EP2328854A1 - Procédé et dispositif de fabrication de méthanol - Google Patents

Procédé et dispositif de fabrication de méthanol

Info

Publication number
EP2328854A1
EP2328854A1 EP09777512A EP09777512A EP2328854A1 EP 2328854 A1 EP2328854 A1 EP 2328854A1 EP 09777512 A EP09777512 A EP 09777512A EP 09777512 A EP09777512 A EP 09777512A EP 2328854 A1 EP2328854 A1 EP 2328854A1
Authority
EP
European Patent Office
Prior art keywords
gas
methanol
reactor
mixture
heat exchanger
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP09777512A
Other languages
German (de)
English (en)
Inventor
Hans Kopetsch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide Global E&C Solutions Germany GmbH
Original Assignee
Lurgi GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lurgi GmbH filed Critical Lurgi GmbH
Publication of EP2328854A1 publication Critical patent/EP2328854A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
    • C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
    • C07C29/1516—Multisteps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
    • B01D5/009—Collecting, removing and/or treatment of the condensate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
    • B01D5/0093—Removing and treatment of non condensable gases
    • 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
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • B01J8/067—Heating or cooling the reactor
    • 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
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00106—Controlling the temperature by indirect heat exchange
    • B01J2208/00265—Part of all of the reactants being heated or cooled outside the reactor while recycling
    • B01J2208/00274—Part of all of the reactants being heated or cooled outside the reactor while recycling involving reactant vapours
    • 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/0004—Processes in series

