PREPARATION AND CHARACTERIZATION OF SILICA GEL POWDERS

Silica gel powders,with particle diameter in the range 10 to 20 nm,were prepared from water glass using ethyl acetate as a latent acid reagent. The products were characterized by TGDTA, TEM, FTIR, BET and some other experiment methods. The process of silica solgel formation and the thermal behavior as well as phase change of the silica powders during heattreating process were studied, and the effect of heattreating temperature on the specific surface area and apparent density of the silica powders was investigated.

Gypsum-based Silica Gel Humidity-controlling Composite Materials:Preparation,Characterization,and Performance

Gypsum was used as substrate,and silica gel was mixed into substrate at a certain mass ratio to prepare humidity-controlling composites;moreover,the moisture absorption and desorption properties of gypsum-based composites were compared with adding different silica gel particle size and proportion.The morphological characteristics,the isothermal equilibrium moisture content curve,moisture absorption and desorption rate,moisture absorption and desorption stability,and humidity-conditioning performance were tested and analyzed.The experimental results show that,compared with pure-gypsum,the surface structure of the gypsum-based composites is relatively loose,the quantity,density and aperture of the pores in the structure increase.The absorption and desorption capacity increase along with the increase of silica gel particle size and silica gel proportion.When 3 mm silica gel particle size is added with a mass ratio of 40%,the maximum equilibrium moisture content of humidity-controlling composites is 0.161 g/g at 98% relative humidity(RH),3.22 times that of pure-gypsum.The moisture absorption and desorption rates are increased,the equilibrium moisture absorption and desorption rates are 2.68 times and 1.61 times that of pure-gypsum at 58.5% RH,respectively.The gypsum-based composites have a good stability,which has better timely response to dynamic humidity changes and can effectively regulate indoor humidity under natural conditions.

Silica Gel Supported Trifluoromethanesulfonic Acid Catalyzed Beckmann Rearrangement of Cyclohexanone Oxime in Liquid Phase

The liquid phase Beckmann rearrangement of cyclohexanone oxime (CHO) using fuming sulfuric acid as a catalyst is a traditional method for preparing ε-caprolactam (CPL). This process has drawbacks, such as environmental pollution, corrosion of equipment, and low added value of by-product ammonium sulfate. This article designed and prepared a green silica gel-supported trifluoromethanesulfonic acid catalyst for the liquid-phase Beckmann rearrangement of CHO to prepare (CPL). The influencing factors of catalyst preparation and the optimal reaction conditions for Beckmann rearrangement were investigated. It was found that the optimal conditions for catalyst preparation were as follows: raw material silica gel:trifluoromethanesulfonic acid = 1:0.2 (mass ratio), room temperature, stirring time of 2.5 hours, and solvent of acetonitrile, silica gel mesh size is 100 - 200. The optimal reaction conditions for Beckmann rearrangement are CHO: catalyst = 1:2 (mass ratio), temperature of 130˚C, solvent of benzonitrile, volume of 30 mL/g CHO, and reaction time of 4 hours. Under the above conditions, the conversion of CHO is 90%, and the selectivity of CPL is 90%.

The Adsorption of Pb(II)Using Silica Gel Synthesized from Chemical Bottle Waste:Optimization Using Box-Behnken Design

The adsorption of Pb(II)on silica gel synthesized from chemical glass bottle waste has been studied.The effect of independent variables(adsorbent dose,initial concentration of Pb(II),contact time,and pH)on the Pb(II)removal from water was evaluated and optimized using the Response Surface Methodology(RSM).Under optimized conditions(adsorbent dose:20 mg;contact time:30 min;initial Pb(II)concentration:120 mg.L^(−1);and pH:8),the removal of Pb(II)was 99.77%.The adsorption equilibrium data obtained from the batch experiment were investigated using different isotherm models.The Langmuir isotherm model fits the experimental data.This shows that the surface of the silica gel synthesized from chemical bottles waste was covered by a Pb(II)monolayer.XRF analysis showed that the synthesized silica gel had a SiO_(2) content of 75.63%.Amorphous silica was observed from XRD analysis.SEM-EDX characterization showed that Pb was adsorbed on the silica gel surface.SEM analysis showed that silica gel has irregular particles with a surface area of 297.08 m2.g^(−1) with a pore radius of 15.74 nm calculated from BET analysis.

