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WO2000069546A1 - Catalyseurs a flux parallele pour l'oxydation de dioxyde de soufre - Google Patents

Catalyseurs a flux parallele pour l'oxydation de dioxyde de soufre Download PDF

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Publication number
WO2000069546A1
WO2000069546A1 PCT/ES1999/000139 ES9900139W WO0069546A1 WO 2000069546 A1 WO2000069546 A1 WO 2000069546A1 ES 9900139 W ES9900139 W ES 9900139W WO 0069546 A1 WO0069546 A1 WO 0069546A1
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WIPO (PCT)
Prior art keywords
catalysts
weight
sepiolite
vanadium
vol
Prior art date
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Ceased
Application number
PCT/ES1999/000139
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English (en)
Spanish (es)
Inventor
Jesús BLANCO ALVAREZ
Pedro Avila Garcia
Mª Esperanza ALVAREZ SAIZ
Carlos Chacon Larios
Juan Miguel Ramos Jimenez
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Consejo Superior de Investigaciones Cientificas CSIC
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Consejo Superior de Investigaciones Cientificas CSIC
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Priority to PCT/ES1999/000139 priority Critical patent/WO2000069546A1/fr
Priority to AU37115/99A priority patent/AU3711599A/en
Publication of WO2000069546A1 publication Critical patent/WO2000069546A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B01D53/8609—Sulfur oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/14—Silica and magnesia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/16—Clays or other mineral silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/74—Preparation
    • C01B17/76—Preparation by contact processes
    • C01B17/78—Preparation by contact processes characterised by the catalyst used
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/74—Preparation
    • C01B17/76—Preparation by contact processes
    • C01B17/78—Preparation by contact processes characterised by the catalyst used
    • C01B17/79—Preparation by contact processes characterised by the catalyst used containing vanadium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/302—Sulfur oxides

