Mesoporous Titanium-containing Silicas. Synthesis and geometrical characteristics

Mesoporous titanium-containing silicas with TiO₂ contents from 1 up to 70 mol% were prepared. The obtained samples have been characterized by the powder X-ray diffraction data, the diffuse reflectance infrared Fourier transform method, and nitrogen adsorption at 77 K. Specific surface area, total pore volume, distribution pore volume on pore sizes were determined from nitrogen adsorption isotherm for synthesized titanosilicas. This revised version was published online in August 2006 with corrections to the Cover Date.     

Specific Sorption Sites for Nitrogen in Zeolites NaLSX and LiLSX

Specific sorption sites for nitrogen, N₂, in NaLSX and LiLSX zeolites were investigated using a DRIFT spectroscopic method. Sorption of molecular hydrogen, H₂, by NaLSX or LiLSX zeolite at 77 K with DRIFT control of perturbation of sorbed molecules allowed to discriminate two or three different types of specific sorption sites in the respective zeolites. Their H–H stretching frequencies are 4077 and 4081 cm^–1 for NaLSX, and 4061, 4084 and 4129 cm^–1 for LiLSX. With reference to an independent investigation by methods of both sorption thermodynamics and molecular modeling for N₂ sorption on LiLSX, the first two of the corresponding bands were ascribed to H₂ sorption on lithium cations, Li⁺, localized in supercages of the faujasite, FAU, zeolite framework at sites SIII and SIII, while the latter band most likely belongs to H₂ sorption on Li⁺ cations at sites SII, and on hydroxyl groups, OH. Sorption of N₂ by Li⁺ cations at sites SIII and SIII is the strongest, resulting in a decrease of intensity of the corresponding DRIFT bands that stem from subsequent H₂ sorption. Nitrogen sorption by Li⁺ cations at sites SII is much weaker. Sorption of N₂ on Na⁺ cations at sites SIII in NaLSX zeolite is also stronger than by Na⁺ cations at sites SII.     

Hydrogenation of acetylene into ethane–ethene mixtures over modified Pd–alumina catalysts

1. Download : Download high-res image (138KB)
2. Download : Download full-size image

     

CrOx-CeO2二元氧化物表面NO的NH3催化还原反应机理

利用原位漫反射红外光谱法研究了473 K下在CrOx-CeO₂二元氧化物表面NO的NH₃催化还原反应的机理。研究了CrO-CeO₂二元氧化物表面在反应过程中的表面吸附物种。为了更加清晰的了解反应过程, 在SCR反应过程中分别切断NH₃和NO的气流, 并采集了所生成的原位漫反射红外光谱图, 通过研究以上结果得出结论:当前状态下的SCR反应过程可能服从E-R机理。     

Effect of Aging on the Synthesis of Kaolin-Based Zeolite Y from Ahoko Nigeria Using a Novel Metakaolinization Technique

Zeolite Y was systematically synthesized from Ahoko Nigerian kaolin in a conventional hydrothermal system using novel metakaolinization technique. The effect of aging on the formation of zeolite phase was investigated during the course of the synthesis. A rapidly processed metakaolin at a temperature of 600°C and exposure time of 50 minutes, which is capable of reducing the energy and cost of producing it was used to study the synthesis of zeolite Y. It was found that aging conditions play a prominent role in the preparation of zeolite Y from Ahoko metakaolin. Aging played a significant role by increasing the crystallinity of the final product even though zeolite Y was obtain without aging. The outcome of zeolite Y synthesized from Ahoko kaolin in 9 hours at 100°C was different from most reports on the synthesis of zeolite Y from kaolin where longing time (72 hours) of crystallization are reported.     

富缺陷BN负载的高分散Cu催化乙醇脱氢制乙醛

生物乙醇作为平台分子通过催化转化的方法可以制备烯烃、乙醛、丁醇和芳香化学品等,其中乙醛是生产乙酸、季戊四醇、三氯乙醛、山梨酸等重要化学品的原料.随着乙醛的需求量逐年增加,发展以乙醇直接脱氢生成乙醛的工艺,具有联产氢气、原子经济性高、产物易分离的优点,符合国际绿色低碳发展战略要求,有望替代当前乙烯氧化法生产工艺.乙醇分子...     

