WO2010029201A1 - Composition d'un matériau à structure poreuse, son procédé de préparation et utilisation d'une composition - Google Patents

Composition d'un matériau à structure poreuse, son procédé de préparation et utilisation d'une composition Download PDF

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Publication number
WO2010029201A1
WO2010029201A1 PCT/ES2009/070332 ES2009070332W WO2010029201A1 WO 2010029201 A1 WO2010029201 A1 WO 2010029201A1 ES 2009070332 W ES2009070332 W ES 2009070332W WO 2010029201 A1 WO2010029201 A1 WO 2010029201A1
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carbon
sepiolite
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Roberto Dos Santos
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Desarrollos Tecnicos Mc, S.L.
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    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B01J20/28071—Pore volume, e.g. total pore volume, mesopore volume, micropore volume being less than 0.5 ml/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/11—Clays
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/311—Porosity, e.g. pore volume
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials

Definitions

  • the invention relates to new materials with wide distribution of pore sizes and to their industrial use in the elimination of contaminating compounds by means of adsorption systems in dynamic regime.
  • the values of the micropore volume, the external surface (corresponding to the area not associated with the micropores) and the threshold diameter (defined as the average diameter of the pores that due to its greater size, cause the first signal in the mercury intrusion porosimetry analysis) are the data that determine the adequacy of the texture of the adsorbent material for use in the different adsorption processes in dynamic regime.
  • micropores (diameters from 0 to 2 nm) confer the storage capacity, while the mesopores (diameters from 2 to 50 nm) and the macropores (diameters from 50 to 10,000 nm), responsible for the surface values external and of the internal diameter of the material, favor the adsorption rate by allowing the rapid diffusion of the adsorbate molecules on the inner surface of the solid.
  • adsorbents for these industrial units therefore requires textures with a wide distribution of pore sizes that include interconnected macro, meso and micropores in order to enable and facilitate the collection, diffusion and storage of undesirable molecules.
  • the adsorption is carried out with activated carbons generally prepared with coconut shell, some types of hardwoods and most of the mineral carbons.
  • activated carbons generally prepared with coconut shell, some types of hardwoods and most of the mineral carbons.
  • the mineral coal or carbonized material of plant origin reacts partially and in a controlled manner with an oxidizing compound such as carbon dioxide, water vapor or mixture of both at temperatures above 800 0 C, with Ia consequent creation of the desired porosity (F. Rodr ⁇ guez and M. Molina, Chemistry and Industry, 563-571, 1998).
  • These materials have a high specific surface area, derived from the numerous micropores they contain but in practice have an absence of larger pores, so that their use, in a dynamic regime, has severe limitations in terms of diffusion.
  • clays are known that have plastic properties, that is, sufficiently moist, that are deformable when light pressure is applied while maintaining the shape and that they become rigid again when dried and vitreous when subjected to high temperatures.
  • plastic properties that is, sufficiently moist
  • they are natural phyllosilicates composed of small particles or crystals, generally of colloidal size, which give rise to textures based on mesoporosity and, therefore, with limited storage capacity in physical adsorption processes due to the absence of micropores.
  • EP-0978313 describes a hive-shaped adsorbent compound consisting of ⁇ -sepiolite that incorporates activated carbon homogeneously dispersed in the silicate structure; The industrial application of these compounds is limited by their low resistance to abrasion and their ability to crumble in the presence of water or water vapor.
  • the material described above is treated at temperatures between 830 and 125O 0 C in an inert or reducing atmosphere for at least 2 hours to significantly improve its physical properties by transforming the ⁇ -sepiolite into a new phase crystalline called enstatite (Grim, RE, 1968 Clay Mineralogy MacGraw-Hill, pp. 596);
  • enstatite Grim, RE, 1968 Clay Mineralogy MacGraw-Hill, pp. 596
  • the preparation of these materials implies a high energy cost derived from a first heat treatment in a controlled atmosphere to manufacture activated carbon and a second treatment, also at high temperature and in an inert or reducing atmosphere, for the generation of the enstatite .
  • the high cost of manufacturing and the complexity of the preparation of these adsorbent materials can certainly discourage its use in a large number of possible industrial applications.
  • the present invention relates to new adsorbent materials, with predetermined porous structure, with wide distribution of pore sizes, and their use in the elimination of existing pollutants in industrial effluents.
