• Bulletin of the Korean Chemical Society
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• v.33 no.8
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• pp.2642-2646
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• 2012

Pretreatment of spent FCC catalyst and its application in remove trace olefins in aromatics were investigated in this research. The most effective pretreatment route of spent FCC catalyst was calcining at $700^{\circ}C$ for 1 h, washing with 5% oxalic acid solution in ultrasonic reactor and dried. Treated spent FCC catalyst was modified with metal halides, then to prepare catalyst to remove trace olefins in aromatics. X-ray diffraction, Pyridine-FTIR, $N_2$ adsorption-desorption and inductively coupled plasma optical emission spectrometer (ICP-OES) were used to investigate the pretreatment process. The result showed that the performance of the treated spent FCC catalyst was much greater than that of the spent FCC catalyst, which indicted the possibility and improvement of this research.

• Applied Chemistry for Engineering
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• v.29 no.4
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• pp.376-381
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• 2018

The purpose of this study is to investigate and optimize an effectiveness process for the recovery of Pd from the spent Pd/C catalyst by the process of hydrogenation of maleic anhydride over Pd/C. Pd solution recovered from Pd/C catalyst was used to prepare Pd/C catalysts. Their characteristics were compared to those of Pd/C catalyst prepared by using a reagent grade precursor solution. Pd in the spent catalyst was leached by the modified process with dry and wet methods to obtain the high recovery ratio of Pd. The burn-out of carbon in the spent Pd/C catalyst was carried out in the rage of $600-900^{\circ}C$. Pd content of carbonized catalyst was confirmed by XRF and ICP. Pd was extracted from carbonized spent catalysts with acid solutions of 1,2 and 4 M HCl at a leaching temperature of $90^{\circ}C$ for 2 h. The high recovery ratio of Pd was shown as 92.4% that leached in 4 M HCl. Also Pd/C catalysts were prepared by using the leached solution and the reagent grade of $H_2PdCl_4$ as a precursor solution and the characteristics were analyzed by XRD, CO-chemisorption and FE-TEM. As a result, the dispersion of the catalyst prepared by using the leached solution was 34.6%, which was found to be equal to or more than that of the Pd/C catalyst prepared by the reagent grade precursor solution.

• Korean Journal of Metals and Materials
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• v.46 no.12
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• pp.823-829
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• 2008

The solvent extraction process for the recovery of vanadium from leaching solution of SCR(selective catalytic reduction) spent catalyst was investigated by using Alamine336 as an extractant. The effects of experimental conditions, such as initial pH and concentration of sulfate ion, and ammonia concentration of stripping solution were studied. The extraction percentage of vanadium were increased with the increase of initial pH of leaching solution and decreased with the increase of sulfate ion. More than 99% of vanadium in leaching solution were extracted and stripped at the A/O ratio of 1.0 in 2 stages. On the basis of these results, an optimum solvent extraction process which vanadium was effectively recovered from SCR spent catalyst was proposed.

• Journal of Korean Society for Atmospheric Environment
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• v.20 no.5
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• pp.663-670
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• 2004

The catalytic oxidation of benzene, toluene and xylene over a spent industrial catalyst (Pd-based) was investigated in a fixed bed flow reactor system. According to the priming condition, the properties of a spent Pd-based catalyst were characterized by XRD(X-ray diffraction). BET(Brunauer-Emmett-Teller) and ICP(Inductively coupled plasma). When air was used as a primer, optimum priming temperature was found to be 200$^{\circ}C$, and the catalytic activity decreased as the priming temperature increased. When a spent Pd-based catalyst primed with air at 200$^{\circ}C$ was re-treated with hydrogen at 200$^{\circ}C$, 300$^{\circ}C$ or 400$^{\circ}C$, respectively, the catalytic activity increased and thermal effect were negligible. $HNO_3$ aqueous solution priming resulted in slight decrease of the catalytic activity, with little effects on $HNO_3$ concentrations. The activity of a spent Pd-based catalyst with respect to VOC molecule was observed to follow sequence: xylene> toluene> benzene. Benzene. toluene and xylene could be removed to almost 100% by a spent Pd-based catalyst primed with hydrogen.

• Resources Recycling
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• v.3 no.1
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• pp.17-24
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• 1994

Recovery of precious metal values from petrochemical spent catalyst is important from the viewpoint of environmental protection and resource recycling. Two types of spent catalysts were used in this study. One used in the manufacture of ethylene contains 0.3% Pd in the alumina substrate. The other used in oil refining contains 0.3% Pt and 0.3% Re. Both spent catalysts are roasted to remove volatile matters as carbon and sulfur. Then, metallic Pd powder from Pd spent catalyst is obtained in the course of grinding, hydrochloric acid or aqua regia leaching and cementation with iron. For the recovery of Pt and Re from Pt-Re spent catalyst, Pt and Re are leached with either HCI or aqua regia, first. Metallic Pt powder is recovered from the leach solution by cementation with Fe powder. Re in sulfide form is precipitated by the addition of sodium sulfide to the solution obtained after Pt recovery. It is found that 6N HCI can be successfully used as leaching agent for both types of spent catalyst. 6N HCI is considered to be better than aqua regia in consideration of reagent and equipment cost.

