EP1214281A1 - Procede de preparation de dimethyl ether - Google Patents

Procede de preparation de dimethyl ether

Info

Publication number
EP1214281A1
EP1214281A1 EP00964077A EP00964077A EP1214281A1 EP 1214281 A1 EP1214281 A1 EP 1214281A1 EP 00964077 A EP00964077 A EP 00964077A EP 00964077 A EP00964077 A EP 00964077A EP 1214281 A1 EP1214281 A1 EP 1214281A1
Authority
EP
European Patent Office
Prior art keywords
heat transfer
dimethyl ether
transfer apparatus
methanol
combined mass
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Withdrawn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
EP00964077A
Other languages
German (de)
English (en)
Inventor
Peter Manfred Roth
Anselm Schmitt
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.)
Siemens Axiva GmbH and Co KG
Original Assignee
Siemens Axiva GmbH and Co KG
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 Siemens Axiva GmbH and Co KG filed Critical Siemens Axiva GmbH and Co KG
Publication of EP1214281A1 publication Critical patent/EP1214281A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • 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
    • C07C41/09—Preparation of ethers by dehydration of compounds containing hydroxy groups
    • 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
    • C07C41/34—Separation; Purification; Stabilisation; Use of additives
    • 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
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
    • B01J2219/00085—Plates; Jackets; Cylinders
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Definitions

  • the invention relates to a process for the continuous production of dimethyl ether by catalytic dehydration of methanol in a reactor at a temperature in the range from 150 ° C to 450 ° C and a pressure of
  • the invention further relates to an apparatus for performing the method.
  • the dehydration product is usually introduced into a column above the bottom.
  • the dimethyl ether is drawn off above the feed point, while a mixture of methanol and water is obtained in the bottom, which is usually worked up in a second column.
  • This process is associated with high energy and investment costs, so that from the point of view of
  • the invention was therefore based on the object of providing an improved, more cost-effective and alternative method.
  • the invention therefore relates to a process for the continuous production of dimethyl ether by catalytic dehydration of methanol in one
  • Reactor at a temperature in the range of 150 ° C to 450 ° C and a pressure of 1 to 40 bar absolute and cleaning of the dehydration product by partial condensation and / or absorption characterized in that the dehydration product after the reactor in a combined substance and Heat transfer apparatus is initiated and here the cooling of the
  • Dehydration product to a temperature below its dew point is carried out that the condensate is countercurrent to the rising gas phase in the combined mass and heat transfer apparatus, that at one end of the combined mass and heat transfer apparatus, the purified, gaseous dimethyl ether is withdrawn, that at the other end of the combined
  • Mass and heat transfer apparatus the resulting liquid condensate, containing dimethyl ether, methanol and water, is drawn off and that, in countercurrent to the rising gas phase, a washing liquid is added to the upper end of the combined mass and heat transfer apparatus in the combined mass and heat transfer apparatus.
  • the invention also relates to an apparatus for performing this method.
  • the combined mass and heat transfer apparatus is preferably designed so that the condensate resulting from indirect cooling in
  • the dimethyl ether thus obtained is always removed in gaseous form from the combined mass and heat transfer apparatus. It is then introduced or liquefied in a further process step or fed to a membrane system or distillation or adsorption (fine cleaning). That in the combined fabric and
  • the condensate obtained from the heat transfer apparatus also contains excess methanol from the reaction and dissolved dimethyl ether.
  • This condensate is worked up by distillation - the dissolved dimethyl ether can be recycled from here together with methanol into the reaction or, for example, burned, or it can be in another
  • Separation stage e.g. B. a two - ion system, pure dimethyl ether can be removed (methanol analogous to above).
  • wash water can be introduced into the combined mass and heat transfer apparatus, which preferably absorbs methanol, but also to a lesser extent, dimethyl ether from the gaseous reaction mixture. It can be fresh water or the above mentioned. Distillation water can be used for this.
  • the described method proves to be considerably more economical than the previously known methods. It is particularly suitable if both a high and a lower dimethyl ether purity are to be produced in parallel. To obtain a comparatively low dimethyl ether purity, only one distillation column compared to at least 2 columns according to the prior art is required. With the new process, the energy requirement is also significantly lower if the dimethyl ether obtained at the upper end of the combined mass and heat transfer apparatus is distilled to extremely high purity in a second column. The new In addition, the method enables an extremely compact and integrated construction, which according to the state of the art would not be possible or could only be implemented with disproportionately high expenditure.
  • Wise is not intended to do this.
  • FIG. 1 A flow diagram of a preferred embodiment of the method according to the invention
  • Fig. 2 a preferred embodiment of a device for performing the
  • methanol is passed through a preheater (W101), into an evaporator (W100) and evaporated here.
  • the methanol vapor is fed into the reactor (R100) via a heater (W110).
  • the catalytic dehydration of the methanol takes place on a suitable catalyst to dimethyl ether and water.
  • the gaseous reaction mixture consisting of the dimethyl ether, the water of reaction, methanol and impurities is then fed to a combined mass and heat transfer apparatus (W140).
  • This combined mass and heat transfer apparatus is preferably designed so that the condensate formed as a result of the external cooling can be conducted in countercurrent to the gas phase.
  • this is a preferably vertical tube heat exchanger, in which the reaction gas is introduced into the tubes from below, the condensate that forms flows downwards in the tubes as a film and over a collecting or liquid collecting base (x in Fig 2) withdrawn and the gaseous and purified dimethyl ether (stream 210) is withdrawn at the upper end of the tubes.
  • This dimethyl ether can be fed to a distillation column to produce a particularly high purity (B30).
  • a suitable cooling liquid is passed around the pipes (jacket space), which cools both the hot reaction gases by indirect heat transfer and the partial ones
  • wash water can be applied to the upper tube sheet, for example as a falling film.
  • the upper tube plate is equipped with a liquid distribution (y), similarly to falling film evaporators.
  • Condensate is fed to a distillation unit (B23 / B24).
  • the condensate is separated either in two stages in high-purity dimethyl ether (stream 227), a methano fraction (stream 231) and water (stream 229) or the dimethyl ether is recycled to the process together with the methanol in one stage as (stream 206) and / or alternatively discharged as (stream 233).
  • the water is removed from the process (stream 230). In a special mode of operation, this water can also be partly returned as washing liquid (stream 237) to the combined mass and heat transfer apparatus (W 140).
  • W140 combined mass and heat transfer apparatus
  • these are in particular tubular heat exchangers or also suitable plate heat exchangers or spiral heat exchangers.
  • this apparatus can also be designed in several stages or, in addition, with suitable mass transfer devices such as packing,
  • the described method can also be carried out in an apparatus according to the scheme or arrangement in FIG. 2.
  • the methanol evaporator (W100) is arranged on the "bottom" of the system.
  • a so-called Robert evaporator can be used for this - a tubular heat exchanger with an internal circulation pipe.
  • the methanol vapor generated here rises and reaches a superheater (W110), which is also designed as a tube apparatus.
  • W110 superheater
  • the tube reactor (R100) is arranged directly above it, and the catalyst-filled tubes flow through it from bottom to top.
  • the combined mass and heat transfer device (W140) is arranged directly above this, the one with one
  • This gas mixture was cooled or partially condensed in the combined mass and heat transfer apparatus at 4 bara to 40 ° C. and at the same time with
  • the condensate including wash water in the combined mass and heat transfer apparatus had a temperature of 100 ° C and the following composition:
  • the condensate can be worked up, for example, in a column system.