  • the present invention relates to a composition of adsorbent material characterized by the fact that it includes activated carbon and enstatite, prepared by a single heat treatment in a controlled atmosphere from carbon and sepiolite and which, eventually, can incorporate aluminum silicates and oxides of alkaline earth elements as additives.
  • the said composition can be formed into granules, pellets, spheres, solid cylinders, hollow cylinders, plates or in a structure of channels parallel to the length of the longitudinal axis in a number greater than 2 and less than 25 channels per square centimeter of cross section generally called monolith or hive.
  • the composition takes the form of hollow cylinders that can be smooth or striated, of any shape and size with a length of approximately 0.5 cm to about 10 cm and a wall thickness between 0.02 cm and 0.5 cm approximately.
  • the passage of the fluid to be purified through the adsorbent material arranged in the form of a hollow cylinder results in a dynamic fluid that combines a turbulent regime caused by the flow that passes between the cylinders with a laminar regime that takes place in the passage of the fluid through the interior of the hollow cylinders; This situation implies a unique behavior that significantly improves the effectiveness of the adsorption phenomenon in dynamic operations.
  • the final composition includes only enstatite and activated carbon in the weight ratios corresponding to predetermined distributions of pore sizes.
  • the present invention further relates to a method for preparing the compositions indicated above.
  • sepiolite powder and selected carbon powder and, eventually, alumina powder and bentonite powder, with a determined weight ratio are mixed dry and homogeneously. subsequently, the mixture is kneaded with water in a high shear kneader.
  • a pseudoplastic mass is produced that easily incorporates the carbon particles.
  • the mass obtained after kneading is molded or extruded to obtain the desired shape and then preferably dried at room temperature for at least 2 hours and 80- 25O 0 C for at least four hours; subsequently the material is subjected to heat treatment between 500 and 600 0 C in an inert atmosphere for at least 2 hours and finally activated at 800 ° C-1000 0 C for at least 2 hours under carbon dioxide and water.
  • this comprises the following phases:
  • sepiolite and carbon are mixed in a sepiolite / carbon weight ratio of 0.5 to 3 and more preferably 0.8 to 2.
  • the carbon content determines the total micropore volume
  • the sepiolite content determines the total volume of mesopores in the final product.
  • composition that includes enstatite and activated carbon is obtained by forming pastes prepared in aqueous medium with a mixture of sepiolite and carbon powders without any other additive or component and by means of a unique heat treatment in a controlled atmosphere.
  • the appearance of macropores in the pieces subjected to heat treatment is due to the consolidation of the interparticle spaces of the previously formed pastes and it was verified that the particle size of the carbon used when conditioning the average volume of the interparticle spaces determines the average size of the macropores in the final product. Therefore, in this invention, the total volume and average size of the macropores can be predetermined by manipulating the quantity and particle size of the coal used as raw material, which has a great importance, since the adsorption speed in dynamic regime will depend on these parameters.
  • the natural sepiolite used as raw material in this invention is ⁇ -sepiolite in a compact micronized form and was supplied by Tolsa S.A., under the name Pansil. It is a hydrated magnesium silicate, whose typical weight content of impurities is as follows:
  • AI 2 O 3 2.6%; Fe 2 O 3 : 0.3%; K 2 O: 0.6%; CaO: 0.9%; Na 2 O: 0.1%.
  • the open zeolitic channels on the surface of the ⁇ -sepiolite create a network of pores of different sizes and dimensions and confer a specific surface
  • the texture has a total pore volume of
  • the disintegrated particle size of this material is 90% less than 1 ⁇ m.
  • any mineral or vegetable coal can be used, with the exception of coking coals, with particle sizes disintegrated so that 90% are less than 20 ⁇ m.
  • the particle size of the carbon used determines the volume of the interparticle spaces responsible for the macroporosity of the finished product.
  • the mixture of dry sepiolite and carbon powders also contains, as additives, bentonite powder and alumina powder in discrete amounts.
  • a weight percentage of bentonite can be between 1 and 3% and alumina between 1 and 6%, in relation to the total weight of the dry powder mixture.
  • the particle sizes disintegrated in both powders must be 90% less than 50 ⁇ m.
  • the bentonite contributes to the plasticity of the wet mass to form and improves the mechanical properties of the final product while, as observed by the X-ray diffraction, the alumina reacts in part with the magnesium oxide present in the surface of the sepiolite forming a spinel (MgCAI 2 O 3 ) that also contributes to improve the hardness of final product (J. Blanco, M. Yates, P. Avila and A. Bahamonde, Journal of Materials Science, 5927-5933, 1994).
