WO2003040259A2 - Körper für die separation einer in einem gasgemisch enthaltenen komponente - Google Patents

Körper für die separation einer in einem gasgemisch enthaltenen komponente Download PDF

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Publication number
WO2003040259A2
WO2003040259A2 PCT/DE2002/004158 DE0204158W WO03040259A2 WO 2003040259 A2 WO2003040259 A2 WO 2003040259A2 DE 0204158 W DE0204158 W DE 0204158W WO 03040259 A2 WO03040259 A2 WO 03040259A2
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WIPO (PCT)
Prior art keywords
bodies
separation
bed
shell
gas mixture
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
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PCT/DE2002/004158
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German (de)
English (en)
French (fr)
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WO2003040259A3 (de
Inventor
Frank Bretschneider
Constant Van Lookeren
Manfred Nebelung
Hagen Klemm
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IPC Process Center GmbH and Co KG
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Original Assignee
IPC Process Center GmbH and Co KG
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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Application filed by IPC Process Center GmbH and Co KG, Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV filed Critical IPC Process Center GmbH and Co KG
Priority to US10/494,910 priority Critical patent/US7014689B2/en
Priority to JP2003542299A priority patent/JP2005508251A/ja
Priority to EP02796494A priority patent/EP1441848A2/de
Priority to AU2002361926A priority patent/AU2002361926A1/en
Publication of WO2003040259A2 publication Critical patent/WO2003040259A2/de
Publication of WO2003040259A3 publication Critical patent/WO2003040259A3/de
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • 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
    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
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    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3291—Characterised by the shape of the carrier, the coating or the obtained coated product
    • B01J20/3293—Coatings on a core, the core being particle or fiber shaped, e.g. encapsulated particles, coated fibers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D—SEPARATION
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    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/408—Alkaline earth metal or magnesium compounds of barium
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2253/104—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01D2253/106—Silica or silicates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
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    • B01D2257/10—Single element gases other than halogens
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01D53/02—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 by adsorption, e.g. preparative gas chromatography
    • B01D53/04—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 by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/047—Pressure swing adsorption
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S55/00—Gas separation
    • Y10S55/05—Methods of making filter

