ES2428442R1 - Deshidrogenación oxidativa de etano a etileno y preparación de catalizador de óxido mezclado multimetálico para tal proceso. - Google Patents

Deshidrogenación oxidativa de etano a etileno y preparación de catalizador de óxido mezclado multimetálico para tal proceso. Download PDF

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Publication number
ES2428442R1
ES2428442R1 ES201331144A ES201331144A ES2428442R1 ES 2428442 R1 ES2428442 R1 ES 2428442R1 ES 201331144 A ES201331144 A ES 201331144A ES 201331144 A ES201331144 A ES 201331144A ES 2428442 R1 ES2428442 R1 ES 2428442R1
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Spain
Prior art keywords
catalyst
ethane
ethylene
application
oxidative dehydrogenation
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Granted
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ES201331144A
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ES2428442A2 (es
ES2428442B1 (es
Inventor
Jaime Sanchez Valente
Jose Manuel López Nieto
Hector ARMENDARIZ HERRERA
Amada MASSO RAMIREZ
Francisco IVARS BARCELO
Maria De Lourdes Alejandra GUZMAN CASTILLO
Roberto QUINTANA SOLÓRZANO
Andrea RODRIGUEZ HERNANDEZ
Paz DEL ANGEL VICENTE
Etel MAYA FLORES
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Pemex Petroquimica
Universidad Politecnica de Valencia
PEMEX PETROQUIMICA
Instituto Mexicano del Petroleo
Original Assignee
Pemex Petroquimica
Universidad Politecnica de Valencia
PEMEX PETROQUIMICA
Instituto Mexicano del Petroleo
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Priority to JP2015537654A priority Critical patent/JP6125023B2/ja
Priority to CN201380065588.2A priority patent/CN104968635B/zh
Priority to PCT/MX2013/000121 priority patent/WO2014062046A1/es
Priority to CA2888633A priority patent/CA2888633C/en
Priority to CA2937242A priority patent/CA2937242C/en
Publication of ES2428442A2 publication Critical patent/ES2428442A2/es
Publication of ES2428442R1 publication Critical patent/ES2428442R1/es
Application granted granted Critical
Publication of ES2428442B1 publication Critical patent/ES2428442B1/es
Priority to JP2016174950A priority patent/JP6369817B2/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/85—Chromium, molybdenum or tungsten
    • B01J23/88—Molybdenum
    • B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/8877—Vanadium, tantalum, niobium or polonium
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    • B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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    • C07C5/42—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor
    • C07C5/48—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor with oxygen as an acceptor
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Abstract

Deshidrogenación oxidativa de etano a etileno y preparación de catalizador de óxido mezclado multimetálico para tal proceso.#La deshidrogenación oxidativa de parafinas ligeras, tal como etano, a temperaturas moderadas (<500ºC) para producir etileno sin la formación de productos secundarios como ácido acético y/u otros hidrocarburos oxigenados, es lograda usando catalizadores multimetálicos libres de teluro, poseyendo la fase ortorrómbica M1 y otras estructuras cristalinas que tienen una función importante en la obtención de los catalizadores de alto rendimiento para la deshidrogenación oxidativa del etano a etileno. Tales catalizadores se prepararon usando métodos térmicos e hidrotérmicos.

Claims (2)