Definitions

  • Catalytic oxidation of sulfur dioxide is a process traditionally used for the manufacture of sulfuric acid.
  • the gas stream containing a concentration of S0 2 equal to or greater than 10% by volume and sufficient oxygen is passed through a fixed bed catalytic reactor to transform sulfur dioxide into sulfur trioxide with conversions greater than 90% vol.
  • a commercial catalyst representative of those used in the sulfuric acid factories for the oxidation of S0 2 in the activated state would have the following weight composition: K2O: 13.0; V 2 O 5 : 6.9; Na 2 0: 0.5; SCfe: 19.9; rest: Si0 2 .
  • These mass catalysts are prepared in the form of extrudates, and are activated by calcination in the presence of S0 2 to form a mixture of vanadium and potassium pyrosulfates which, housed in the interticular spaces of the silica, can be in liquid form under conditions of reaction, Tandy, GH, J. Appl. Chem., 6, 68 (1968).
  • RECTIFIED SHEET (RULE 91) by weight of sulfur it emits gases that typically contain between 1000 and 4000 ppm of S0 2 and about 10-50 ppm of SO3.
  • Pat US 3,987,153 a catalyst is described in the form of an extruded tablet or granule prepared with CSVO3 and RbVC activated with sulfates and supported on refractory oxides, where the formed SO3 is transformed into acid sulfuric acid with the help of hydrogen peroxide.
  • Squires, Pat. US 3,957,953 finely divided V 2 Os particles are deposited on a panel of dolomite and calcium carbonate granules to transform the generated SO3 into calcium sulfate.
  • the catalyst is prepared by coating honeycomb ceramic structures of a material of low thermal expansion coefficient, probably cordierite, with a catalytically active material based on vanadium compounds, Humphrey , RA and Dahlberg, NW, Power, 52-54, March, 1996.
  • the requirements for a catalyst are high selectivity, low cost, long duration and easy handling; however, and especially when it is intended to treat large volumes of gases, there are also necessary conditions, a high resistance to abrasion and a physical form that causes low values of loss of load.
  • the catalyst is arranged in parallel sheets or plates, or preferably it is formed in parallelepipeds that are perforated along the longitudinal axis by parallel channels, with a density of 4-70 channels per cm 2 of cross section.
  • the pressure drop or pressure drop caused by the passage of gases through the catalyst formed in this way is two or three orders of magnitude lower than that which occurs when conventional beds of particles are used, see for example DeLuca, JP and Campbell, LE. Adv. Mat. Cat., 293 (1977).
  • These perforated parallelepiped structures which are called monoliths or honeycomb, have their greatest industrial application in the catalytic converters of gasoline cars, although their use has been extended in recent years to other industrial applications, eg Blanco, Pat. Eng. 8,803,453.
  • the active phase is either deposited by impregnation, as is the case with the noble metals proposed by Matsuda, Pat. US 4,350,670, and which logically exhibits low abrasion resistance, since the gases, when the catalyst surface is worn away, will mainly drag metals deposited on it, or the active phase is deposited as a coating on a support inert ceramic, as is the case of the Altman patent, Pat.
  • Catalysts prepared in accordance with this invention formed in a honeycomb structure with a geometric parallelepiped shape and is perforated by channels parallel to its longitudinal axis in the number of 2-60 channels per square centimeter of cross section, in a square, hexagonal shape , triangular or round, the wall thickness being less than 1.5 mm.
  • the preparation of catalysts is carried out by extrusion of pastes containing, together with the support components and / or precursors of the active phase of the catalyst, magnesium and aluminum silicates, especially ⁇ -sepiolite which, in effect, facilitate or enable the forming operation, and also confer exceptional mechanical properties on the finished product.
  • Sepiolite is a naturally occurring hydrated magnesium silicate for which various structural formulas have been proposed, such as Si ⁇ 2 Mg 8 ⁇ 3 or (OH) 4.8H 2 ⁇ with stoichiometric variations in the number of protons, surface hydroxyl groups and crystallization water molecules, depending on their origin and subsequent purification treatments.
  • the use of sepiolite as a catalyst component is relatively recent. Thus, for example, its use is described as a support for noble metals used as catalysts in the reduction of hydrocarbons in Pat. Esp. 530.566 or as a nickel support for hydrogenation and dehydrogenation processes in Pat. Esp. 524.260.
  • the natural sepiolite used in this invention is ⁇ -sepiolite in a compact form, commercially known as Vallecas sepiolite, whose typical impurity content is as follows: AI2O3: 2.6%; Fe 2 0 3 : 0.3%; K2O: 0.6%; CaO: 0.9%; Na ⁇ O:
  • the sepiolite content of the materials prepared in this invention is preferably 20-80% by weight.
  • sepiolites have a fibrous structure consisting of talc type tapes parallel to the fiber axis with two layers of tetrahedral units of silica attached to a layer of octahedral units of magnesium through oxygen atoms. More detailed information is found in the review by Alvarez A (Palygorskite-sepiolite. Occurrences. Genesis and Uses. Section VI, p. 253-286. Edited by Singer and E. Galán, Elsevier 1984).
