A study was carried out on the effect of the nature of the support, composition of the active phase, and heat treatment conditions on the activity of trimetallic Ni‑Co‑Mo catalysts in the hydrotreating of a mixed diesel fraction. Temperature‑programmed desorption was used to show the effect of the amount and strength of the acid sites of the support on the activity of catalysts with the same elemental composition. We established the nickel‑to‑cobalt as well as phosphorus‑to‑molybdenum ratios in these trimetallic hydrotreating catalysts corresponding to the greatest desulfurization and minimum formation of polycyclic aromatic hydrocarbons in the hydrogenate.
A study was carried out on the quality of the cobalt carbonate raw material and heat treatment conditions on the activity of Co-Mo and Ni-Mo hydrotreating catalysts for a mixed diesel fraction. The relevant properties of the impregnation solution are the purity of the cobalt carbonate starting material and the synthesis temperature. A Raman spectroscopic method was proposed for monitoring the cobalt carbonate quality. Heat treatment of the catalyst was found to affect its activity. The optimal ultimate calcination temperatures for the Co-Mo and Ni-Mo catalysts were found to be very different.
The developed approaches to increasing the selectivity of analysis by laser Raman spectroscopy, the use of chemometrics and a proprietary algorithm for self-tuning calibration models with the efficiency and speed of the method have shown a rare andexcellent opportunity for information equivalent on-line control of all technological stages of the production of poly- -olefin oils and other products through a network of fiber-optic probes. The oligomers of -olefins C6, C8 and C10 obtained by the technology of heterogeneous chromium-oxide catalysis developed at RN-RDC, as shown by the Raman spectra, differ from analogues obtained by homogeneous synthesis by a variety of structures of unsaturated groups, as well as by a greater width and variability of molecular mass distribution, which makes it possible to regulate a wide range assortment of low and high molecular weight products. A specialcase - the atypically high sensitivity of Raman spectra to the length of the chain - make it possible in the synthesis process to predict and adjust in real time the molecular weight of oligomers and other target properties, and replacing a fleet of traditional analytical equipment with one method.
The method of alpha-olefin oligomerization employing a heterogeneous catalyst for production of base oils used in motor and transmission oils manufacturing is considered, which has better performance and is eco-friendlier than methods employing homogeneous highly corrosive catalysts like BF3, or AlCl3. New methods and technology for online analysis of the reaction products and process flows have been developed, allowing automated process control.
Experimental data on the effect of the method of introducing boron and Ni(Co) and Mo compounds on the physicochemical properties and hydrodesulfurization activity of catalysts in the hydrotreatment of straight-run diesel fraction are presented. The dependence of the hardness of grains, their specific surface area, spectral and microstructural characteristics on the method of preparation of catalyst samples containing 0.7–0.8 wt % B 2 O 3 was determined.
Based on systematized collection of Raman spectra of about 40 monounsaturated olefins, spectral patterns and invariant relations were established that formed the basis of the method for determining total olefins (total unsaturation per 100 carbon atoms) and their main classes in solutions of saturated hydrocarbons. Self-tuning of the model by calculating the proportion of spectrally unresolvable C=C components using the intensity of conjugated methyl groups increased its accuracy. In terms of repeatability, speed and cost-effectiveness of the analysis, the Raman-method is superior to standard methods of gas and adsorption chromatography and other modern spectralcorrelation methods. The accuracy and stability of the results repeatability is confirmed by more than annual series of parallel comparisons with the data of known method. It is shown that five types of olefins in paraffin model solutions are sufficient to construct calibration curves in units of the number of C=C bonds per 100 carbon atoms. These units make it possible to transform the data to the iodine scale and unify the calibration model for different fractions regardless of the hydrocarbon chain length. The Raman technique can be extended to analyze other mixtures of nonaromatic hydrocarbons and be used for remote control of processes via fi ber optic cables in industrial production.
Based on the systematized collection of the Raman spectra of about 40 monounsaturated olefins, spectral regularities and invariant relations were established that formed the basis of the method for determining total olefins (total unsaturation per 100 carbon atoms) and their main classes in solutions of saturated hydrocarbons. Self-adjusting of the model by calculating the proportion of spectrally unresolvable C=C components with the use of the intensity of conjugated methyl groups increased its accuracy. In terms of repeatability, speed and cost-effectiveness of the analysis, the Raman-method is superior to standard methods of gas and adsorption chromatography and other modern spectral-correlation methods. The accuracy and stability of the results repeatability is confirmed by more than annual series of parallel comparisons with the data of known method. It is shown that five types of olefins in paraffin model solutions are sufficient to construct calibration curves in units of the number of C=C-bonds per 100 carbon atoms. These units allow recalculating data to the iodine scale and unifying the calibration model for different fractions regardless of the length of the hydrocarbon chains. The Raman technique can be extended to analyze other mixtures of non-aromatic hydrocarbons and be used for remote control of processes via fiber optic cables in industrial production.
The results of tests of a new fiber-optic probe–objective for measuring both IR diffuse-reflection spectra and other types of spectra of solids at various temperatures are presented. In comparison with the conventional devices, the new scheme for measuring diffuse-reflection spectra has such advantages as the minimum distortion of spectra by the specular and Fresnel diffuse components of the reflection from surface irregularities and the linearity of the concentration dependences. The use of a fiber-optic probe–objective provides the ability for the simultaneous analysis of the solid phase and outgoing gases with increasing temperature and calibration of the spectral methods using the thermogravimetric-analysis data. An example of monitoring the process of drying catalysts in laboratory studies when analyzing composite and other materials is used to consider the prospects for using the probe–objective.