scholarly journals Spectroscopic study on peculiarities of fumed silica hydridesilylation with triethoxysilane under fluidized bed conditions

2021 ◽  
Vol 12 (4) ◽  
pp. 314-325
Author(s):  
P. O. Kuzema ◽  
◽  
A. V. Korobeinyk ◽  
V. A. Tertykh ◽  
◽  
...  

Fumed silica has found widespread application in industry due to variety of fascinating properties. Owing to its specific manufacturing process, it consists of finely dispersed particles and is featured with large specific surface area covered by profoundly reactive silanol groups which are available for chemical grafting. Spherical shape of fumed silica particles and lacking porosity provides a space-filling structure. These characteristics implement the fume silica’s utilization as high-surface-area carriers for various catalysts, i.e. metallic nanometer-sized particles, organic moieties, etc. Currently a great attention is called to on-surface grafting to improve the silica-based carrier. Most of research is carried out in area of liquid phase chemistry involving an abundance of expensive and often toxic solvents while the space-filling properties of silica are favoring reactions in fluidized bed conditions. In current research fumed silica (A-300) was a subject for hydridesilylation with triethoxysilane under fluidized bed conditions. In all synthesis reported in current research the insignificant amount of solvent (1.00 wt. % of the amount used in typical wet-chemical modifications method) was spent for the silica surface silylation. While the mass ratio of silica/TES was kept constant, other conditions, i.e. solvent/catalyst presence, surface pretreatment, additional treatment with water, and the fluidized bed heating mode have been varied. FTIR spectroscopy revealed the interaction between groups of triethoxysilane and silica surface silanol groups and demonstrated the effect of modification conditions on the density of the hydridesilyl groups coverage. The results of FTIR spectroscopic studies have confirmed the presence of grafted silicon hydride groups on the surface of modified silica, as well as the presence of ethoxy and/or silanol groups – either intact or formed due to hydrolysis of the ethoxy groups. Titrimetric and spectrophotometric analysis was performed to estimate the concentration of grafted SiH groups (in all samples prepared under fluidized bed conditions their concentration ranged within about 0.28–0.55 mmol/g as dependent on the reaction conditions). Other important aspects of fluidization such as the presence of solvent and/or hydrolyzing agent, bed heating mode and the effect of the silica sample thermal pre-treatment are also discussed.

2016 ◽  
Vol 17 (1) ◽  
pp. 88-92
Author(s):  
I.S. Protsak ◽  
E.M. Pakhlov ◽  
V.A. Tertykh

This paper presents the results of studies of dimethyl carbonate interaction with sites of the fumed silica surface. The investigations were performed in a vacuum quartz cuvette using IR spectroscopy method. Chemical interaction of dimethyl carbonate with sites of the dehydrated silica surface was shown to occur at temperature of 200 °C and higher, chemisorption processes take place involving both structural silanol groups and siloxane bridges on the surface.


1993 ◽  
Vol 66 (1) ◽  
pp. 48-60 ◽  
Author(s):  
H. Cochrane ◽  
C. S. Lin

Abstract The present study uses a commercial heat cured silicone rubber formula (including a process aid) and mixing techniques to investigate the effect of varying fumed silica properties—including load, surface area, silica structure level, and surface pretreatment levels—on the rubber processing, curing, and cured physical properties. Based on the results, a simple silica network reinforcement model was developed to explain the changes in processing, curing, and vulcanizate properties of the silicone elastomers. The network is held together by silica-silica interactions and silica-polymer-silica bridge bonds between the silica aggregates. Increasing the silica loading, surface area, and structure level increases the number of interactions and hence the network strength. The pretreatment of the silica surface with organosilane molecules reduces the strength of silica-silica and silica-polymer interactions, therefore, weakening the silica network. Furthermore, the good interrelations between the initial plasticity, crepe hardening, curing, modulus yield, and durometer values strongly supports the concept of the presence of a silica network within the compounds under the low strain conditions of the tests.