  • the ⁇ -sepiolite in a compact form is dried at 200 ° C in order to remove physically adsorbed water. Subsequently, it is milled by selecting a particle size below 200 ⁇ m in diameter.
  • This sepiolite has a specific surface area of 250 m 2 g "1 , measured by nitrogen adsorption by the BET method; when this material is treated at 500 ° C, a specific surface loss is observed, obtaining values close to 150 m 2 g " 1 , due to the disappearance of pores of smaller diameter. This treatment, without
  • the two basic elements and differentiators of the technique proposed in this invention are the use of ⁇ -sepiolite and the formation of the oxidation catalysts of S0 2 to SO 3 in honeycomb structures.
  • the utility of this technique for obtaining three different types of catalysts is shown below. First, the process of preparing platinum catalysts is described; Next, the method for the preparation of vanadium / potassium / Ti ⁇ 2 mass catalysts is indicated, and finally, the procedure for preparing vanadium / potassium / S ⁇ 0 2 catalysts is also shown.
  • honeycomb supports described in this invention for the preparation of platinum catalysts in common have the presence of ⁇ -sepiolite. This material is used mixed with boehmite with eventual addition of aluminum silicate.
  • the boehmite used maintains a specific surface area of approximately 215 m 2 g "1 , after treatment at 500 ° C for 4 hours in air.
  • This type of alumina is used in the production of supported platinum catalysts, since it provides numerous points anchoring to platinum, so that its distribution on the surface of the support favors the oxidation reaction of SO 2.
  • the pores of average diameter greater than 60 A occupy a volume close to 0, 7 cm 3 g "1 and have an average pore diameter of about 16 A The selected average size of this
  • RECTIFIED SHEET RULE 91 material is below 200 ⁇ m.
  • the main impurities that generally accompany the alumina used are carbon: 0.3%; S ⁇ 0 2 and Fe 2 ⁇ 3 : 0.01% and Na ⁇ : 0.002%, with respect to the total weight of the product.
  • the aluminum silicate used has a particle size of less than 50 ⁇ m, in order to improve the Theological properties of the prepared pastes and thus, to promote their extrusion.
  • This silicate has a specific surface area of 37 m 2 g "1 , with a pore volume of 0.18 cm 3 g " 1 V with an average diameter of 160 A.
  • the supports are prepared by dry mixing the selected components for a sufficient time, to ensure that the particles are distributed homogeneously.
  • the next stage corresponds to kneading, after adding the necessary amount of water.
  • the honeycomb paste is extruded and dried at low temperature before moving to the air calcination stage at 500 ° C.
  • the impregnation of the calcined supports with a platinum salt is carried out, to subsequently reduce the platinum cation to metallic platinum to 400-450 ° C.
  • the catalysts themselves are prepared by impregnating with a platinum salt of a support made with mixtures of alumina, aluminum silicate and ⁇ -sepiolite, the content of the latter material being equal to or less than 80% by weight and the amount of platinum deposited between 0.1 and 1% by weight. These catalysts at temperatures of 400-500 ° C and space velocities of 200-10,000 h "1 , CN, convert 85-95% vol. Of sulfur dioxide to sulfur trioxide.
  • Prepared platinum catalysts have a specific surface that is the proportional sum of their respective supports.
  • the catalyst containing 80% sepiolite and 20% alumina has a specific surface area of 162 m 2 g "1 , an experimental value that approximates that calculated taking into account the percentages of its components.
  • the components used in this invention correspond to an anatase with a purity of 98.7% by weight, with a specific surface area of 70 m 2 g "1 and an average particle size of 0.4 ⁇ m, the pore volume for an average diameter greater than 60 A being 0.6 cm 3 g "1 and the average pore diameter around 2300 A.
  • ⁇ -sepiolite has been used and in some cases also aluminum silicate, both described above.
  • water-soluble vanadium and potassium salts have been used at room temperature.
  • These mass catalysts are prepared by dry mixing the support components together with the precursor salts of the active phase. Kneading is carried out with the amount of water required for each mixture of solids for subsequent extrusion with honeycomb configuration. The materials obtained are subjected to a drying process in order to remove the absorbed water. Subsequently, they are treated between 400-500 ° C under SO 2 / SO 3 atmosphere for a time to obtain the oxidation catalysts.
  • the silica is supplied with properly treated diatomaceous earth, with a specific surface area of 10 m 2 g "1 , a pore volume of 0.75 cm 3 g "1 and an average pore diameter of 8500 eu corresponds to interparticular spaces.
  • the particles of diatom, aluminum silicate, ⁇ -sepiolite and potassium salt are mixed dry.
  • an aqueous solution of the vanadium salt is prepared, with controlled acidity, which is added on the powder mixture, kneading until a homogeneous paste is obtained.
  • this paste is processed by extrusion for its formation in honeycomb structures. These materials undergo a drying process in order to remove the absorbed water. Subsequently, they are treated between 400-500 ° C in
