EP1590295A1 - Procede de desulfuration de monoxyde de carbone gazeux - Google Patents

Procede de desulfuration de monoxyde de carbone gazeux

Info

Publication number
EP1590295A1
EP1590295A1 EP04700125A EP04700125A EP1590295A1 EP 1590295 A1 EP1590295 A1 EP 1590295A1 EP 04700125 A EP04700125 A EP 04700125A EP 04700125 A EP04700125 A EP 04700125A EP 1590295 A1 EP1590295 A1 EP 1590295A1
Authority
EP
European Patent Office
Prior art keywords
gas
sulfur compounds
content
less
sulfur
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Withdrawn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
EP04700125A
Other languages
German (de)
English (en)
Inventor
Werner Breuer
Karl-Heinz Köhler
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.)
Covestro Deutschland AG
Original Assignee
Bayer MaterialScience AG
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 Bayer MaterialScience AG filed Critical Bayer MaterialScience AG
Publication of EP1590295A1 publication Critical patent/EP1590295A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B01D53/508—Sulfur oxides by treating the gases with solids
    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/40—Carbon monoxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/80—Phosgene
    • 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
    • Y02P20/141—Feedstock

Definitions

  • EP-A 1180544 describes in column 6, lines 16-40, the use of tri-iron-tetra-oxide at 400 ° C for the absorption of hydrogen sulfide on the contact in the form of iron sulfide; in a downstream stage, residual amounts of hydrogen sulfide are bound to zinc oxide as zinc sulfide.
  • EP-A 722 774 describes in the examples the use of iron (LTI) oxide in combination with molybdenum oxide on an alumina support at at least 350 ° C for the absorption of hydrogen sulfide as sulfide on the contact.
  • This CO gas which contains predominantly hydrogen sulfide as a sulfur component, is then continuously in a chemical absorption stage over
  • the erfmdungshiele method is characterized by high efficiency, efficiency and availability, which is given by the following factors:
  • the used in the inventive method, loaded with sulfur compounds CO gas should be largely dust-free, before the first stage of
  • Binder for increasing the mechanical strength fabrics such as e.g. Cement, lime or gypsum.
  • loosening agents are used, which increase the gas diffusion into the material, so that in addition to the surface of the granular, porous masses and the deeper layers participate in the chemical absorption.
  • a loosening agent e.g. Sawdust or sawdust in question (see DE-A 28 45 725, DE-A 20 06 758), wherein care must be taken that these loosening agents contain no acids which can react with the binders in the masses.
  • the grid baskets are separated by the bottom and / or cover plates so that each grid basket forms its own separate gas space, but preferably all grid baskets are coupled to common inlet and outlet lines.
  • Preferably used mesh baskets are flown by the CO gas to be desulfurized from above, so that the CO gas flows through a 120 to 180 cm high, preferably about 150 cm high Biogasmasse bed and exits through a located in the bottom region of the basket horizontally arranged grid plate , Between this grid plate and the bottom plate of the basket, the exiting CO gas is deflected to a centrally disposed discharge line, via which it leaves the Abso ⁇ tionsturm.
  • the desulfurized CO gas is then fed to the activated carbon adsorption stage.
  • the temperature in the heat exchanger is adjusted so that the CO gas inlet temperature in this stage is less than 50 ° C, preferably not more than 35 ° C.
  • the CO gas Before entering the CO gas in the activated carbon adsorption towers is the CO gas but not mixed with an amount of at least 150 mg / Nm 3, more homogeneous than 310 mg / Nm 3 of gaseous ammonia.
  • the oxygen content in the CO gas which is in excess of the oxidation reaction in the preceding chemical absorption stage, should not be more than 0.15% by volume.
  • the activated carbon adsorption towers are available in multiple places and can flow through both in series and in parallel, depending on the operational requirements become.
  • the activated carbon towers are fixed-bed reactors and designed as cylindrical apparatus with a sieve bottom; they contain a continuous package of granular activated carbon, which flows through from top to bottom. Suitable granular activated carbons have a sufficient strength to avoid unacceptably high Feinabriebmengen, which may arise in particular during regeneration operations.
