NiO
x
-promoted Cu-based catalysts derived
from CuNi phyllosilicates were synthesized, characterized, and tested
in the selective hydrogenation of adipic acid to 1,6-hexanediol. The
reduction of the CuNi phyllosilicate allows finely dispersed Cu0 and Cu+ on the surface. The reduced Cu36Ni5PS catalyst was found to have a higher turnover frequency
for the selective hydrogenation of adipic acid than the reduced Cu41PS, Cu40Ni1PS, and Cu31Ni10PS catalysts. This catalyst is also effective at hydrogenation
of succinic acid, glutaric acid, butyric acid, pentanoic acid, and
hexanoic acid to their respective alcohols. The higher activity of
the reduced Cu36Ni5PS catalyst is attributed
to a higher oxidation state of Cu cations.
A reduction–silylation–reduction
method was developed
to synthesize hydrophobic Cu catalysts derived from Cu phyllosilicates
(CuPS). Triethoxy(octyl)silane (OTS) was used as the coupling agent.
The OTS-grafted, reduced CuPS catalysts were applied in the hydrogenation
of levulinic acid (LA) to γ-valerolactone (GVL). The most promising
catalyst was synthesized by reducing CuPS at a high temperature (350
°C for 3 h), followed by OTS grafting, and then by repeating
the previous reduction step. High LA conversion (95.7%), GVL yield
(85.2%), and stability (3 cycles with a 7.5% loss of initial activity)
were obtained at a mild reaction condition (130 °C with a H2 pressure of 12 bar). A high reduction temperature not only
leads to a low oxidation state of Cu species but also suppresses the
formation of silylation-induced acids. Moreover, the intrinsic activity
of a reduced CuPS catalyst was nearly intact after subjecting to silylation
and the second reduction treatment.
Chemical modification of silicon nitride (SiN) surfaces by silanization has been widely studied especially with 3-(aminopropyl)triethoxysilane (APTES) and 3-(glycidyloxypropyl) dimethylethoxysilane (GOPES). However few reports performed the experimental and computational studies together. In this study, surface modification of SiN surfaces with GOPES and APTES covalently bound with glutaraldehyde (GTA) was investigated for antibody immobilization. The monoclonal anti-cytokeratin-FITC (MACF) antibody was immobilized on the modified SiN surfaces. The modified surfaces were characterized by water contact angle measurements, atomic force microscopy and fluorescence microscopy. The FITC-fluorescent label indicated the existence of MACF antibody on the SiN surfaces and the efficiency of the silanization reaction. Absorption of APTES and GOPES on the oxidized SiN surfaces was computationally modeled and calculated by Materials Studio software. The computational and experimental results showed that modification of the SiN surfaces with APTES and GTA was more effective than the modification with GOPES.
Silver/silver chloride (Ag/AgCl) is commonly used as a reference electrode in electrochemical measurements. However, commercial macroscopic Ag/AgCl electrodes cannot be used in micro-electrochemical sensors. Thus, many scientists are trying to miniaturize reference electrodes to integrate into one sensor chip. In this paper a new approach for fabrication of Ag/AgCl thin films coated with agarose gel as planar reference electrodes for potentiometric sensors is introduced. A silver thin film of 220-250 nm was sputtered and patterned on silicon dioxide/silicon substrates by lithography and lift-off techniques. A AgCl layer was coated on the Ag film by using a Ag[NH 3 ] 2 Cl complex at 80°C in vacuum. The thickness of the AgCl layers was about 5 µm. The Ag/AgCl layers were then coated with an agarose gel. The AgCl layers were characterized by X-ray diffraction, micro Raman spectroscopy and scanning electron microscopy. The Open Circuit Potential (OCP) measurements with the fabricated electrodes as reference electrodes in pH 7 buffer solutions were performed in comparison with a commercial Ag/AgCl electrode. The potential difference between the fabricated Ag/AgCl electrodes and the commercial Ag/AgCl electrode was insignificant. The coating of the agarose layer as a protection layer of the Ag/AgCl electrodes enhanced the durability of the modified electrodes. The results indicated that the fabricated Ag/AgCl thin films coated with the agarose gel could be used as planar reference electrodes for potentiometric sensors.
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