  1. OFICINA ESPAÑOLA DE PATENTES Y MARCAS
    N.º solicitud: 201331144
    ESPAÑA
    Fecha de presentación de la solicitud: 25.07.2013
    Fecha de prioridad:
    INFORME SOBRE EL ESTADO DE LA TECNICA
    51 Int. Cl. : Ver Hoja Adicional
    DOCUMENTOS RELEVANTES
    Categoría
    56 Documentos citados Reivindicaciones afectadas
    X
    P. BOTELLA et al., “Selective oxidative dehydrogenation of ethane over MoVSbO mixed oxide 1-6,10-15,
    catalysts”, Applied Catalysis A: General, 2006, vol. 298, páginas 16-23.
    19-22,26,28-31
    X
    US 4524236 A (J. H. MCCAIN) 18.06.1985, 1-10,16-18,
    columna 2, línea 64 – columna 3, línea 46; columna 5, líneas 8-47; Tablas I y II.
    23-25,27
    X
    F. IVARS et al., “Selective oxidation of propane over AMoVSbO catalysts (A=Li,Na,K,Rb,Cs)”, Topics in Catalysis, 2008, vol. 50, nº 1-4, páginas 74-81. 23-25,27,29
    A
    EP 544372 A1 (ENIRICERCHE) 02.06.1993, página 2, línea 25 – página 3, línea 42; reivindicaciones. 1-31
    A
    WO 03064035 A1 (CONSEJO SUPERIOR DE INVESTIGACIONES CIENTÍFICAS, UNIVERSIDAD POLITÉCNICA DE VALENCIA) 07.08.2003, todo el documento. 1-31
    A
    US 7319179 B2 (J. M. LOPEZ-NIETO et al.) 15.01.2008, todo el documento. 1-31
    Categoría de los documentos citados X: de particular relevancia Y: de particular relevancia combinado con otro/s de la misma categoría A: refleja el estado de la técnica O: referido a divulgación no escrita P: publicado entre la fecha de prioridad y la de presentación de la solicitud E: documento anterior, pero publicado después de la fecha de presentación de la solicitud
    El presente informe ha sido realizado • para todas las reivindicaciones • para las reivindicaciones nº:
    Fecha de realización del informe 11.02.2014
    Examinador E. Dávila Muro Página 1/4
    INFORME DEL ESTADO DE LA TÉCNICA
    Nº de solicitud: 201331144
    CLASIFICACIÓN OBJETO DE LA SOLICITUD
    B01J23/28 (2006.01) B01J23/22 (2006.01) B01J23/18 (2006.01) C07C5/48 (2006.01) C07C11/04 (2006.01)
    Documentación mínima buscada (sistema de clasificación seguido de los símbolos de clasificación)
    C07C, B01J
    Bases de datos electrónicas consultadas durante la búsqueda (nombre de la base de datos y, si es posible, términos de búsqueda utilizados)
    INVENES, EPODOC, WPI, XPESP, NLP, REGISTRY, CAPLUS
    Informe del Estado de la Técnica Página 2/4
    OPINIÓN ESCRITA
    Nº de solicitud: 201331144
    Fecha de Realización de la Opinión Escrita: 11.02.2014
    Declaración
    Novedad (Art. 6.1 LP 11/1986)
    Reivindicaciones Reivindicaciones 1-31 SI NO
    Actividad inventiva (Art. 8.1 LP11/1986)
    Reivindicaciones Reivindicaciones 1-31 SI NO
    Se considera que la solicitud cumple con el requisito de aplicación industrial. Este requisito fue evaluado durante la fase de examen formal y técnico de la solicitud (Artículo 31.2 Ley 11/1986).
    Base de la Opinión.-
    La presente opinión se ha realizado sobre la base de la solicitud de patente tal y como se publica.
    Informe del Estado de la Técnica Página 3/4
    OPINIÓN ESCRITA
    Nº de solicitud: 201331144
    1. Documentos considerados.-
    A continuación se relacionan los documentos pertenecientes al estado de la técnica tomados en consideración para la realización de esta opinión.
    Documento
    Número Publicación o Identificación Fecha Publicación
    D01
    P. BOTELLA et al., Applied Catalysis A: General, 2006, vol. 298, pgs. 16-23 2006
    D02
    US 4524236 A (J. H. MCCAIN) 18.06.1985
    D03
    F. IVARS et al., Topics in Catalysis, 2008, vol. 50, nº 1-4, pgs. 74-81 2008
  2. 2. Declaración motivada según los artículos 29.6 y 29.7 del Reglamento de ejecución de la Ley 11/1986, de 20 de marzo, de Patentes sobre la novedad y la actividad inventiva; citas y explicaciones en apoyo de esta declaración