Definitions

  • the invention relates to bodies for the separation of a component contained in a gas mixture.
  • the gas mixtures can be, for example, raw gases containing hydrocarbons, such as natural gas, or also exhaust gas. Harmful components contained in such gas mixtures, e.g. Sulfur can also be removed in the form of compounds in order to make the gas mixture free of negative properties during further use and processing or to release gas free of harmful components to the environment.
  • nitrogen or nitrogen oxides can also be separated in order to improve their suitability for combustion or to release almost nitrogen oxide-free exhaust gases into the environment.
  • phosphorus, halogens or their compounds can also be separated.
  • Such gas mixtures are cleaned using solid substances, the separation being carried out by sorption.
  • the surface of the material used can be used to ensure a higher separation capacity.
  • an increase in surface area can be achieved by the geometric design and in particular the specific surface of a fabric by the porosity.
  • suitable materials mainly chemical compounds, have been used as granules in a wide variety of grain sizes and a favorable porosity, often set by appropriate sintering.
  • the gas mixture to be cleaned or freed from a component is then passed through a fixed bed formed from a bed of the granulate and the respective component to be separated is sorbed.
  • the bed forms a throttle point for the gas flow, so that a dynamic pressure which is influenced by the grain size and the dimensioning of the bed is recorded on the inlet side.
  • This requires an increased output for gas production.
  • abrasion occurs, which impedes the gas flow and this effect can severely limit the service life of a bed, so that an exchange in relatively short time intervals is necessary.
  • each substance suitable for separation has a limited separation capacity, essentially influenced by the usable surface and mass. and a saturation range, so that full use cannot usually take place.
  • bodies should be used for the separation selected components from gas mixtures are used, the active area for the separation is designed in the form of a porous shell.
  • This shell can enclose at least one cavity or at least one core that is not active for the separation on all sides, so that a closed body is formed.
  • the term pores should not include the individual pores.
  • This body is particularly preferably spherically curved and can also be designed as a hollow sphere.
  • a spherical shape is not only advantageous because of the spherical geometry with a large surface area, but also offers favorable fluidic conditions when a gas mixture is passed through a bed formed from such bodies during the separation, since a correspondingly reduced dynamic pressure is reached at the inlet side of such a bed can be.
  • the bodies according to the invention can optionally also be hollow cylinders.
  • the shell shape with a correspondingly limited thickness up to a maximum of 5 mm, preferably less than 2 mm, can also ensure an almost constant separation performance over a large usable period, this being guaranteed at least up to the vicinity of the saturation limit. This can improve the quality of separation, and consequently that of
  • the degree of purity of the treated gas was kept constant and also reduce operating costs.
  • the bodies according to the invention can be used for the separation at least up to a load which is close to the saturation limit without the gas purity being significantly influenced.
  • Spherical bodies can be produced in a manner known per se.
  • a powder which essentially consists of a substance suitable for the respective component to be separated, is applied as a dispersion / suspension to a spherical core and, after drying, is subjected to sintering.
  • the core can consist of a material which is inactive for the separation, but the thermal behavior of this material should be taken into account, taking into account the thermal expansion and shrinkage during sintering, in order to avoid cracking of the shell as far as possible.
  • the core can also be made of an organic material, e.g. Pre-expanded polystyrene exist, which can be safely expelled at temperatures below 700 ° C, so that in these cases the bodies are present as hollow spheres.
  • the ratio of the outside diameter to the shell thickness should be in the range from 2 to 1 to 10 to 1, the smaller ratios with small outside diameters of the bodies being preferred. If possible, the shell thickness should not be greater than 3 mm, whereby an upper limit of 8 mm should not be exceeded.
  • the mechanical strength and porosity of the shell can be influenced by the powder used, in particular its grain size, possibly with additives that remain in the shell and the sintering conditions. the.
  • the sintering should be carried out in such a way that just sufficient mechanical strength with the highest possible porosity is achieved.
  • outer dimensions (outer diameter) and the mass of the body according to the invention can be varied taking into account the respective application, the porosity being kept constant.
  • sintering aids for example SiO 2
  • the proportion of SiO 2 should be less than 10% by mass, preferably less than 5% by mass.
  • the shell can be made from different materials. It can be formed from metal oxides or metal oxide mixtures, with oxides of II-valent metals being preferred. For example, for the separation of sulfur in the form of hydrogen sulfide with oxides of II-valent metals (e.g. Cu, Fe, Co, Ni, Zn) can be separated from a gas mixture, such as natural gas, by chemical conversion.
  • a gas mixture such as natural gas
  • ZnO react with H 2 S to ZnS and
  • ZnS is chemically more stable than H 2 S and can be held in solid form on the body.
  • ZnS can react with H 2 O to form sulfuric acid, ZnO again forming in the shell at the same time, which can be used for a new separation.
  • bodies made of Al 2 0 3 can be used as a catalyst.
  • the Al 2 0 3 can also form the shell of such a body.
  • the so-called Claus process can then be carried out with these catalysts and the ZnO bodies, in which S0 2 and 2H 2 S react catalytically to 3S and 2H 2 0.
  • Certain zeolites which are also known per se, can also be used for the separation of sulfur compounds.
  • Zeolites as they are referred to, for example, in US Pat. No. 6,197,092, can also be used as so-called molecular sieves for the separation of nitrogen, this advantageously being possible by means of a pressure swing adsorption process (PSA) which is also mentioned there ,
  • PSA pressure swing adsorption process
  • Phosphorus, halogens or their compounds can also be separated using such molecular sieves.
  • BaC0 3 can be used as the shell material, which reacts with N0 2 to form BaO. Regeneration is also possible here.
  • the BaO formed is heated (T approx. 450 ° C.) and BaC0 3 can be formed again with carbon compounds (for example C0 2 ).
  • the bodies according to the invention can also be used for gas drying and e.g. Extract water or water vapor from a gas / gas mixture.
  • the bodies according to the invention can be used in devices in which, in containers through which a gas mixture for the separation is passed, at least one body is formed from a bed of so-called fixed beds.
  • the bodies can also form a fluidized bed or fluid bed, in particular because of their increased strength with the same porosity, the gas mixture being used with an increased volume flow.
  • Such a bed can also be formed by bodies moved as a result of gravitational or mechanical forces. The bodies can be continuously fed to the area of such a bed that is active for the separation, removed from the bed with the component loaded with the component to be separated, fed to a regeneration and returned to the circuit.
  • the gas mixture flows through this bed for separation and a component is held there by chemical and / or physical effects, so that gas emerging from this bed or a cascade of several such beds is largely free of this component.
  • regeneration is necessary. This can be achieved by supplying heat, ie heating the beds or the entire container. In particular when ZnS is formed, the regeneration can also be carried out by adding water. Water vapor or fluid containing water vapor can be passed through the bed in order to trigger the regression of ZnS to ZnO.
  • Switching from one container to the other can be time-controlled but also regulated, in the latter case the concentration of the corresponding component in the emerging gas stream being determined and when a limit value is exceeded, the switching of the gas flow to another container is initiated.
  • Form beds can have at least approximately the same outside dimensions / outside diameter in each bed.
  • Bodies with different dimensions can be used in several beds forming a cascade and there is the possibility of using bodies with different outside dimensions / outside diameters in one bed.
  • the flow conditions of the gas mixture should be influenced in such a way that the pressure drop is kept as small as possible and nevertheless there is sufficient contact or dwell time in the beds for the separation.
  • the bodies according to the invention should be present in the beds as a loose bed, without the use of binders.
  • a catalytically active substance can also advantageously be additionally present in the beds, with which the separation is facilitated, made possible and, if necessary, the required reaction time or energy supplied can be reduced.
  • Such a catalytically active substance for example platinum
  • nitrogen monoxide can be catalytic oxidized to nitrogen dioxide and nitrogen dioxide can be separated from an exhaust gas by chemical reaction with BaC03.
  • Figure 1 is a diagram of the time course of the
  • Solid spheres were produced as a comparative example and hollow spheres as bodies according to the invention.
  • the specific breaking strength of the hollow bodies according to the invention was 2.9 MPa, whereas the solid spheres only reached 1.99 MPa.
  • the specific surface of the comparison body was 41.7 m 2 / g and that of the body according to the invention was 48.6 m 2 / g.
  • the temperature was kept constant at 400 ° C.
  • the load was measured in mg over time.
  • the increase in the mass increase representing the separation of hydrogen sulfide from the gas mixture turns out to be significantly smaller, at least after reaching about 50% of the maximum separation capacity, that is to say before the saturation limit has been reached for the full comparison bodies.
  • the result of this is that, after a certain time, significantly less hydrogen sulfide can be separated and chemically converted into ZnS than is possible with the hollow spherical bodies according to the invention.
  • a total mass of 332 g / l of hydrogen sulfide could be separated in both investigations.
  • this mass could already be reached after 38 minutes, whereas the comparison bodies required 57 minutes, which also demonstrates an increased separation effect, that is to say not only faster but also a larger amount of hydrogen sulfide can be separated from a gas mixture and a higher purity of a gas mixture treated in this way can be recorded.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Gas Separation By Absorption (AREA)
PCT/DE2002/004158 2001-11-08 2002-11-06 Körper für die separation einer in einem gasgemisch enthaltenen komponente Ceased WO2003040259A2 (de)

