affected the preconcentration performance for the steroids. When using six layers of Au NPs coated on 5–20‐μm silica gel, the detection limits for steroids were below 80 ng L^?1; the preconcentration efficiency was over 170‐fold higher than that of the original steroid solution. Our findings provide further evidence that nanotechnology has much to benefit analytical science.     

苯基化硅胶的物理结构和表面性质的研究

本文利用苯基三氯硅烷和硅胶表面羟基反应制备了苯基化硅胶。测定了苯基化硅胶的物理结构、水蒸气吸附等温线、润湿热、差热分析(DTA)和红外光谱(IR)。结果表明,所有苯基化硅胶的真密度(dT)、比表面(S)和比孔体积(V)均减少, 而表观密度(dA)增加, 但苯基化对不同硅胶的平均孔半径(r)有不同的影响; 苯基化硅胶对水蒸气吸附, 对水、苯和环己烷的润湿热均显著减少; 苯基化硅胶的热稳定性大于甲基化硅胶, 甲基化硅胶的表面是高度憎水的, 但苯基化硅胶的憎水性则很弱。     

Reverse Phase Thin-Layer Chromato-Graphy of some Metal Ions on Butyl-Amine Impregnated Silica Gel G in Formic Acid Medium

Abstract

Reversed phase thin layer chromatography of metal ions have been performed on s-butylamine and t-butylamine impregnated silica gel thin layers in formic acid and sodium formate systems. Separation potential of impregnated silica gel thin layers was explored. Impregnated silica gel layers were found to be more selective (strongly sorbing) than unimpregnated silica gel chromo-toplates. Several important binary and ternary separations were achieved on impregnated thin layers.     

Preparation and characterization of carbosilane dendrimer-bonded silica gel and its use in LC

Divergently synthesized carbosilane dendrimers generations 1(G1) and 2 (G2) with allyl end groups were bonded onto silica gel. Reactions between the dendrimers and acid-processed silica gel took place, with toluene reflux and organic base as catalyst. Chemically bonded silica gel was characterized by transmission electron microscopy (TEM), infrared (IR), and other methods. The chemically modified silica gels were packed into high-pressure liquid chromatography (HPLC) column and their separation characters were evaluated. G2-bonded silica gel was effective in separating homologous compounds of alcohol, alkyl-substituted benzene, N-substituted benzene, metacrylic acid ester and phthalate. __________ Translated from Journal of Shandong University, 2005, 40(6) (in Chinese)     

Composite of SiO2 and Hydrogel Having Microphase Separated Structure: Physical Properties Dependence on pH

Abstract

Organic-inorganic composite gel was prepared by using PEG-modified urethane acrylate (PMUA) gel and tetraethoxysilane (TEOS). PMUA gel was prepared by the phase-inversion emulsion polymerization of PMUA emulsion. The gelation of PMUA emulsion using this method enables PMUA gel to swell with H₂O, TEOS, and ethanol. Hydrolysis and condensation reaction rates of the sol-gel process are strongly influenced by the pH controlled by catalysts such as HCl and NH₄OH. Additionally, the morphology on the cross section of composite and the amount of silica ingredient incorporated into the composite gel were dependent on solvent, the molar ratio of H₂O to TEOS, as well as the pH value.

As the silica content increased, due to hydrogen bonds interacting between PMUA gel and SiO₂, particles, the tensile strength of composites considerably increased, whereas the elongation at break decreased. The incorporation of silica ingredient in PMUA gel/silica composites was verified with FTIR/ATR and SEM. The amount of the silica component in the composite was indirectly investigated by using TGA thermal analysis.     

New Inexpensive and Selective Sorbent Phases for Rapid Thin Layer Chromatographic Analysis of Metal Ions

Abstract

New sorbent phases have been developed by impregnating silica gel G with different inorganic salts for the analysis of metal ions by thin layer chroma to graphy in carboxylic acids media. Thin layers prepared from silica gel G impregnated with ammonium chloride or barium nitrate show the unusual selectivity towards metal ions in comparison to the thin layers prepared from plain silica gel G or silica gel impregnated with silver nitrate or aluminium nitrate. Many qualitative separations     

A convenient method to immobilize 4-dimethylaminopyridine on silica gel as a heterogeneous nucleophilic catalyst for acylation

A catalyst comprised of 4-dimethylaminopyridine (DMAP) functionalized silica gel (SG-DMAP) was prepared via a convenient N-alkylation of 4-methylaminopyridine (MAP) with γ-chloropropylated silica gel promoted by potassium iodide. FT-IR, TG, SEM results illustrated that the DMAP was successfully immobilized on silica gel and the BET result suggested the pore structure was not altered after immobilization process. The highest immobilization amount of 0.75 mmol/g was obtained at 130 °C for 12 h. Activity test demonstrated that silica gel immobilized DMAP could be serve as a heterogeneous catalyst for the acylation with significant activity and stability.     

Characterization of Modified Silica Gel as a Source of Ethene for Standard Gaseous Mixtures

The application of chemically modified silica gel as a source of gaseous standard mixture containing ethene as a measured component is described. The surface of silica gel was chemically modified, which resulted in the formation of N-oxide of diethylaminopropylsilylated silica gel. This compound undergoes thermal decomposition at 245°C, yielding known amounts of ethene. The process of thermal decomposition of chemically modified silica gel took place in a desorber furnace connected on-line via a four-port valve to the device being calibrated. Such a solution provides convenient calibration of a GC/FID system after direct introduction of a stream of the generated mixture onto the front of a GC. It was found that 480 ± 15 mg of ethene can be generated per 1 g of the modified gel.     

Adsorption of atrazine on soils: model study

The adsorption of the widely used herbicide atrazine onto three model inorganic soil components (silica gel, gamma-alumina, and calcite (CaCO(3)) was investigated in a series of batch experiments in which the aqueous phase equilibrated with the solid, under different solution conditions. Atrazine did not show discernible adsorption on gamma-alumina (theta=25 degrees C, 3.8相似文献