Definitions

  • the invention relates to the production of methanol from a synthesis gas containing hydrogen and carbon oxides, wherein passing the synthesis gas through a first, preferably water-cooled reactor in which a portion of the carbon oxides is catalytically converted to methanol, and wherein the obtained synthesis gas and methanol vapor Mixture a second, preferably gas-cooled reactor feeds, in which a further portion of the carbon oxides is converted to methanol.
  • Such a process for the production of methanol is known, for example, from EP 0 790 226 B1.
  • the methanol is produced in a cyclic process in which a mixture of fresh and partially reacted synthesis gas is first fed to a water-cooled reactor and then to a gas-cooled reactor in which the synthesis gas is converted to methanol on a copper-based catalyst.
  • the methanol produced in the process is separated from the synthesis gas to be recycled, which is then passed as a coolant in countercurrent through the gas-cooled reactor and preheated to a temperature of 220 to 280 0 C before it is introduced into the first synthesis reactor.
  • FR 2 533 554 A1 describes a process for preparing alcohols from synthesis gas in two reactor stages, wherein a liquid fraction rich in methanol and higher alcohols is separated from the product of the second reactor stage by condensation from the gas stream.
  • the gas stream is at least partially recycled to the first reactor stage to increase the ratio H 2 / CO to a value> 1.8.
  • Intermediate condensation of methanol between the two reactor stages should be avoided in order to reduce the water content of the resulting mixture and thereby facilitate the subsequent dehydrogenation of the alcohols.
  • U.S. Patent 4,968,722 discloses a process for the production of methanol in which the methanol product is removed by absorption between two reactor stages to thereby increase the product yield of the equilibrium reaction in the second reactor stage.
  • an intermediate condensation is described as disadvantageous since it requires large heat exchange surfaces.
  • EP 0 483 919 A2 describes a process for the production of methanol, in which the reaction of the synthesis gas takes place in a plurality of fluidized bed reactors connected in series, wherein a separation of methanol formed by cooling and condensation takes place between the reactor stages.
  • the object of the invention is to reliably avoid the condensation of methanol on the second reactor, in particular when using highly active catalysts.
  • the dew point of the entering into the second reactor mixture depends essentially on the methanol concentration.
  • the dew point of the mixture is significantly lowered to about 40 ° C. (namely, the temperature in the preceding methanol separator), so that there is no danger of methanol condensation in the second reactor, since the distance the temperature of the reactor components from the dew point is also sufficiently large at the outlet of the second reactor to reliably avoid dew point undershoot.
  • the methanol yield of the second reactor stage can be increased since the reaction equilibrium is shifted to the product side or a higher reaction potential for the conversion of the gas in the second reactor is created.
  • a particularly economical use of the system is achieved if the withdrawn from the methanol separator gas stream is preheated in the gas / gas heat exchanger before it is fed to the second reactor. As a result, the heat is kept in the system and used for necessary heating of the gas stream to the required reaction temperature in the second reactor.
  • the invention also extends to a plant for the production of methanol from a synthesis gas containing hydrogen and carbon oxides, which is suitable for carrying out the method described above.
  • the plant comprises a first, preferably water-cooled, reactor in which part of the carbon oxides is catalytically converted to methanol, a second, preferably gas-cooled, reactor to which the gas mixture obtained from the first reactor is fed via a line and in which another part of the carbon oxides is reacted to methanol, and a methanol separator for separating the methanol from the synthesis gas.
  • a gas / gas heat exchanger for cooling the gas mixture obtained from the first reactor is provided following the first reactor.
  • At least one additional heat exchanger for further cooling of the gas mixture is provided between the gas / gas heat exchanger and the methanol separator.
  • a line leads from the methanol separator to the inlet of the second reactor, via which the separated synthesis gas is fed to the second reactor for further reaction.
  • the conduit is preferably passed through the gas / gas heat exchanger to preheat the syngas to the required reaction temperature while achieving optimum utilization of the thermal energy.
  • the single figure shows schematically a plant for carrying out the process according to the invention
  • a mixture of fresh and recirculated synthesis gas is passed through a line 1 into a first synthesis reactor 2.
  • This first reactor 2 is preferably a tube reactor known per se, in which, for example, a copper-based catalyst is arranged in tubes 3.
  • a coolant used under elevated pressure boiling water which is introduced in the conduit 4.
  • a mixture of boiling water and steam is withdrawn in line 5 and leads to the energy of a steam drum, not shown, known per se.
  • the synthesis gas entering the first reactor 2 is preheated to a suitable temperature sufficient to respond to the catalyst. It is also possible initially to heat the synthesis gas only to a temperature below the response temperature of the catalyst and to achieve the further preheating over the hot water jacket in the reactor. The water temperature must of course be above the response temperature of the catalyst.
  • the gas temperature at the inlet of the first reactor 2 at 180 to 250 0 C and the pressure in the range of 2 to 12 MPa (20 to 120 bar), preferably in the range of 4 to 10 MPa (40 to 100 bar).
  • the coolant, which is withdrawn via the line 5, usually has a temperature in the range of 220 to 280 0 C.
  • In the first reactor 2 are in an exothermic reaction, depending on the state of the catalyst 40 to 80% of the through the line 1 in the Reactor 2 given carbon oxides implemented.
  • a first mixture essentially consisting of synthesis gas and methanol vapor, is withdrawn via line 6, the methanol content being 4 to 10% by volume, usually 5 to 8% by volume.
  • This mixture is preferably passed completely through a gas / gas heat exchanger 7 to lower the temperature below the dew point of the methanol by heat exchange with synthesis gas recycled via the line 8.
  • the dew point temperature depends essentially on the concentration of the methanol and is at a methanol concentration at the outlet of the first reactor 2 of, for example. 7 mol% at about 125 0 C.
  • the gas / liquid mixture passes through at least one further heat exchanger 9 in order to lower the temperature even further.
  • This second heat exchanger is preferably air or water cooled.
  • the gas / liquid mixture is then fed to a methanol separator 10, in which the liquid methanol phase is separated from the gas phase.
  • the largely methanol-free gas stream is via the line. 8 - 7 - KEIL & SCHAAFHAUSEN
  • the so preheated gas stream reactor via line 8 to a second synthesis 11 supplied, for example, is configured with a copper-based catalyst as provided with cooling tubes 12 fixed bed reactor.
  • the catalyst is preferably provided on the shell side, but may also be arranged in the tubes as in the first reactor 2.
  • synthesis gas which is introduced via the line 13 at a temperature of 40 to 150 0 C and the second reactor 11 in cocurrent with the brought up via the line 8, preheated in the gas / gas heat exchanger 7 gas stream flows through from the first reactor 2.
  • the temperature of the cooling gas at the inlet to the second reactor 11 is determined by the mixing ratio between recirculated and fresh synthesis gas and is chosen the lower the higher the reactivity of the introduced via the line 8 gas flow into the second reactor 11.
  • the synthesis gas serving as a coolant is preheated in the second reactor 11 and then flows through the line 1 to the first reactor 2.
  • the synthesis gas entering the first reactor 2 should have hydrogen and carbon oxides in approximately the following proportions:
  • a product mixture essentially containing synthesis gas and methanol vapor leaves the second reactor 11 through a line 14 and flows in a known manner through a cooler, not shown, with methanol being condensed. Subsequently, gases and liquid are separated in a separation tank and the crude methanol product is removed and purified by distillation. The gases are then passed with the aid of a compressor as synthesis gas to be recycled (recycle gas) via the line 13 through the second reactor 11 and, after the preheating thus carried out, into the first reactor 2. Some of the gases are removed from the cycle (purge), as usual, to limit the accumulation of inert components.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