Silica Gel from Chemical Glass Bottle Waste as Adsorbent for Methylene Blue:Optimization Using BBD

This research focuses on the effective removal of methylene blue dye using silica gel synthesized from chemical glass bottle waste as an environmentally friendly and cost-effective adsorbent.The adsorption process was optimized using Box-Behnken Design(BBD)and Response Surface Methodology(RSM)to investigate the influence of pH(6;8 and 10),contact time(15;30 and 45 min),adsorbent mass(30;50 and 70 mg),and initial concentration(20;50 and 80 mg/L)of the adsorbate on the adsorption efficiency.The BBD was conducted using Google Colaboratory software,which encompassed 27 experiments with randomly assigned combinations.The silica gel synthesized from chemical glass bottle was characterized by XRD,FTIR,SEM-EDX and TEM.The adsorption result was measured by spectrophotometer UV-Vis.The optimized conditions resulted in a remarkable methylene blue removal efficiency of 99.41%.Characterization of the silica gel demonstrated amorphous morphology and prominent absorption bands characteristic of silica.The Langmuir isotherm model best described the adsorption behavior,revealing chemisorption with a monolayer coverage of methylene blue on the adsorbent surface,and a maximum adsorption capacity of 82.02 mg/g.Additionally,the pseudo-second-order kinetics model indicated a chemisorption mechanism during the adsorption process.The findings highlight the potential of silica gel from chemical glass bottle waste as a promising adsorbent for wastewater treatment,offering economic and environmental benefits.Further investigations can explore its scalability,regenerability,and reusability for industrial-scale applications.

Preparation of Silica Gels with High Adsorption Activity for Extraction of Zirconium

Silica gels with a high specific surface area and high adsorption activity ,which have high selectivity and high adsorption capacity for zirconium in acidic high level radioactive liquid waste (HLLW), have been prepared from water-glass and hydrochloric acid through adding surfactants. The surfactant modifies the surface of the primary sol particles, thus suppresses the growth of the primary particle,but accelerates their agglomeration. The action of the surfactant is similar to that of the organic structure-directing agent and makes the sol cluster cross-linkage ring-like network in short order. The specific surface area of the silica gel is 998 m 2/g; the static adsorption capacity and the adsorption distribution coefficient for zirconium in HLLW are 32.6 mg/g and 56.1 mL/g, respectively.

Selective removal of 2,4-dichlorophenoxyacetic acid from water by molecularly-imprinted amino-functionalized silica gel sorbent

A molecularly-imprinted amino-functionalized sorbent for selective removal of 2,4-dichlorophenoxyacetic acid （2,4-D） was prepared by a surface imprinting technique in combination with a sol-gel process. The 2,4-D-imprinted amino-functionalized silica sorbent was characterized by FT-IR, nitrogen adsorption and static adsorption experiments. The selectivity of the sorbent was investigated by a batch competitive binding experiment using an aqueous 2,4-D and 2,4-dichlorophenol （2,4-DCP） mixture or using an aqueous 2,4-D and 2,4- dichlorophenylacetic acid （DPAC） mixture. The largest selectivity coefficient for 2,4-D in the presence of 2,4-DCP was found to be over 18, the largest relative selectivity coefficient between 2,4-D and 2,4-DCP over 9. The static uptake capacity and selectivity coefficient of the 2,4-D-imprinted functionalized sorbent are higher than those of the non-imprinted sorbent. The imprinted functionalized silica gel sorbent offered a fast kinetics for the extraction/stripping of 2,4-D, 73% of binding capacity （200 mg/L 2,4-D onto 20 mg of imprinted sorbent） was obtained within 5 min and the adsorbed 2,4-D can be easily stripped by the mixture solution of ethanol and 6 mol/L HC1 （V：V =1：1）. In a test of five extraction/stripping cycles, the adsorption capacity of the sorbent was all above 93% of that of the fresh sorbent. Experimental result showed the potential of molecularly-imprinted amino-functionalized sorbent for selective removal of 2,4-D.

