WO2015106952A1 - Procédé et dispositif de production de diméthyle éther - Google Patents

Procédé et dispositif de production de diméthyle éther Download PDF

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Publication number
WO2015106952A1
WO2015106952A1 PCT/EP2015/000005 EP2015000005W WO2015106952A1 WO 2015106952 A1 WO2015106952 A1 WO 2015106952A1 EP 2015000005 W EP2015000005 W EP 2015000005W WO 2015106952 A1 WO2015106952 A1 WO 2015106952A1
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WO
WIPO (PCT)
Prior art keywords
synthesis gas
carbon dioxide
hydrogen
separated
separation
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.)
Ceased
Application number
PCT/EP2015/000005
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German (de)
English (en)
Inventor
Thomas Bartesch
Andreas Peschel
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.)
Linde GmbH
Original Assignee
Linde 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 Linde GmbH filed Critical Linde GmbH
Publication of WO2015106952A1 publication Critical patent/WO2015106952A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01—Preparation of ethers
    • 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
    • B01J2219/00004—Scale aspects
    • B01J2219/00006—Large-scale industrial plants

Definitions

  • the invention relates to a process for the production of dimethyl ether, wherein from a carbon dioxide, hydrogen and carbon monoxide-containing synthesis gas
  • Carbon dioxide is removed to obtain a predominantly consisting of carbon monoxide and hydrogen feed gas, which is subsequently reacted in a single-stage process to dimethyl ether.
  • the invention relates to a device for carrying out the
  • DME Dimethyl ether
  • DME burns without the formation of soot and sulfur oxides and has an octane equivalent to that of diesel, it is appropriate to replace, or at least supplement, LPG and diesel fuel as motor vehicles. To what extent DME can take on this role in the future depends not least on the costs incurred for its production.
  • DME is produced on an industrial scale in two-stage process, wherein in the first stage from a synthesis gas methanol is produced from the
  • Oxygen is generated by tri-reforming. This process is not very flexible with regard to the synthesis gas composition and, not least because of the required air fractionator, is also expensive. In particular, when the synthesis gas is obtained by steam reforming from natural gas alone, the molar H 2 / CO ratios necessary for the direct DME synthesis can not be realized in practice even with the use of internal carbon dioxide recirculation.
  • Object of the present invention is therefore to provide a method of the type described above and a device for its implementation, by which it is possible to use syngas with comparatively high molar H 2 / CO ratios for the direct DME synthesis can.
  • Synthesis gas is separated to obtain the feed gas with a defined molar ratio of hydrogen to carbon monoxide whose value is between 0.9 and 2.0, preferably between 1, 0 and 1, 5 and more preferably between 1, 1 and 1, 4 lies.
  • the hydrogen is only separated from the synthesis gas after carbon dioxide has been completely or partially removed. It is advantageous under and the increased hydrogen partial pressure resulting from the separation of the carbon dioxide from the synthesis gas, which allows separation of the hydrogen with a higher selectivity, thus minimizing the losses of valuable CO and CO 2 in this process step.
  • the separation of the hydrogen any method known from the prior art for the separation of hydrogen from synthesis gas can be used.
  • the hydrogen from the synthesis gas is via a
  • Permeate side of the hydrogen is obtained. Further developing the invention, it is proposed to treat the synthesis gas with the aid of a multistage membrane reactor, so that separated hydrogen is produced at at least two different pressure stages. In order to adjust the hydrogen content to the desired value, it may be useful to split the synthesis gas into two partial streams, of which only one is subjected to hydrogen separation, while the second is passed unchanged in the bypass and subsequently combined with the partial stream reduced in hydrogen content.
  • heat required for synthesis gas production is provided in whole or in part by means of hot flue gases which are generated by one or more burners and whose heat is transferred to the reactants by indirect heat exchange, as is the case, for example, in steam reforming, a preferred embodiment provides
  • Embodiment of the inventive method from the synthesis gas separated hydrogen supply at least one of these burners as fuel.
  • Further embodiments of the method according to the invention provide for purifying at least part of the hydrogen fraction separated from the synthesis gas in order to obtain a hydrogen fraction of increased purity and subsequently to use this for desulfurization of an insert for synthesis gas production and / or to deliver it as a hydrogen product against credit.
  • To separate carbon dioxide from the synthesis gas is preferably a
  • Sour gas scrubbing such as an amine or a methanol wash used.
  • the carbon dioxide removal is suitably operated so that a feed gas for the DME synthesis can be obtained, the carbon dioxide content is between 100ppm and 5mol%.
  • the separated from the synthesis gas carbon dioxide is suitably compressed, recycled and used in the production of synthesis gas. In order to prevent accumulated in the process along with the separated carbon dioxide, under the conditions of syngas production inert substances, part of the carbon dioxide fraction can be discharged as a purge and used elsewhere or disposed of.
  • Feed gas for direct DME synthesis is preferably to a value
  • Synthesis gas preferably upstream of carbon dioxide separation