• Applied Chemistry for Engineering
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• v.8 no.4
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• pp.679-684
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• 1997

The major constituents in spent FCC catalysts are Si, Al, Fe, Ti, alkali metals and some others. The spent catalyst is also composed small amounts of rare metals such as Ce, Nd, Ni and V. The selective adsorption and concentration of Ce and Nd from the leaching solution of spent FCC catalysts with sulfuric acid($0.25mol/dm^3$) were carried out by the column method with a chelate resin having a functional group of aminophosphoric acid type. Ce and Nd were separated from eluate liquor containing Al, Nd and V by the precipitation process with oxalic acid. Vanadium is purified from chloride ion coexistance by solvent extraction, employing tri-n-octyl phosphine oxide as extractant with Al in the raffinate solution. Rare metals with the purity of 99 percent were obtained from the spent FCC catalyst.

• Journal of the Korean Applied Science and Technology
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• v.37 no.4
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• pp.723-732
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• 2020

The spent RHDS (Residue HydroDeSulfurization) catalyst is deactivated mainly by deposition of various contaminants such as coke, sulfur and vanadium on the surface of catalyst. To eliminate those contaminants, the following remanufacturing process was conducted. The first, heavy oil on the surface of the spent RHDS catalyst was removed by kerosene and dehydrated. The second, the high temperature incineration was carried out to eliminate coke and sulfur components deposited on the surface of spent RHDS catalyst. The third, the excessive quantity of Vanadium deposited on the surface of catalyst was removed by leaching process as follows: ultrasonic agitation was carried out at 50℃, for 10 seconds with 0.5% and 1% oxalic acid solution. The purpose of this process is to find out regenerated RHDS catalyst can be used as SCR catalyst for NOx reduction by controlling the vanadium residual content of the regenerated RHDS catalyst through leaching process. The composition of regenerated RHDS catalyst was analyzed by XRF and the NOx reduction efficiency was also measured by continuous catalytic fixed bed reactor. As the result, regenerated catalyst, with 0.5% oxalic acid, ultrasonic agitation in 10 seconds, showed the most stable NOx reduction efficiency. Also, in comparison with commercial SCR catalyst, the NOx reduction performance of regenerated catalyst was similar to that of commercial SCR catalyst at the temperature 375℃ and higher whereas was lower than commercial SCR catalyst at the temperature range between 200~250℃. Therefore, it was confirmed that the regenerated catalyst as powder form wash coated on the surface of metal corrugated substrate can be used for commercial SCR catalyst.

• Resources Recycling
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• v.20 no.4
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• pp.36-45
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• 2011

The recovery of platinum group metals (PGMs) from the leach solution of spent auto-catalyst and the wash solution of the leach residue was investigated in the laboratory scale experiments by the cementation process using metal powders as the reductant. In this study, the effect of Al, Mg and Zn powders on the cementation process was particularly examined. Aluminum powder was selected as the most suitable reductant for the cementation of PGMs. At the cementation time of 10 minute under the aluminium stoichimetric amount of 19.3 and the reaction temperature of $50{\sim}60^{\circ}C$, the recovery of platinum group metals from the leach solution of the spent auto-catalyst was found to be 99.3%, 99.4%, 90.2% for Pt, Pd and Rh, respectively. Under the same conditions with the aluminium stoichimetric amount of 45, the recovery of platinum group metals from the wash solution of the leach residue of spent catalyst was observed to be 97%, 97% and 90% for Pt, Pd and Rh, respectively. In addition, it was possible to upgrade the platinum group metals in the precipitates obtained from the cementation process by about 10% through the removal of metal impurities by the nitric acid leaching at ambient temperature.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.19 no.10
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• pp.598-602
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• 2018

This study examined the characteristics of the waste catalyst used in the petroleum refinery operations. The total pore volume, specific surface area, and average pore size of the spent catalyst used in the petroleum refinery operations were 3.96cc/g, 13.81m2/g, and 1.15A, respectively. The weight loss observed in the range from $25^{\circ}C-700^{\circ}C$ for the spent catalysts using TG and DTA was approximately 23 wt. %. EDS analysis of the waste catalyst sample showed that the five major components were vanadium, nickel, manganese, iron, and copper. The extraction system is attractive for liquid-liquid extraction. In this study, Cynex 272 was used to extract vanadium from waste catalyst. The electrochemical characteristics of the extracted vanadium solution were measured by cyclic voltammetry (CV). As a result, an oxidation / reduction peak appeared, indicating the potential of an electrolytic solution.

• Journal of the Korean Applied Science and Technology
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• v.27 no.3
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• pp.273-281
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• 2010

Nickel recovery method was studied by the wet process from the catalyst used in hydrogenation process. Nickel content in waste catalyst was about 16%. At the waste catalyst leaching system by the alkaline solution, selective leaching of nickel was possible by amine complex formation reaction from ammonia water and ammonium chloride mixed leachate. The best leaching condition of nickel from mixed leachate was acquired at the condition of pH 8. LIX65N as chelating solvent extractant was used to recover nickel from alkaline leachate. The purity of recovered nickel was higher than 99.5%, and the whole quantity of nickel was recovered from amine complex.