The effect of heat and IR radiation on the fluorescence of cellulose

The emission spectra of pure cellulose samples of various origins were monitored during several heating/cooling cycles. During heating the emission intensity decreased due to the greater probability for internal conversion at higher temperatures. Cooling resulted in an emission recovery that was nearly reversible over several heating/cooling cycles, provided that the final 0temperature was sufficiently low. The change in the relative emission yield with temperature showed two regimes, both with linear decreases but different slopes, suggesting different mechanisms for the internal conversion in these regions. Heating to temperatures higher than 160°C for filter papers and higher than 145°C for microcrystalline cellulose initiated reactions that caused changes in the emission spectra typical of thermal degradation. If the samples were heated beyond these threshold temperatures the emission recovery on cooling after the first heat treatment occurred to a much higher intensity level than that observed initially, indicating the formation of a multitude of new chromophores due to thermal reactions. Exposure of the samples to IR radiation caused a slow increase in the emission intensity for almost 600h.     

Effects of sampling methodologies on FT-IR data base searching

The sampling methodologies employed in Fourier Transform Infrared (FT-IR) spectroscopy tend to distort to a degree the data obtained relative to that which would be obtained via transmittance. This distortion complicates data base searching. A standard sample of polystyrene was investigated using the techniques of transmittance, attenuated total reflectance (ATR), diffuse reflectance (DRIFT) and photoacoustic spectroscopy (PAS). Several types of corrections are employed to minimize the distortions due to sampling methodologies.These corrections are evaluated with respect to four distinct search algorithms. The results obtained indicate that proper mathematical treatment of the data prior to data base searching enhances the discrimination value of a data base search.     

Hydroxylation of the silica in microfabricated thin layer chromatography plates as probed by time‐of‐flight secondary ion mass spectrometry and diffuse reflectance infrared Fourier transform spectroscopy

Microfabricated silica thin layer chromatography (TLC) plates have previously been prepared on patterned carbon nanotube forests. The high temperatures used in their fabrication reduce the number of hydroxyl groups on their surfaces. Fortunately, silica can be rehydroxylated. In diffuse reflectance infrared Fourier transform spectroscopy (DRIFT), a silanol peak below 3740 cm^?1 indicates a well‐hydroxylated silica surface that is fit for chromatography. Hydroxylations of our materials with HF are so effective that it is not possible to discern the position of this peak. In contrast, this signal is discernable when the plates are treated with NH₄OH. To find a more convenient method for studying the surfaces of TLC plates, time‐of‐flight secondary ion mass spectroscopy (ToF‐SIMS) was considered. ToF‐SIMS is advantageous because multiple microfabricated TLC plates must be scraped to obtain enough silica for one DRIFT analysis, while static SIMS can be performed on very small regions (500 × 500 µm² or less) of individual plates. Ratios of the SiOH⁺ and Si⁺ ToF‐SIMS signals for microfabricated TLC plates correlated well with ~3740 cm^?1 silanol peaks from DRIFT. Thus, SIMS allows direct analysis of all of our treated and untreated plates, including those hydroxylated with HF. The best hydroxylation condition for HF, which was better than any studied for NH₄OH, was around 150 ppm at room temperature. The best hydroxylation condition for NH₄OH was 50 °C for 72 h. ToF‐SIMS versus DRIFT results of commercial TLC plates were also obtained and evaluated. Copyright © 2014 John Wiley & Sons, Ltd.     

Application de la Spectroscopie Infra Rouge à L'étude du Comportement Thermique de la Cellulose Partie I.

In this work, we describe and evaluate the use of the Fourier transform infra red (FTIR) spectroscopy in DRIFT mode (diffuse reflectance infra red Fourier transform) in an environmental device to follow the functional evolution of cellulose during thermal treatments. The potentialities (and difficulties) of the technic are given. This revised version was published online in July 2006 with corrections to the Cover Date.