  • the compression step can take place upstream or downstream of the methanol wash.
  • a further embodiment of the method according to the invention provides that a carbon dioxide fraction obtained in the device for the separation of carbon dioxide is completely or partially recycled and used as starting material for the synthesis gas production. Furthermore, it should also be possible to accumulate elsewhere or supplied from outside the process carbon dioxide for
  • a preferred embodiment of the method according to the invention provides that the synthesis gas to be treated is produced by dry reforming or steam and / or autothermal reforming or steam reforming and / or partial oxidation (POX) from natural gas using water and / or carbon dioxide as feedstocks.
  • POX partial oxidation
  • the invention relates to a device for the production of dimethyl ether with a synthesis gas generator, a device for the separation of carbon dioxide from a producible in the synthesis gas generator, carbon dioxide, hydrogen and
  • the stated object is achieved in that it comprises a device for separating hydrogen, in which hydrogen can be separated from the synthesis gas in order to separate the feed gas, which is in fluid communication both with the device for separating off carbon dioxide and with the DME reactor with a defined molar ratio of hydrogen to carbon monoxide whose value is between 0.9 and 2.0, preferably between 1, 0 and 1, 5 and particularly preferably between 1, 1 and 1, 4.
  • the means for separating hydrogen is designed as a single or multi-stage membrane system, with the aid of which the separated
  • Hydrogen can be obtained at one or more different pressure levels.
  • the means for separating hydrogen is preferably arranged downstream of the means for separating carbon dioxide; an arrangement
  • the means for separating carbon dioxide may be any means known in the art for separating carbon dioxide
  • Synthesis gas is known.
  • the device for separating off is preferred 5 000005
  • Carbon dioxide as amine or methanol wash or as a membrane system.
  • a further preferred embodiment of the device according to the invention provides a compressor arranged upstream of the DME reactor, which is located downstream of the device for separating off carbon dioxide, if this is designed as amine scrubbing or as a membrane system. If the means for separating carbon dioxide is a methanol wash, it is possible to place the compressor upstream or downstream thereof.
  • the compressor can be equipped with several sections as well as with intercooling and
  • Gas / liquid separation be carried out and is suitably operable so that in the DME reactor unreacted feedstocks can be recycled without further compression step in the synthesis gas to be treated, preferably upstream of the carbon dioxide separation.
  • the device according to the invention can be a recycle compressor
  • Entrance side of the synthesis gas generator is connected so that separated from the synthesis gas carbon dioxide is returned to the synthesis gas generator and as
  • Feedstock for synthesis gas production can be used.
  • the recycle compressor with multiple sections and with intermediate cooling and
  • Each of the sections of the recycle compressor may be connected to a carbon dioxide source inside and / or outside of the device according to the invention, in which carbon dioxide is obtained at the pressure level corresponding to the compressor section, so that carbon dioxide from this source also with the help of the recycle compressor as the synthesis gas generator Use can be fed.
  • the synthesis gas generator is one
  • the invention makes it possible to control the composition of the feed gas for direct DME synthesis in a relatively simple manner and to adapt to changing synthesis conditions, as for example by the aging of the DME synthesis of the catalyst used or the change of the catalyst type can occur.
  • it allows the use of a steam reformer for synthesis gas production, in its operation can be dispensed with an expensive air separator.
  • the embodiment shows a device for producing dimethyl ether from a hydrogen-rich synthesis gas by direct DME synthesis.
  • synthesis gas generator S which is, for example, a steam or an autothermal reformer or a combination of steam and autothermal reformer, a carbon dioxide, hydrogen and carbon monoxide
  • the synthesis gas 1 is therefore first supplied to the means for separating carbon dioxide C, which is preferably carried out as amine or methanol wash to separate excess carbon dioxide 2, which is then fed via the compressor V1 to the synthesis gas generator S as insert 3 to the carbon monoxide content of the synthesis gas 1 raise.
  • the reduced in carbon dioxide synthesis gas 4 is subsequently continued in the device for the separation of hydrogen H to adjust the hydrogen / carbon monoxide ratio, optionally by the separation of hydrogen to a defined value.
  • the separated from the synthesis gas stream 4 hydrogen fraction 6 is withdrawn from the device for the separation of hydrogen H, which is preferably designed as a single or multi-stage membrane system, and used for example as a fuel for firing the synthesis gas generator S. It is also conceivable to subject all or part of the hydrogen fraction 6 to purification (not shown) and then to release it as a hydrogen product.
  • the pressure of generated in the device for the separation of hydrogen H is also conceivable to subject all or part of the hydrogen fraction 6 to purification (not shown) and then to release it as a hydrogen product.
  • the carbon dioxide-rich residual gas stream 10 at least partially as a recycle gas (not shown in Figure 1) the compressor V1 and / or the carbon dioxide separation C are supplied.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