  • the particle size distribution should be chosen so that the pressure drop of the CO gas in the entire adsorption stage is not more than 0.4 bar.
  • Activated carbons with a specific surface area of 1,000 to 1,200 m 2 / g and a pore volume with pore sizes below 20 nm are from 0.5 to 0.7 ml / g, eg. the activated carbon "D 47-4" of company "VFT".
  • an active column adsorption tower If an active column adsorption tower has reached the sulfur loading limit, it is separated from the composite with the remaining towers and regenerated separately.
  • the CO gas leaves the plant with a content of organic and inorganic sulfur compounds of less than 5 mg / Nm 3 , preferably less than 2 mg / Nm 3 . This corresponds to an adsorption rate of the sulfur compounds of more than 95%.
  • the thus purified CO gas is brought to a pressure of 3.5 bar, and in a subsequent classical drying step according to the prior art by precondensation in a brine heat exchanger at a temperature of 3 ° C and by subsequent drying in silica gel-filled Towers dewatered to a residual content of less than 10 ppm.
  • the entire process is continuously monitored analytically at various points in the entire process in order to be able to detect and respond to limit value violations of substance concentrations in CO gas with sufficient speed.
  • the following substances in the CO gas are continuously monitored by so-called online analytical methods:
  • Ammonia in the CO gas is determined photometrically using the "BINOS” device from Endress and Hauser Oxygen in the CO gas is determined by a paramagnetic measurement method with the "OXLMAT” device from Siemens.
  • sampling points in the input and output stream of the CO gas are attached to the process sections to be monitored in order to assess the efficiency of a part of the process. By periodic decommissioning of individual turbine towers due to capacity creation and regeneration required, the sampling points are allocated accordingly; an exception are the conversion towers, as there is no regular regeneration required.
  • the analytical data are registered and recorded in evaluable form. If predetermined limit values are exceeded, alarms are issued, in critical
  • BASF D 10-10) filled towers of the conversion stage Before entering the conversion towers, an amount of 100 kg / h of steam is continuously added to the CO gas.
  • the CO gas is at this stage at a pressure of 2.8, bar.
  • the CO gas leaving the conversion stage is cooled via cross-flow heat exchangers, in which part of the heat of the escaping gas is released to the gas entering the conversion stage, via the water heat exchanger to about 30 ° C.
  • the continuous analytical examination of the exiting CO gas by so-called "on-line gas chromatography” gives for the content of organic sulfur compounds 50 mg / Nm 3 and for the content of inorganic sulfur compounds 3,450 mg / Nm 3 , which corresponds to a conversion rate of the organic sulfur compounds of 98 , 5% corresponds.
  • the CO raw gas generation source, the apparatus used, and the physical conditions pressure and temperature are identical to Example 1.
  • the sulfur content of the CO gas is significantly increased compared to Example 1, the gas flow rate is reduced.
  • the CO gas leaving the conversion stage has, after continuous analytical examination, a content of organic sulfur compounds of 100 mg / Nm 3 and an inorganic sulfur compound content of 5,900 mg / Nm 3 , which corresponds to a conversion rate of the organic sulfur compounds of 98.3%.

Abstract

L'invention concerne un procédé de fabrication de monoxyde de carbone gazeux essentiellement libre de composés soufre, un procédé de désulfuration de monoxyde de carbone gazeux contenant du soufre, ainsi que l'utilisation de ce gaz dans des synthèses chimiques, par ex. la synthèse de phosgène à partir de monoxyde de carbone et de chlore.
EP04700125A 2003-01-16 2004-01-05 Procede de desulfuration de monoxyde de carbone gazeux Withdrawn EP1590295A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE10301434A DE10301434A1 (de) 2003-01-16 2003-01-16 Verfahren zur CO-Gas-Entschwefelung
DE10301434 2003-01-16
PCT/EP2004/000018 WO2004063094A1 (fr) 2003-01-16 2004-01-05 Procede de desulfuration de monoxyde de carbone gazeux