Preparation of organically functionalized silica gel as adsorbent for copper ion adsorption

A novel adsorbent （AMPS-silica） was synthesized by bounding AMPS （2-acrylamido-2-methylpropanesulfonic acid） onto silica surface, which functioned with γ-methacryloxypropyltrimethoxysilane reagent. The adsorbent was characterized by nitrogen adsorption/desorption measurement, thermogravimetric analysis （TGA） and potentiometric titration analysis. The TGA result indicated that the surface modification reactions introduced some organic functional groups onto the surface of silica. The surface area of AMPSsilica was 389.7 m2/g. The adsorbent was examined for copper ion removal in series of batch adsorption experiments. Results showed that the adsorption of Cu2＋ onto AMPS-silica was pH dependent, and the adsorption capacity increased with increasing pH from 2 to 6. The adsorption kinetics showed that Cu^2＋ adsorption was fast and the data fitted well with a pseudo secondorder kinetic model. The adsorption of Cu^2＋ onto AMPS-silica obeyed both Freundlich and Langmuir isotherms, with r^2 = 0.993 and r^2 = 0.984, respectively. The maximum Cu^2＋ adsorption capacity was 19.9 mg/g. The involved mechanism might be the adsorption through metal binding with organic functional groups such as carboxyl, amino and sulfonic groups. Cu^2＋ loaded on AMPS-silica could be desorbed in HNO3 solution, and the adsorption properties remain stable after three adsorption-desorption cycles.

Silica gel supported AlCl_3 catalyzed Friedel-Crafts acylation of aromatic compounds

Silica gel supported aluminium trichloride（SiO2-AlCl3） has been shown to be a mild,efficient,and chemoseiective heterogeneous Lewis acid catalyst for the acylation of aromatic compounds with acid chlorides.The catalyst can be reused up to five times after simple washing with ether and is stable（as a bench top catalyst）.

Flocculation of flotation tailings in presence of silicate gel and polymer

Flotation tailings were successfully flocculated in the presence of cationic polyacrylamide and silica gel.The effects of various parameters such as polymer weight,charge density,and pH on the rate of flocculation were also investigated in the current study.The flocculation mechanism of the flocculant on tailings was investigated using zeta potential and Fourier transform infrared(FTIR)measurements.The results obtained reveal that 1)sodium silicate gel,used as a binder for the consolidation of tailings form primary flocs,acts as an anchor and the adsorption of polymer flocculant on these anchors results in the formation of larger flocs and,consequently,enhanced settling rate;2)flocculation in the presence of silica gel and polymer has a faster settling rate than single-polymer flocculation owing to the mechanisms of charge neutralization and bridging as identified using zeta potential and FTIR measurements.A pilot level study was conducted to investigate the influence of processed water on the flotation of scheelite.The results show that the proposed tailing disposal method could improve scheelite recovery by 2%(approximately)and could reduce the daily operation costs of the plant by approximately 108.57 USD.

Efficient CO_2 capture on low-cost silica gel modified by polyethyleneimine

In this work, a series of polyethyleneimine （PEI） functionalized commercial silica gel were prepared by wet impregnation method and used as CO2 sorbent. The as-prepared sorbents were characterized by N2 adsorption, FT-1R and SEM techniques. CO2 capture was tested in a fixed bed reactor using a simulated flue gas containing 15.1% CO2 in a temperature range of 25-100 ~C. The effects of sorption temperature and amine content on CO2 uptake of the adsorbents were investigated. The silica gel with a 30 wt% PEI loading manifested the largest CO2 uptake of 93.4 mgcoz/gadsorbent （equal to 311.3 mg^oz/gPEI） among the tested sorbents under the conditions of 15.1% （v/v） CO2 in N2 at 75 ~C and atmospheric pressure. Moreover, it was rather low-cost. In addition, the PEI-impregnated silica gel exhibited stable adsorption-desorption behavior during 5 consecutive test cycles. These results suggest that the PEI-impregnated silica gel is a promising and cost-effective sorbent for CO2 capture from flue gas and other stationary sources with low CO2 concentration.

Removal of siloxanes from biogas using acetylated silica gel as adsorbent

Biogas can be used as an alternative energy source for producing heat and electricity;however, volatile methylsiloxanes(VOSiC) present in biogas can severely damage heat exchangers, turbines and gas engines. Consequently, e cient removal of VOSiC from biogas that is used as a biofuel is required. In this work, acetylated silica gel(Ac@SG) was synthesized,via treatment of microporous silica gel(SG) with acetic anhydride as an adsorbent, for removal of VOSiC from biogas,and characterized with XRD, SEM–EDS, N2-BET and FT-IR. This Ac@SG adsorbent exhibited a meso-/microporous structure and hydrophobic surface, indicating it was a more e cient adsorbent for removing hexamethyldisiloxane(L2) and octamethylcyclotetrasiloxane(D4) from biogas samples than conventional SG. It was found that the adsorption capacities of Ac@SG reached 304 mg L2/g for hexamethyldisiloxane and 916 mg D4/g for octamethylcyclotetrasiloxane at lower temperatures in the experimental range, and water had no significant e ect on its absorption e ciency. The used Ac@SG could be easily regenerated by heating it at 110 °C, and the adsorption capacity of recycled Ac@SG for hexamethyldisiloxane and octamethylcyclotetrasiloxane was kept constant in four recycle adsorption experiments.