La présente invention concerne un procédé et un dispositif de production de diméthyle éther (9), le dioxyde de carbone (2) étant séparé du gaz de synthèse (1) contenant du dioxyde de carbone, de l'hydrogène et du monoxyde de carbone pour obtenir un gaz d'alimentation (7), composé essentiellement de monoxyde de carbone et d'hydrogène, qui est ensuite converti dans un processus (D) à une étape en diméthyle éther (9). Il est caractéristique que l'hydrogène (6) soit, le cas échéant, séparé du gaz de synthèse pour obtenir le gaz d'alimentation (7) avec un rapport molaire défini entre hydrogène et monoxyde de carbone dont la valeur est comprise entre 0,9 et 2,0, de préférence entre 1,0 et 1,5 et plus préférablement entre 1,1 et 1,4, afin d'obtenir un gaz d'alimentation idéal, d'un point de vue de toute la technique des procédés, pour la synthèse directe du DME.
PCT/EP2015/000005 2014-01-16 2015-01-05 Procédé et dispositif de production de diméthyle éther Ceased WO2015106952A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102014000507.0A DE102014000507A1 (de) 2014-01-16 2014-01-16 Verfahren und Vorrichtung zur Erzeugung von Dimethylether
DE102014000507.0 2014-01-16

Publications (1)

Publication Number Publication Date
WO2015106952A1 true WO2015106952A1 (fr) 2015-07-23

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PCT/EP2015/000005 Ceased WO2015106952A1 (fr) 2014-01-16 2015-01-05 Procédé et dispositif de production de diméthyle éther

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DE (1) DE102014000507A1 (fr)
WO (1) WO2015106952A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3521267A1 (fr) * 2017-11-22 2019-08-07 Linde Aktiengesellschaft Procédé d'obtention de diméthyléther et de dioxyde de carbone

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102023121868A1 (de) * 2023-08-16 2025-02-20 Forschungszentrum Jülich GmbH Verfahren zur Erzeugung von elektrischem Strom und/oder Wärme

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060287405A1 (en) * 2005-06-17 2006-12-21 Korea Gas Corporation Process for the preparation of dimethylether from hydrocarbons
WO2009007113A1 (fr) * 2007-07-12 2009-01-15 Haldor Topsøe A/S Procédé de préparation d'éther diméthylique
DE102012001804A1 (de) * 2012-01-31 2013-08-01 Linde Aktiengesellschaft Verfahren zur direkten Dimethylethersynthese aus Synthesegas

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060287405A1 (en) * 2005-06-17 2006-12-21 Korea Gas Corporation Process for the preparation of dimethylether from hydrocarbons
WO2009007113A1 (fr) * 2007-07-12 2009-01-15 Haldor Topsøe A/S Procédé de préparation d'éther diméthylique
DE102012001804A1 (de) * 2012-01-31 2013-08-01 Linde Aktiengesellschaft Verfahren zur direkten Dimethylethersynthese aus Synthesegas

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3521267A1 (fr) * 2017-11-22 2019-08-07 Linde Aktiengesellschaft Procédé d'obtention de diméthyléther et de dioxyde de carbone

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DE102014000507A1 (de) 2015-07-16

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