  • mass catalysts are prepared with ⁇ -sepiolite, titanium dioxide, vanadium and potassium, where the content of titanium dioxide is equal to or less than 60% in prison, that of vanadium is equal to or greater than 7% by weight as V 2 O 5 , with an atomic ratio of K / V of 3-4; These catalysts at temperatures of 43-490 ° C and space velocities of 200-10,000 h * 1 , CN, convert 75-80% vol. from sulfur dioxide to sulfur trioxide.
  • Mass catalysts with ⁇ -sepiolite, diatomaceous earth, vanadium and potassium where the diatomaceous earth content is equal to or less than 80% by weight, that of vanadium is equal to or greater than 7% by weight as V 2 ⁇ 5 , with an atomic ratio of K / V of 3-4; these catalysts at temperatures of 430-490 ° C and space velocities of 200-10,000 h "1 , CN, convert 90-99% vol. of sulfur dioxide to sulfur trioxide.
  • ⁇ -sepiolite ⁇ -sepiolite are mixed dry with 120 g of boehmite for 5 hours. It is then kneaded at room temperature for 4 hours, adding 400 ml of water. The paste is conditioned and extruded, obtaining parallelepiped structures with honeycomb configuration, which are dried for 12 hours at 110 ° C and subsequently treated at 500 ° C in air for 4 hours.
  • the support thus obtained has a wall thickness of 0.09 cm and 8.2 cells per c 2 of cross section.
  • 222 ml of an aqueous solution of chloroplatinic acid with a platinum concentration of 600 ppmv are prepared and the support is impregnated therewith, then dried at 110 ° C for 4 hours before being reduced in a stream of Ammonia diluted 5% in nitrogen at 440 ° C for two hours.
  • the resulting product is a material with a content of 0.17% by weight of platinum with respect to the total catalyst weight.
  • 320 g of ⁇ -sepiolite are mixed dry with 320 g of boehmite and 160 g of aluminum silicate for 5 hours. Then, knead at room temperature for 4 hours, adding 800 ml of water. The paste is conditioned and extruded, obtaining a support with honeycomb configuration of square cells. The monoliths are dried for 12 hours at 110 ° C, before being treated at 500 ° C in air for 4 hours. The support thus obtained has a wall thickness of 0.09 cm and 8.2 cells per cm 2 of cross section.
  • the support is impregnated with 80 ml of an aqueous solution of chloroplatinic acid containing 700 ppmv of platinum.
  • the drying and reduction process is
  • Example 3 Activity tests of supported platinum catalysts.
  • the catalysts of examples 1 and 2 are subjected to activity tests, using a N 2 comment containing 0.1 and 7% vol. of S0 2 and 0 2 , respectively.
  • the space speed varies between 5200 and 6400 h “1 (CN), the linear speed between 0.7 and 0.9 ms " 1 (CN), the temperature between 450-470 ° C, with a working pressure of 1, 1 atmospheres
  • the concentration of S0 at the inlet and outlet of the reactor is analyzed by gas chromatography.
  • the monolithic catalysts of Examples 4, 5 and 6 are tested in the oxidation reaction of S0 2 to SO3 under the following conditions: temperature of 450 ° C, space velocity (CN) between 5200-6650 h " ⁇ linear speed (CN ) between 0.8-0.9 ms "1 , pressure of 1.1 atmospheres and an inlet concentration of reactants in volume of 0.1 and 7% of S0 2 and O2 respectively and N 2 up to balance, measuring the conversion from S0 2 to SO3 after 15 hours of operation.
  • the conversion values obtained for the catalyst containing 50% titanium dioxide corresponds to approximately 80% vol. higher amounts of T0 2 fill the fibrous structure of ⁇ -sepiolite, while amounts less than 50% by weight, give rise to coating defects of the silicate structure. Both phenomena are reflected in a decrease in the catalytic performance of prepared solids.
  • the mixture of the three solids and the acid solution is kneaded for a total time of 4 hours.
  • the paste is then conditioned and extruded into parallelepiped structures that are dried at room temperature for 40 hours and then treated at 110 ° C for an additional 48 hours.
  • the monolithic catalysts have a wall thickness of 0.09 cm and a density of 8.2 cells per cm 2 of cross section.
  • the final composition by weight of this catalyst corresponds to 80% in Si0 2 , 7% of V 2 0 5 and a K / V atomic ratio of 3.5.
  • Example 10 Activity tests of the more vanadium / potassium / Si0 2 catalysts
  • the catalysts of examples 8 and 9 are tested in the oxidation reaction of S0 2 to SO 3 at a temperature between 450-470 ° C, space velocity (CN) between 5000-6000 h “1 , linear velocity (CN) around 1 ms "1 , pressure 1.1
  • Example 11 Activity tests in a process of joint elimination of nitrogen and sulfur oxides.
  • Activity tests have been carried out in a multi-stream parallel flow reactor at a temperature of 450 ° C, firstly installing a conventional honeycomb catalyst for the selective reduction of nitrogen oxides.
  • the oxidation catalyst of S0 2 in Example 8 is placed in the same reactor.
  • the concentration of reactants in the fed gas corresponds to 1000 ppmv of NO x , 1000 ppmv of Nhh, 1000 ppmv of S0 2 , 5.2 % vol. from 0 2 and N 2 to balance. It operates with a space velocity for each catalyst of approximately 15,000 h ".1
  • the final conversion of NO is 80% vol. And 60% vol. With respect to that of S0 2 after 16 hours of operation.