  • the bentonite used as raw material in this invention was supplied by Oil-Dry Corporation under the name of Bentonite of Paraná. It is an aluminum silicate whose weight content of impurities is as follows: Fe 2 O 3 : 5.9%; K 2 O: 1, 8%; MgO: 1.6%; CaO: 0.5%; Na 2 O: 0.8%, with a BET specific surface area of 95 m 2 g "1 , a total pore volume of 0.17-0.18 cm 3 g " 1 , based on mesoporosity.
  • the alumina that is eventually used as an additive in the preparation of the materials object of this invention mostly has a gamma-like crystalline structure.
  • the raw material used was supplied by Condea with the name of Pural SB; This conveniently dehydrated material has a specific BET surface area of 264 m 2 g "1 , a total pore volume of 0.40-0.45 cm 3 g " 1 , similarly based on mesoporosity.
  • the structure of these new materials typically has a micropore volume of 0.1 to 0.2 cm 3 g "1 corresponding to the activated carbon that is formed during the heat treatment, which confers adsorbate storage capacity, also contains a volume of mesopores around 0.2 cm 3 g "1 derived mainly from the clays used and a macropore volume that typically ranges between 0.3 and 0.6 cm 3 g " 1 formed from the interparticle spaces that provide external surface and threshold diameter values around 100 m 2 g "1 and 1700 nm respectively, which guarantee high adsorption speeds in units operating in a dynamic regime.
  • the present invention also relates to the use of a composition, as defined and described above, as adsorbent material for liquids, gases and vapors in units operating in a dynamic regime.
  • the size classification - micro, meso and macro - used in this document is the one adopted by the IUPAC "Manual of Symbols and Terminology of Physicochemical Quantities and Units" E. Butterworths. London (1972).
  • the values of the volumes of pores and specific surface of the materials are determined by the intrusion of mercury and by adsorption of nitrogen following the BET method.
  • the disintegrated particle size is calculated from data obtained in mercury intrusion tests.
  • Mineral powder with a particle size of less than 15 ⁇ m in 90% and sepiolite powder with a particle size of less than 0.3 ⁇ m in 90% are used as raw materials.
  • Santa Catarina (Brazil) has a calorific value of less than 9.6 MJ / Kg., An ash content of 45% and a total humidity of 14% by weight.
  • Sepiolite supplied by TOLSA SA (Spain) when dried at 200 0 C in air for 3 hours, has a surface area of 182 m 2 g "1 and a mesopore volume of 0.42 mlg" 1 without significant presence of micropores (0.02 mlg "1 ) and absence of macropores.
  • the hollow cylinders obtained in this way have a specific surface area of 420 m 2 g "1 , an outer surface of 87 m 2 g “ 1 , a micropore volume of 0.125 mlg “1 , a mesopore volume of 0.228 mlg “ 1 , a macropore volume of 0.453 mlg "1 and threshold diameter of 1700 nm.
  • the mechanical properties of the cylinders obtained are suitable for industrial use; similarly, its structure proved to be perfectly stable to water or water vapor.
  • the static adsorption capacity of the material obtained was determined with different adsorption at temperatures of 22-24 0 C.
  • the values obtained in the corresponding tests were 0.24 g of orthodichlorobenzene, 0.30 g of toluene, 0.31 g of trichlorethylene and 0.36 g of acetone per gram of adsorbent.
  • Example 2 To prepare the adsorbent material, the procedure described in Example 1 is followed, although the dry powder mixture contains alumina and bentonite powder as additives with a weight ratio carbon / sepiolite / alumina / bentonite of 40/52/6/2 .
  • the disintegrated particle size of alumina and bentonite powders is 90% less than 40 ⁇ m.
  • the cylinders thus obtained have a specific surface area of 390 m 2 g "1 , an external surface area of 99 m 2 g “ 1 , a micropore volume of 0,120 mlg “1 , a mesopore volume of 0.207 mlg “ 1 , a volume of macropores of 0.517 mlg “1 and a threshold diameter of 1700 nm.
  • the mechanical properties of the cylinders obtained are appropriate for industrial use, and also their structure remains perfectly stable to water or water vapor.
  • the evaluation of the adsorption capacity in dynamic regime of this material was carried out in a 10 mm reactor. of internal diameter at a pressure of 0.94 kg cnr ⁇ 2 and at 3O 0 C temperature.
  • the cylinders were cut to lengths less than 3 mm. to introduce them into the reactor where they were previously dried at 15 ° C in air flow for 12 hours.
  • the reactor temperature was then lowered to 3O 0 C and maintaining this temperature, an air flow with a content of 10 ppm of o-dichlorobenzene was fed at a linear velocity of 0.32 ms "1 (measured under normal conditions).
  • the concentration of the organic compound at the inlet and outlet of the reactor was measured with a sensitivity of ⁇ 0.1 ppm by means of a flame ionization detector, the break-up time elapsed until the concentration of the o -dichlorobenzene at the outlet reaches the value of 0.3 ppm
  • the amount of o-dichlorobenzene adsorbed in the solid cylinders was 0.14 grams per gram of adsorbent If the density of the liquid o-dichlorobenzene, under the test conditions , is 1, 305 g mi "1 , the adsorbed volume of liquid o-dichlorobenzene will be 0.107 millimeters per gram, very close to the corresponding volume of the micropores of the material.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Geochemistry & Mineralogy (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