Separation and purification of deoxynivalenol(DON) mycotoxin from wheat culture using a simple two-step silica gel column chromatography

Deoxynivalenol（DON） is a type B trichothecenes mycotoxin produced by several Fusarium species, often found in foodstuffs for humans and animals. DON is in great demand for the toxicological researches both in vivo and in vitro. In this work, wheat culture was inoculated with a Fusarium graminearum PH-1 strain for DON production. The solvent system for crude extraction was acetonitrile-water（84：16, v/v）. A simple two-step silica gel column chromatography was employed to separate the DON mycotoxin from wheat culture, combined with preparative high performance liquid chromatography（preparative HPLC） to purify the compound. The solvent system for the second silica gel column chromatography was methylene chloride-methanol（17：1, v/v）, which provided a good elution effect selected on thin layer chromatography（TLC）. The target compound was identified by HPLC, and the chemical structure was confirmed by mass spectrometry（MS） and ~1H and ^（13）C nuclear magnetic resonance（NMR） spectroscopy. A total of 433 mg of purified DON was obtained from 1 kg of wheat culture, with a purity of 99.01%. The study had provided an easy-operating and cost-effective method to isolate an expensive compound in a simple way.

Silica-gel Supported V Complexes： Preparation, Characterization and Catalytic Oxidative Desulfunzation

In this manuscript, a series of catalyst SG n-[VVO2-PAMAM-MSA] (SG silica gel, PAMAM polyamidoamine, MSA 5-methyl salicylaldehyde, n=0, 1, 2, 3) was prepared and their structures were fully characterized by Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and inductive coupled plasma emission spectrometer (ICP) etc. XPS revealed that the metal V and SG n-PAMAM-MSA combined more closely after the formation of Schiff base derivatives. Their catalytic activities for oxidation of dibenzothiophene were evaluated using tert-butyl hydroperoxide as oxidant. The results showed that the catalyst SG 2.0-[VVO2-PAMAM-MSA] presented good catalytic activity and recycling time. Meanwhile, the optimal condition for the catalytic oxidation of SG 2.0-[VVO2-PAMAM-MSA] was also investigated, which showed that when the oxidation temperature was 90 °C, time was 60 min, the O/S was 3:1, and the mass content of catalyst was 1%, the rate of desulfurization could reach 85.2%. Moreover, the catalyst can be recycled several times without significant decline in catalytic activity.

Synthesis of Hydroxypropyl-β-cyclodextrin Bonded Silica-gel and its Application to Resolution

In order to set up a simple and effective method for resolution of optical isomers, hydroxypropyl-β-cyclodextrin was bonded to silica-gel, which can be used for preparation of thin-layer chromatography plates. Resolution of clenbuterol and propranolol were investigated on these thin-layer chromatography plates using different combinations of solvent systems at ambient temperature. The best simultaneous resolution was achieved in solvent system of acetonitrilen-butanol （50：50, v/v）. Rst values of resolution of clenbuterol hydrochloride and propranolol hydrochloride are 3.6 and 4.3, respectively. The spots of different enantiomers are separated clearly. The results showed that hydroxypropyl-β-cyclodextrin bonded silica-gel could be successful in resolution of chiral adrenergic drugs. The study offers a direct, rapid and reliable method for separation of this kind of optically active compounds.

Hierarchically Structured Monolithic ZSM-5 through Macroporous Silica Gel Zeolitization

The hierarchically structured ZSM-5 monolith was prepared through transforming the skeletons of the macroporous silica gel into ZSM-5 by the steam-assisted conversion method. The morphology and monolithic shapes of macroporous silica gel were well preserved. The hierarchically structured ZSM-5 monolith exhibited the hierarchical porosity, with mesopores and macropores existing inside the macroporous silica gel, and micropores formed by the ZSM-5. The products have been characterized properly by using the XRD, SEM and N2 adsorption–desorption methods.