Pour la fabrication de méthanol à partir d'un gaz de synthèse contenant de l'hydrogène et des oxydes de carbone, le gaz de synthèse est guidé à travers un premier réacteur de préférence refroidi par eau dans lequel une fraction des oxydes de carbone est transformée en méthanol par catalyse. Le mélange obtenu contenant du gaz de synthèse et de la vapeur de méthanol est guidé vers un deuxième réacteur de préférence refroidi par gaz, dans lequel une fraction ultérieure des oxydes de carbone est transformée en méthanol. Le mélange extrait du premier réacteur est guidé à travers un échangeur thermique gaz/gaz dans lequel le mélange est refroidi jusqu'à une température inférieure à son point de rosée. Puis, dans un séparateur de méthanol, le méthanol est séparé du flux de gaz et extrait tandis que le flux de gaz résiduel est acheminé vers le deuxième réacteur.
EP09777512A 2008-09-30 2009-07-29 Procédé et dispositif de fabrication de méthanol Withdrawn EP2328854A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008049622A DE102008049622B4 (de) 2008-09-30 2008-09-30 Verfahren und Anlage zur Herstellung von Methanol
PCT/EP2009/005484 WO2010037441A1 (fr) 2008-09-30 2009-07-29 Procédé et dispositif de fabrication de méthanol

Publications (1)

Publication Number Publication Date
EP2328854A1 true EP2328854A1 (fr) 2011-06-08

Family

ID=41202562

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09777512A Withdrawn EP2328854A1 (fr) 2008-09-30 2009-07-29 Procédé et dispositif de fabrication de méthanol

Country Status (5)

Country Link
US (1) US8629190B2 (fr)
EP (1) EP2328854A1 (fr)
CN (2) CN102171170A (fr)
DE (1) DE102008049622B4 (fr)
WO (1) WO2010037441A1 (fr)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2624947B1 (fr) 2010-10-06 2016-04-27 Silicon Fire AG Procédé et installation de synthèse d'hydrocarbure
EP2438980A1 (fr) 2010-10-06 2012-04-11 Silicon Fire AG Procédé et dispositif de préparation et d'installation de méthanol à base d'hydrogène à des fins de dénitrification
EP2438982A1 (fr) 2010-10-06 2012-04-11 Silicon Fire AG Procédé de préparation et d'utilisation d'un alcool et utilisation de l'alcool pour l'augmentation du degré d'action et de la puissance d'un moteur à combustion interne
EA029293B1 (ru) * 2012-07-18 2018-03-30 Хальдор Топсёэ А/С Способ и реакционная система для получения метанола
CN103768824A (zh) * 2012-10-23 2014-05-07 北京日新达能技术有限公司 丙烯醛废气处理系统
WO2014166536A1 (fr) 2013-04-11 2014-10-16 Silicon Fire Ag Procede et dispositif de réglage de puissance d'un moteur à combustion interne
EP3016924A1 (fr) 2013-04-26 2016-05-11 Silicon Fire AG Procédé et système de réacteur de synthèse de méthanol avec recyclage du gaz circulant et du gaz de purge
EP3126042A1 (fr) * 2014-04-02 2017-02-08 Haldor Topsøe A/S Réacteur pseudo-isotherme
CN104353329B (zh) * 2014-11-25 2016-11-30 北京时代浩鼎科技股份有限公司 甲醇分离器
CN107635956B (zh) 2015-05-11 2020-11-13 托普索公司 一种用于甲醇合成的新方法
CN105218310B (zh) * 2015-10-23 2017-06-13 湖南安淳高新技术有限公司 甲醇合成反应装置及甲醇合成反应方法
DK3205622T3 (en) 2016-02-11 2018-08-06 Ulrich Wagner METHOD OF SYNTHESIS OF METHANOL
DE102017206763A1 (de) * 2017-04-21 2018-10-25 Siemens Aktiengesellschaft Verfahren und Vorrichtung zum Umsetzen von Kohlenstoffdioxid zu Methanol
EP3401006A1 (fr) * 2017-05-11 2018-11-14 Casale Sa Convertisseur catalytique à lit multiple avec refroidissement inter-lit
EP3401300B1 (fr) 2017-05-12 2021-06-23 L'air Liquide, Société Anonyme Pour L'Étude Et L'exploitation Des Procédés Georges Claude Procédé pour la production du méthanol
EP3401299B1 (fr) 2017-05-12 2021-11-03 L'air Liquide, Société Anonyme Pour L'Étude Et L'exploitation Des Procédés Georges Claude Réacteur destiné à effectuer des réactions d'équilibre exothermiques
WO2020157566A1 (fr) * 2019-01-31 2020-08-06 Sabic Global Technologies, B.V. Configuration de synthèse en boucle de gaz de synthèse en méthanol
EP3714971B1 (fr) 2019-03-28 2022-02-02 Sener, Ingeniería y Sistemas, S.A. Système et procédé de production de méthanol à partir d'un gaz de synthèse riche en hydrogène et co2/co
EP3741738B1 (fr) 2019-05-22 2022-09-21 L'air Liquide, Société Anonyme Pour L'Étude Et L'exploitation Des Procédés Georges Claude Procédé de fabrication de méthanol
EP3808724A1 (fr) 2019-10-16 2021-04-21 L'air Liquide, Société Anonyme Pour L'Étude Et L'exploitation Des Procédés Georges Claude Procédé de fabrication de méthanol par synthèse en plusieurs étapes
EP3808725A1 (fr) 2019-10-16 2021-04-21 L'air Liquide, Société Anonyme Pour L'Étude Et L'exploitation Des Procédés Georges Claude Procédé de fabrication en plusieurs étapes de méthanol
EP4015496B8 (fr) 2020-12-15 2023-06-07 L'Air Liquide, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Procédé et installation de production de méthanol à partir de gaz de synthèse substochiométrique
EP4180386A1 (fr) 2021-11-16 2023-05-17 TotalEnergies OneTech Procédé de conversion continue de h2s en h2 et en soufre