Publications (1)

Publication Number Publication Date
EP1590295A1 true EP1590295A1 (fr) 2005-11-02

Family

ID=32602604

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04700125A Withdrawn EP1590295A1 (fr) 2003-01-16 2004-01-05 Procede de desulfuration de monoxyde de carbone gazeux

Country Status (8)

Country Link
US (1) US6942842B2 (fr)
EP (1) EP1590295A1 (fr)
JP (1) JP2006515263A (fr)
CN (1) CN100404414C (fr)
DE (1) DE10301434A1 (fr)
HK (1) HK1088885A1 (fr)
TW (1) TW200508150A (fr)
WO (1) WO2004063094A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2067742A1 (fr) 2007-11-29 2009-06-10 Bayer MaterialScience AG Procédé destiné à la fabrication de phosgènes ayant une émission de CO réduite

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DE10348116B4 (de) * 2003-10-16 2015-02-19 Bayer Intellectual Property Gmbh CO-Generator und Verfahren zur Herstellung von kohlenmonoxidhaltigem Gas durch Umsetzung eines kohlenstoffhaltigen Brennmaterials
US7427385B2 (en) * 2004-12-17 2008-09-23 Exxonmobil Research And Engineering Company Systems and processes for reducing the sulfur content of hydrocarbon streams
JP4785515B2 (ja) * 2005-12-08 2011-10-05 住友化学株式会社 塩素の製造方法
US20100303710A1 (en) * 2005-12-08 2010-12-02 Sumitomo Chemical Company, Limited Process for producing chlorine
DE102006002157A1 (de) * 2006-01-17 2007-07-19 Bayer Materialscience Ag Verfahren zur Herstellung heller Isocyanate
CN100387692C (zh) * 2006-03-30 2008-05-14 湖北省化学研究院 制取高纯一氧化碳气体的低、常温脱除有机硫工艺
DE102007020444A1 (de) * 2007-04-27 2008-11-06 Bayer Materialscience Ag Verfahren zur Oxidation eines Chlorwasserstoffenthaltenden Gasgemisches
CN101584962B (zh) * 2008-05-23 2012-07-18 北京三聚环保新材料股份有限公司 一种高强度羟基氧化铁脱硫剂及其制备方法
JP5336828B2 (ja) * 2008-12-02 2013-11-06 三井化学株式会社 塩化カルボニルの製造方法および製造装置、ならびに、ポリイソシアネートの製造方法および製造装置
CN101913845A (zh) * 2010-08-04 2010-12-15 姜辉 一种用于湿法气体脱硫的高含铁陶瓷填料
JP5667253B2 (ja) * 2013-08-01 2015-02-12 三井化学株式会社 塩化カルボニルの製造装置およびポリイソシアネートの製造装置
CN112423860A (zh) * 2018-07-17 2021-02-26 Sabic环球技术有限责任公司 在环境温度从富一氧化碳气流中去除硫化物的方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2067742A1 (fr) 2007-11-29 2009-06-10 Bayer MaterialScience AG Procédé destiné à la fabrication de phosgènes ayant une émission de CO réduite
DE102007057462A1 (de) 2007-11-29 2009-06-10 Bayer Materialscience Ag Verfahren zur Herstellung von Phosgen mit reduzierter CO-Emission

Also Published As

Publication number Publication date
US20040141901A1 (en) 2004-07-22
TW200508150A (en) 2005-03-01
CN100404414C (zh) 2008-07-23
DE10301434A1 (de) 2004-07-29
US6942842B2 (en) 2005-09-13
JP2006515263A (ja) 2006-05-25
HK1088885A1 (en) 2006-11-17
WO2004063094A1 (fr) 2004-07-29
CN1738768A (zh) 2006-02-22

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