La présente invention concerne des matériaux adsorbants qui présentent des structures poreuses appropriées pour leur utilisation dans l'élimination de composés contaminants en régime dynamique. Ces nouveaux matériaux adsorbants sont obtenus à partir de pâtes préparées en milieu aqueux avec des mélanges de poudre de charbon et de poudre d'argiles naturelles présentant une taille de particules désagrégées inférieure à 20 μm pour 90 % d'entre elles. Une fois mis en forme et séchés, lesdits matériaux sont soumis à un traitement thermique unique en présence de vapeur d'eau et de dioxyde de carbone pour obtenir des adsorbants présentant une grande distribution de tailles de pores. La structure desdits matériaux contient les micropores correspondants à ceux du charbon actif qui sont obtenus pendant l'activation du charbon et, de la même manière, contient les mésopores correspondants principalement aux argiles utilisées et les macropores formés à partir des espaces interparticulaires.
PCT/ES2009/070332 2008-09-15 2009-08-03 Composition d'un matériau à structure poreuse, son procédé de préparation et utilisation d'une composition WO2010029201A1 (fr)

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BRPI0804104-0 2008-09-15
BRPI0804104 BRPI0804104A2 (pt) 2008-09-15 2008-09-15 composição de um material com estrutura porosa, método para preparar a mesma e uso de uma composição

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WO2010029201A1 true WO2010029201A1 (fr) 2010-03-18

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108745275A (zh) * 2018-06-07 2018-11-06 中国科学院广州地球化学研究所 一种粘土矿物基材料及其制备方法和应用

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2278535A1 (es) * 2006-01-27 2007-08-01 Aplicacions Biotecnologiques En Salut Alimentacio I Medi Ambient, Bionatur, S.L. Adsorbentes con enstatita en su composicion para operacion de unidades en regimen dinamico.
ES2315179A1 (es) * 2007-06-22 2009-03-16 Jesus Blanco Alvarez Una composicion absorbente que contiene - sepiolita, ensatatita o sus mezclas, metodo de obtencion y uso.

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES2278535A1 (es) * 2006-01-27 2007-08-01 Aplicacions Biotecnologiques En Salut Alimentacio I Medi Ambient, Bionatur, S.L. Adsorbentes con enstatita en su composicion para operacion de unidades en regimen dinamico.
ES2315179A1 (es) * 2007-06-22 2009-03-16 Jesus Blanco Alvarez Una composicion absorbente que contiene - sepiolita, ensatatita o sus mezclas, metodo de obtencion y uso.

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
M.YATES ET AL.: "Vapour adsorption capacity of controlled porosity honeycomb monoliths", MICROPOROUS AND MESOPOROUS MATERIALS, vol. 65, 4 November 2003 (2003-11-04), pages 219 - 231 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108745275A (zh) * 2018-06-07 2018-11-06 中国科学院广州地球化学研究所 一种粘土矿物基材料及其制备方法和应用
CN108745275B (zh) * 2018-06-07 2020-06-12 中国科学院广州地球化学研究所 一种粘土矿物基材料及其制备方法和应用

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AR073299A1 (es) 2010-10-28
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