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0152648A1 (fr) * 1984-02-02 1985-08-28 Metallgesellschaft Ag Procédé pour la production d'un mélange de méthanol et d'alcools supérieurs
EP1210309B1 (fr) * 1999-09-07 2003-12-03 Uhde GmbH Procede et installation pour la production de methanol
WO2006018610A1 (fr) * 2004-08-20 2006-02-23 Davy Process Technology Ltd Processus destine a une utilisation dans des reactions en phase gazeuse

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FR2533554A1 (fr) 1982-09-23 1984-03-30 Inst Francais Du Petrole Production d'alcools a partir de gaz de synthese
ES2026632T3 (es) 1988-02-05 1992-05-01 Process Engineering Consultants Pec B.V. Un procedimiento para producir metanol.
CA2053578A1 (fr) 1990-10-29 1992-04-30 Swan T. Sie Procede de production de methanol
GB9023465D0 (en) 1990-10-29 1990-12-12 Shell Int Research Process for the production of methanol
DE19605572A1 (de) * 1996-02-15 1997-08-21 Metallgesellschaft Ag Verfahren zum Erzeugen von Methanol
DE102004028200B3 (de) 2004-05-28 2005-12-15 Hippweb E.K. Verfahren zur Durchführung heterogen katalytischer exothermer Gasphasenreaktionen für die Methanolsynthese

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0152648A1 (fr) * 1984-02-02 1985-08-28 Metallgesellschaft Ag Procédé pour la production d'un mélange de méthanol et d'alcools supérieurs
EP1210309B1 (fr) * 1999-09-07 2003-12-03 Uhde GmbH Procede et installation pour la production de methanol
WO2006018610A1 (fr) * 2004-08-20 2006-02-23 Davy Process Technology Ltd Processus destine a une utilisation dans des reactions en phase gazeuse

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
FRIEDRICH ASINGER: "Methanol - Chemie- und Energierohstoff - Die Mobilisation der Kohle", 1986 *
See also references of WO2010037441A1 *

Also Published As

Publication number Publication date
US20110178187A1 (en) 2011-07-21
DE102008049622B4 (de) 2012-10-31
WO2010037441A1 (fr) 2010-04-08
DE102008049622A1 (de) 2010-04-22
CN102171170A (zh) 2011-08-31
CN105732313B (zh) 2018-12-04
US8629190B2 (en) 2014-01-14
CN105732313A (zh) 2016-07-06

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