Priority Applications (4)

Application Number Priority Date Filing Date Title
US10/494,910 US7014689B2 (en) 2001-11-08 2002-11-06 Body for isolating a constituent contained in a gas mixture
JP2003542299A JP2005508251A (ja) 2001-11-08 2002-11-06 ガス混合物に含まれる成分を分離するための多孔性中空ボディ
EP02796494A EP1441848A2 (de) 2001-11-08 2002-11-06 Körper für die separation einer in einem gasgemisch enthaltenen komponente
AU2002361926A AU2002361926A1 (en) 2001-11-08 2002-11-06 Body for isolating a constituent contained in a gas mixture

Applications Claiming Priority (2)

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DE10155643.8 2001-11-08
DE10155643A DE10155643A1 (de) 2001-11-08 2001-11-08 Körper für die Separation einer in einem Gasgemisch enthaltenen Komponente

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WO2003040259A2 true WO2003040259A2 (de) 2003-05-15
WO2003040259A3 WO2003040259A3 (de) 2003-07-24

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DE (1) DE10155643A1 (https=)
WO (1) WO2003040259A2 (https=)

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US7137249B2 (en) 2004-08-12 2006-11-21 Ford Global Technologies, Llc Thermally stable lean nox trap
US7622095B2 (en) 2004-08-12 2009-11-24 Ford Global Technologies, Llc Catalyst composition for use in a lean NOx trap and method of using
US7749474B2 (en) 2004-08-12 2010-07-06 Ford Global Technologies, Llc Catalyst composition for use in a lean NOx trap and method of using
US7811961B2 (en) 2004-08-12 2010-10-12 Ford Global Technologies, Llc Methods and formulations for enhancing NH3 adsorption capacity of selective catalytic reduction catalysts

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US7137249B2 (en) 2004-08-12 2006-11-21 Ford Global Technologies, Llc Thermally stable lean nox trap
US7622095B2 (en) 2004-08-12 2009-11-24 Ford Global Technologies, Llc Catalyst composition for use in a lean NOx trap and method of using
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US7811961B2 (en) 2004-08-12 2010-10-12 Ford Global Technologies, Llc Methods and formulations for enhancing NH3 adsorption capacity of selective catalytic reduction catalysts
US8138114B2 (en) 2004-08-12 2012-03-20 Ford Motor Company Methods and formulations for enhancing NH3 adsorption capacity of selective catalytic reduction catalysts

Also Published As

Publication number Publication date
WO2003040259A3 (de) 2003-07-24
EP1479436A3 (de) 2004-12-29
EP1441848A2 (de) 2004-08-04
US20050072305A1 (en) 2005-04-07
EP1479436A2 (de) 2004-11-24
US7014689B2 (en) 2006-03-21
DE10155643A1 (de) 2003-05-28
AU2002361926A1 (en) 2003-05-19
JP2005508251A (ja) 2005-03-31

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