Silica gel-assisted solvothermal production of CdS,Cu_xS (x=1,2) and ZnS with different morphologies

CdS, CuxS (x=1, 2) and ZnS with different morphologies were produced by the solvothermal reactions of M(CH3COO)2·2H2O (M=Cd, Cu and Zn) and NH2CSNH2 in hexane with and without silica gel as a hard template at 200 ℃ for 24 h. The product phases were detected using X-ray diffraction (XRD). Different morphologies were characterized using a scanning electron microscope (SEM). The existence of silica gel in modeling morphologies of the sulfides was characterized using Fourier transform infrared (FTIR) spectrometer. Raman spectra of different products show the vibrations at the same wavenumbers, although they are composed of different morphologies. Photoluminescence (PL) emissions of the corresponding phases with different morphologies are at the same values, but their intensities are increased by template adding.

Preparation and Characterization of Silica Aerogels Derived from Ambient Pressure

Silica aerogels were prepared by sol-gel technique from industrial silicon derivatives （polyethoxydisiloxanes, E40）, followed by silylation and drying under ambient pressure. The specific surface area, pore size distribution and thermal conductivity of the silica aerogels were investigated and the results showed that the diameter of the silica particles is about 6 nm and the average pore size of the silica aerogels is 14.7 nm. The specific surface area of which is about 1000 m^2.g^-1 and the thermal conductivity is about 0.014 wm^-l.K^-1 at room temperature and pressure of 1.01×10^5 Pa. The Si-CH3 groups were also detected on the internal surface of the silica aerogels, which show hydrophobic. Silica aerogels derived by this technique is low cost and have wide applications.

Novel Silica Gel Supported Polyether Ionic Liquids: Efficient Catalysts Applied in Transformation of Carbon Dioxide

Three new catalysts based on the silica gel supported polyether ionic liquids(ILs), i.e., [HO-PECH-MIM]ClSi, [H2N-PECH-MIM]Cl-Si, and [HOOC-PECH-MIM]Cl-Si, were prepared, and their chemical structures were characterized by infrared(IR) spectroscopy and nuclear magnetic resonance(NMR) spectroscopy. Thermogravimetric analyzer(TG), X-ray diffractometer(XRD) and scanning electron microscope(SEM) were used to evaluate their thermal stability,crystalline structure and apparent morphology, respectively. Surface areas of the prepared catalysts were calculated by the Brunauer-Emmett-Teller(BET) method. The catalytic reaction for the synthesis of propylene carbonate(PC) using CO_2 and propylene oxide(PO) in the presence of the prepared catalysts was studied. The influences of times of recycling and catalyst structure on catalytic performance were also investigated. The experimental results showed that the silica gel supported polyether ILs catalysts successfully prepared under mild condition could possess the advantages of high activity, excellent thermal stability, good selectivity and easy recycling, while the phase transition of the liquid polyether ILs catalysts was also achieved. When the reaction temperature was 90 °C, the CO_2 pressure was 2.0 MPa and the dosage of the catalyst was 2.5%, [HOOC-PECH-MIM]Cl-Si was found to have the best catalytic performance in the catalytic process, with the conversion rate reaching 100% and the selectivity equating to 98.2%. The conversion rate and selectivity still could reach more than 90% even after the catalyst was reused for 15 times.

INVESTIGATION OF THE INTERACTIONS BETWEEN WATER AND MODIFIED SILICA GEL BY IGC AND TPD

In this work, the thermodynamic parameters for the adsorption of water vapor on untreated silica gel and silica gel treated with hygroscopic salts and silane coupling agent were determined by lnverse Gas Chromatography （IGC） in the infinite dilution region. The desorption activation energies of the water vapor on virgin and modified silica gels were estimated by using the Temperature Programmed Desorption （TPD） technique. The interactions between the water and the virgin and modified silica gels were discussed. Results showed that the thermodynamic parameters and desorption activation energy of water vapour on the silica gels increase with decreasing pore size and increasing the surface hydrophilic properties. The desorption activation energy of virgin and modified silica gels was found to increase with increasing the thermodynamic parameters. The larger the adsorption parameters and the desorption activation energy were, the interactions between water and virgin and modified silica gels were.