EP1534414B1 - Procede et dispositif d'injection de co2 diphasique dans un milieu gazeux en transfert - Google Patents

Procede et dispositif d'injection de co2 diphasique dans un milieu gazeux en transfert Download PDF

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Publication number
EP1534414B1
EP1534414B1 EP03763931A EP03763931A EP1534414B1 EP 1534414 B1 EP1534414 B1 EP 1534414B1 EP 03763931 A EP03763931 A EP 03763931A EP 03763931 A EP03763931 A EP 03763931A EP 1534414 B1 EP1534414 B1 EP 1534414B1
Authority
EP
European Patent Office
Prior art keywords
carbon dioxide
gas
gaseous medium
injector
phase
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.)
Expired - Lifetime
Application number
EP03763931A
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German (de)
English (en)
French (fr)
Other versions
EP1534414A2 (fr
Inventor
Dominique Bras
José Buil
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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 Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP1534414A2 publication Critical patent/EP1534414A2/fr
Application granted granted Critical
Publication of EP1534414B1 publication Critical patent/EP1534414B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/09—Mixing systems, i.e. flow charts or diagrams for components having more than two different of undetermined agglomeration states, e.g. supercritical states
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/10—Mixing gases with gases
    • B01F23/12—Mixing gases with gases with vaporisation of a liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
    • B01F23/30—Mixing gases with solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/30—Injector mixers
    • B01F25/31—Injector mixers in conduits or tubes through which the main component flows
    • B01F25/313—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced in the centre of the conduit
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/834—Mixing in several steps, e.g. successive steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/911—Axial flow
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F2025/91—Direction of flow or arrangement of feed and discharge openings
    • B01F2025/918—Counter current flow, i.e. flows moving in opposite direction and colliding
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/0318—Processes
    • Y10T137/0324—With control of flow by a condition or characteristic of a fluid
    • Y10T137/0329—Mixing of plural fluids of diverse characteristics or conditions
    • 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
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/8593—Systems
    • Y10T137/87571—Multiple inlet with single outlet
    • Y10T137/87652—With means to promote mixing or combining of plural fluids