    La invención se refiere a un proceso para la deshidrogenación oxidativa de etano a etileno que comprende hacer reaccionar etano con un agente oxidante en presencia de una catalizador sólido de óxido mixto multimetálico libre de Te y de fórmula MoVhSbjAjOx, siendo A= Nb, W, Ga, Bi, Sn, Cu, Ti, Fe, Co, Ni, Cr, Zr, metales de tierras raras o metales alcalinos. La invención también se refiere al método de obtención del catalizador y al catalizador de óxido mixto multimetálico de fórmulas MoVhSbjAjOx y MoVhSbjOx obtenidos por dicho procedimiento.
    El documento D01 divulga un proceso selectivo de deshidrogenación oxidativa de etano utilizando un catalizador MoVhSbjOx el cual no incluye Te en su composición. Este catalizador se prepara mediante tratamiento hidrotérmico a 175ºC de una solución de los correspondientes precursores metálicos seguido de activación por calcinación en corriente de nitrógeno a 425ºC-700ºC (ver página 17). Su caracterización permite observar una fase cristalina M1 y otras fases cristalinas M2 y/o MoO3 adicionales (ver Tabla 1 y página 19). El proceso de deshidrogenación oxidativa del etano utilizando este catalizador se lleva a cabo en un reactor a temperatura de 340ºC-400ºC, presión atmosférica y velocidad de flujo de 25-100 ml min-1. Se consigue una conversión de etano superior al 60% y una selectividad a etileno superior al 80% utilizando un catalizador de este tipo (ver páginas 17-19).
    El documento D02 divulga un procedimiento para la deshidrogenación oxidativa de etano a etileno a baja temperatura utilizando un catalizador óxido calcinado de fórmula MoaVbNbcSbdXe siendo X al menos un metal del grupo Li,Sc,Na,Be, Mg,Ca,Sr,Ba,Ti,Zr,Hf,Y,Ta,Cr,Fe,Co,Ni,Ce,La,Zn,Cd,Hg,Al,Tl,Pb,As,Bi,Te,U,W presentes en combinación con oxígeno en forma de varios óxidos. El catalizador se prepara mediante tratamiento hidrotérmico de una solución de los precursores metálicos a 20ºC-100ºC seguido de activación mediante calcinación a 220ºC-550ºC en corriente de aire u oxígeno. El proceso de deshidrogenación oxidativa del etano se lleva a cabo en un reactor a presión de 1-30 atmósferas, temperatura de 150ºC-450ºC, tiempo de contacto entre la mezcla de reacción y el catalizador de 0,1-100 segundos y velocidad espacial de 50-5000 h-1. Se consigue una selectividad a etileno mayor de 75% para una conversión de etano del 50% (ver columna 2, línea 64-columna 3, línea 46, columna 5, líneas 14-47). En los ejemplos recogidos en D02 se divulgan numerosos catalizadores de distinta composición pero ninguno incluye Te en su formulación (ver Tablas I y II).
    El documento D03 un procedimiento para la oxidación selectiva de propano utilizando un catalizador óxido calcinado de fórmula A-MoVSbO siendo A un metal alcalino (A=Li,Na,K,Rb,Cs). El catalizador se prepara por tratamiento hidrotérmico a 175ºC de una solución de los precursores metálicos y se activa mediante calcinación a 600ºC en atmósfera inerte. El proceso de conversión del propano se lleva a cabo en un reactor a presión atmosférica y temperatura de 340ºC-420ºC (ver páginas 75-76). Los catalizadores divulgados en D03 no incluyen Te en su formulación y presentan una fase cristalina M1 y otras fases cristalinas M2 y/o MoO3 adicionales (ver Tablas 1 y 2, y páginas 77-78).
    En consecuencia, a la vista de lo divulgado en los documentos D01-D03 se considera que el objeto de la invención recogido en las reivindicaciones 1-31 no cumple los requisitos de novedad ni actividad inventiva según los Arts. 6.1 y 8.1 LP/1986.
    Informe del Estado de la Técnica Página 4/4
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