Landscapes

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

Abstract

La présente invention concerne un procédé de préparation en continu de diméthyl éther par déshydratation catalytique de méthanol dans un réacteur à une température comprise entre 150 DEG C et 450 DEG C et une pression comprise entre 1 et 40 bar absolu, et purification du produit de déshydratation par absorption et/ou condensation partielle. L'invention se caractérise en ce que le produit de déshydratation, à la sortie du réacteur, est introduit dans un appareil de transfert de chaleur et de masse combiné et y est refroidi jusqu'à une température inférieure à son point de rosée.
EP00964077A 1999-09-09 2000-08-31 Procede de preparation de dimethyl ether Withdrawn EP1214281A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19943219A DE19943219A1 (de) 1999-09-09 1999-09-09 Verfahren zur Herstellung von Dimethylether
DE19943219 1999-09-09
PCT/EP2000/008506 WO2001017937A1 (fr) 1999-09-09 2000-08-31 Procede de preparation de dimethyl ether

Publications (1)

Publication Number Publication Date
EP1214281A1 true EP1214281A1 (fr) 2002-06-19

Family

ID=7921424

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00964077A Withdrawn EP1214281A1 (fr) 1999-09-09 2000-08-31 Procede de preparation de dimethyl ether

Country Status (3)

Country Link
EP (1) EP1214281A1 (fr)
DE (1) DE19943219A1 (fr)
WO (1) WO2001017937A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6924399B2 (en) * 2001-12-28 2005-08-02 Mitsubishi Heavy Industries, Ltd. Method of manufacturing dimethyl ether
CN1304369C (zh) * 2004-10-12 2007-03-14 山东新华万博化工有限公司 硫酸二甲酯的制备工艺
CN102093172B (zh) * 2010-12-13 2014-01-15 云南瑞升烟草技术（集团）有限公司 一种应用于烟草制品处理的无异味高纯二甲醚的制备方法及设备
TWI652257B (zh) * 2014-01-07 2019-03-01 德商林德股份有限公司 藉由分離技術處理二甲醚反應器之產物流的方法
EP3689440B1 (fr) * 2019-02-01 2023-11-29 Polymetrix AG Procédé et dispositif de nettoyage de gaz de processus mis en circulation provenant des traitements des matériaux granulés
CN109748827B (zh) * 2019-02-03 2021-09-14 山东凯瑞英材料科技有限公司 连续合成硫酸二甲酯的工艺方法

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59199648A (ja) * 1983-04-27 1984-11-12 Mitsubishi Chem Ind Ltd ジメチルエ−テルの製造法
AU603070B2 (en) * 1986-11-18 1990-11-08 Rwe-Dea Aktiengesellschaft Fur Mineraloel Und Chemie Process for the purification of dimethylether
DE3876790D1 (de) * 1988-05-04 1993-01-28 Rwe Dea Ag Verbessertes verfahren zur herstellung von reinem dimethylether.
DE69016521T2 (de) * 1989-07-03 1995-06-01 Chemical Res & Licensin Verfahren zur Herstellung von Dialkylethern.
DE4132993A1 (de) * 1991-10-04 1993-04-08 Rwe Dea Ag Verfahren zur herstellung von dimethylether
DE4208028A1 (de) * 1992-03-13 1993-09-16 Leuna Werke Ag Verfahren zur herstellung von hochreinem dimethylether

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO0117937A1 *

Also Published As

Publication number Publication date
DE19943219A1 (de) 2001-03-15
WO2001017937A1 (fr) 2001-03-15

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