2021 ◽  
Vol 13 (4) ◽  
pp. 1947
Author(s):  
Al Ibtida Sultana ◽  
Nepu Saha ◽  
M. Toufiq Reza

Hydrogen (H2) is largely regarded as a potential cost-efficient clean fuel primarily due to its beneficial properties, such as its high energy content and sustainability. With the rising demand for H2 in the past decades and its favorable characteristics as an energy carrier, the escalating USA consumption of pure H2 can be projected to reach 63 million tons by 2050. Despite the tremendous potential of H2 generation and its widespread application, transportation and storage of H2 have remained the major challenges of a sustainable H2 economy. Various efforts have been undertaken by storing H2 in activated carbons, metal organic frameworks (MOFs), covalent organic frameworks (COFs), etc. Recently, the literature has been stressing the need to develop biomass-based activated carbons as an effective H2 storage material, as these are inexpensive adsorbents with tunable chemical, mechanical, and morphological properties. This article reviews the current research trends and perspectives on the role of various properties of biomass-based activated carbons on its H2 uptake capacity. The critical aspects of the governing factors of H2 storage, namely, the surface morphology (specific surface area, pore volume, and pore size distribution), surface functionality (heteroatom and functional groups), physical condition of H2 storage (temperature and pressure), and thermodynamic properties (heat of adsorption and desorption), are discussed. A comprehensive survey of the literature showed that an “ideal” biomass-based activated carbon sorbent with a micropore size typically below 10 Å, micropore volume greater than 1.5 cm3/g, and high surface area of 4000 m2/g or more may help in substantial gravimetric H2 uptake of >10 wt% at cryogenic conditions (−196 °C), as smaller pores benefit by stronger physisorption due to the high heat of adsorption.


1997 ◽  
Vol 162 (1-2) ◽  
pp. 181-191 ◽  
Author(s):  
R. Moene ◽  
L.F. Kramer ◽  
J. Schoonman ◽  
M. Makkee ◽  
J.A. Moulijn

Author(s):  
Kailun Yang ◽  
Recep Kas ◽  
Wilson A. Smith

<p>This study evaluated the performance of the commonly used strong buffer electrolytes, i.e. phosphate buffers, during CO<sub>2</sub> electroreduction in neutral pH conditions by using in-situ surface enhanced infrared absorption spectroscopy (SEIRAS). Unfortunately, the buffers break down a lot faster than anticipated which has serious implications on many studies in the literature such as selectivity and kinetic analysis of the electrocatalysts. Increasing electrolyte concentration, surprisingly, did not extend the potential window of the phosphate buffers due to dramatic increase in hydrogen evolution reaction. Even high concentration phosphate buffers (1 M) break down within the potentials (-1 V vs RHE) where hydrocarbons are formed on copper electrodes. We have extended the discussion to high surface area electrodes by evaluating electrodes composed of copper nanowires. We would like highlight that it is not possible to cope with high local current densities on these high surface area electrodes by using high buffer capacity solutions and the CO<sub>2</sub> electrocatalysts are needed to be evaluated by casting thin nanoparticle films onto inert substrates as commonly employed in fuel cell reactions and up to now scarcely employed in CO<sub>2</sub> electroreduction. In addition, we underscore that normalization of the electrocatalytic activity to the electrochemical active surface area is not the ultimate solution due to concentration gradient along the catalyst layer.This will “underestimate” the activity of high surface electrocatalyst and the degree of underestimation will depend on the thickness, porosity and morphology of the catalyst layer. </p> <p> </p>


2004 ◽  
Vol 4 (5-6) ◽  
pp. 21-28
Author(s):  
S.-C. Kim ◽  
D.-K. Lee

TiO2-coated granular activated carbon was employed for the removal of toxic microcystin-LR from water. High surface area of the activated carbon provided sites for the adsorption of microcystin-LR, and the adsorbed microcystin-LR migrated continuously onto the surface of TiO2 particles which located mainly at the exterior surface in the vicinity of the entrances of the macropores of the activated carbon. The migrated microcystin-LR was finally degraded into nontoxic products and CO2 very quickly. These combined roles of the activated carbon and TiO2 showed a synergistic effect on the efficient degradation of toxic microcystin-LR. A continuous flow fluidized bed reactor with the TiO2-coated activated carbon could successfully be employed for the efficient photocatalytic of microcystin-LR.


Nanoscale ◽  
2015 ◽  
Vol 7 (25) ◽  
pp. 10974-10981 ◽  
Author(s):  
Xiulin Yang ◽  
Ang-Yu Lu ◽  
Yihan Zhu ◽  
Shixiong Min ◽  
Mohamed Nejib Hedhili ◽  
...  

High surface area FeP nanosheets on a carbon cloth were prepared by gas phase phosphidation of electroplated FeOOH, which exhibit exceptionally high catalytic efficiency and stability for hydrogen generation.


Author(s):  
Sisir Maity ◽  
Dheeraj Kumar Singh ◽  
Divya Bhutani ◽  
Suchitra Prasad ◽  
Umesh V. Waghmare ◽  
...  

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