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Abstract

La présente invention concerne un nouveau procédé de préparation de catalyseurs conformes aux exigences de diverses applications industrielles du processus d'oxydation catalytique de SO2 à SO3. Ces matières ou leurs supports sont formés dans des structures en nid d'abeilles, par extrusion des pâtes précurseurs correspondantes à l'aide d'un silicate naturel. Ce procédé permet de préparer des catalyseurs de platine à support et des catalyseurs massiques de vanadium/potassium, réunissant de grandes performances catalytiques et fluidodynamiques pour le processus d'oxydation indiqué. Ces catalyseurs sont particulièrement adaptés pour le traitement ou la dépuration de grands volumes de gaz à faible contenu en SO2, généralement émis par les unités de combustion et autres processus industriels.
PCT/ES1999/000139 1999-05-14 1999-05-14 Catalyseurs a flux parallele pour l'oxydation de dioxyde de soufre Ceased WO2000069546A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/ES1999/000139 WO2000069546A1 (fr) 1999-05-14 1999-05-14 Catalyseurs a flux parallele pour l'oxydation de dioxyde de soufre
AU37115/99A AU3711599A (en) 1999-05-14 1999-05-14 Parallel flow catalysts for sulfur dioxide oxidation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/ES1999/000139 WO2000069546A1 (fr) 1999-05-14 1999-05-14 Catalyseurs a flux parallele pour l'oxydation de dioxyde de soufre

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4350670A (en) * 1979-08-20 1982-09-21 Hitachi, Ltd. Process for treating flue gas
WO1999011372A1 (fr) * 1997-09-03 1999-03-11 Intercat, Inc. Systems d'additif sox bases sur l'utilisation d'especes multiples de particules

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4350670A (en) * 1979-08-20 1982-09-21 Hitachi, Ltd. Process for treating flue gas
WO1999011372A1 (fr) * 1997-09-03 1999-03-11 Intercat, Inc. Systems d'additif sox bases sur l'utilisation d'especes multiples de particules

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
J. BLANCO, P. AVILA, A. BAHAMONDE, M. YATES, J.L. BELINCHON, E. MEDINA, A. CUEVAS: "Influence of the operation time on the performance of a new SCR monolithic catalyst", CATALYSIS TODAY, vol. 27, 1996, pages 9 - 13 *
J. BLANCO, P. AVILA, M. YATES, A. BAHAMONDE: "The use of sepiolite in the preparation of titania monoliths for the manufacture of industrial catalysts", PREPARATION OF CATALYSTS VI SCIENTIFIC BASES FOR THE PREPARATION OF HETEROGENEOUS CATALYSTS, 1995, pages 755 - 764 *

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