Definitions

  • the invention relates to a method and a device for injecting two- phase CO 2 , "solid gas” into a transfer gas medium.
  • CO 2 is used in many industrial applications; Carbonation, pH regulation and the neutralization of Basque agents are examples of others.
  • the carbon dioxide can be injected into a liquid medium or a gaseous medium.
  • the CO 2 is injected in gaseous form, or liquid depending on the case.
  • CO 2 in solid form, or dry ice for cleaning surfaces.
  • US 4,747,421 discloses the use of solid CO 2 in the field of the semiconductor industry for the removal of a photoresist film on the surface of a substrate.
  • EP 0 631 846 discloses an apparatus for producing an aerosol for cleaning the interior surfaces of a tool chamber.
  • EP 0 288 263 discloses an apparatus for removing small particles from the surface of a substrate using a mixture of solid and gaseous carbon dioxide.
  • US 4,389,820 discloses a machine for generating an accelerated sublimated particle flux for surface etching.
  • the use of CO 2 avoids surface contamination as well as atmospheric contamination.
  • FR 2 198 778 discloses a method and apparatus for the preparation of foundry molds, wherein carbon dioxide gas is used for the delivery of gaseous components in a catalytic amount, both in the gasification of the mixture of liquid chemical components and in the adjustment of the quantities of components to be added.
  • WO 02/24316 A discloses a cooling device using an inverse carnot type cycle to generate an aerosol consisting of solid CO2 particles for cleaning microelectronic surfaces.
  • US 5,616,067 describes surface cleaning equipment intended in particular for the printing and electronics industries, using abrasive CO2 particles injected together with pressurized air.
  • An object of the present invention is to provide a solution to the problem of carbon dioxide injection in particular in large quantities, in enclosures containing a gaseous medium reactive or not, in transit under pressure.
  • Another object is to propose an injection device capable of implementing this method.
  • the injected carbon dioxide is in the form "gas + solid", the injection is done directly in the gaseous medium to be treated, through a wall of the enclosure which closes the medium to be treated.
  • the enclosure may be for example a pipe or pipe present in a circuit.
  • the transformation of liquid carbon dioxide into two-phase carbon dioxide involves a direct expansion device known as cryogenic expansion.
  • the device, of the variable flow valve type firstly restricts the flow of the fluid, then an increase in the flow diameter has the effect of relieving the gas causing a loss of pressure so that the pressure in output of the device corresponds to that of the triple point of CO 2 .
  • Liquid CO 2 is transformed into a mixture of CO 2 gas and solid CO 2 (dry ice).
  • the process of the invention uses a cryogenic fluid with a density at least twenty times greater than its gas phase.
  • the injection of carbon dioxide involves an injector which is stitched into the wall of the chamber and transfers the mixture "gas + solid" to the center of the transfer channel of the gaseous medium.
  • the injection of a gas inerting in carbon dioxide, at the outlet of the cryogenic valve prevents clogging at the outlet of said valve and at the outlet of the injector, in the gaseous medium.
  • the inerting gas providing a gas sweep at the different elements of the device in which the two- phase CO 2 circulates, prevents pollution by foreign bodies, in particular moisture, and avoids the accumulation of dry ice at points where the geometry that its circulation would be difficult without entrainment by the inerting gas.
  • the liquid CO 2 is made available at a pressure generally of between 10 ⁇ 10 5 and 22 ⁇ 10 5 Pa (ie between 10 and 22 bar) and at a temperature generally of between -35 ° C. and -20 ° C.
  • the two-phase carbon dioxide is injected so that it is injected into the center of the gaseous medium and distributed partly at the current and partly at the counter-current of the gaseous flow.
  • the mixing and entrainment of the CO 2 is best ensured, thus avoiding its accumulation.
  • the risk of formation of plugs is very large given the temperature of this CO 2 (-80 ° C), so it is essential to immediately disperse it in the gaseous medium to be treated.
  • the presence of the inerting gas injected into the two- phase CO 2 according to the invention also makes it possible to limit the risk of plugging.
  • This inerting gas must be inert with respect to the chemical species present as well as regulators (flow control valves, injector specific to the invention, etc ). It is particularly advantageous to use as carbon dioxide inerting gas from the vaporization of a fraction of the liquid carbon dioxide provided, and taken upstream of the device. cryogenic relaxation. It should be noted that CO 2 not introducing a new chemical species can by extension also be considered as an inert gas.
  • the quantity of carbon dioxide injected is preferably regulated as a function of a target of a physical or chemical parameter to be reached, the measurement of this parameter is carried out in the gaseous medium, downstream of the injection point.
  • the cryogenic valve variable rate of the invention is controlled according to this set.
  • a cryogenic safety valve of the all-or-nothing type can also be placed upstream of the variable-flow cryogenic valve to cut off the supply of liquid CO 2 in the event of a malfunction, for example if the pressure is too high. high in the gaseous medium to be treated, if the temperature is too low or if another parameter considered major has exceeded a warning threshold.
  • the operator of the installation can also control this valve. When the supply of the variable rate cryogenic valve is cut off, the protection of the sensitive elements of the device by a low flow rate of the inerting gas is maintained.
  • the injector enters the enclosure over a length equivalent to half the width of said enclosure and according to a preferred variant, the device comprises, for supplying the inerting gas of the injection device, upstream cryogenic expansion device, means for sampling and vaporization of a fraction of the liquid carbon dioxide provided.
  • the device can therefore operate by being connected to a single source of carbon dioxide feed. It is also possible to use an inert gas present at the place of application or compressed air, it being understood that the inerting gas must not modify the behavior of the mixture obtained, and must not be contraindicated for the equipment .
  • Figure 1 is a schematic view of a device according to the invention and by Figures 2 and 2A which represent an example of an injector according to the invention, the Figure 2A being a sectional view along the axis AA of the end of the injector of the Figure 2 .
  • the injection device 1 is intended to supply two-phase carbon dioxide "gas + liquid" in a gaseous medium 2, under pressure transfer in a chamber 3, and this from a storage tank 4 of carbon dioxide liquid in which the liquid carbon dioxide is stored at a pressure between 14.10 5 and 20.10 5 Pa (between 14 and 20 bar) and at a temperature between -35 ° C and -20 ° C
  • the device 1 comprises a liquid CO 2 supply line formed of a liquid line 5 extending from the tank 4 to a variable rate cryogenic valve 6 which regulates a parameter "A" measured in the medium. gas 2 downstream of the injection point.
  • a filter 7 equipped with a stainless steel filter cartridge is placed upstream of the valve 6, it provides filtration of liquid carbon dioxide to protect the valve seat of solid impurities that may be present in the pipes.
  • a cryogenic expansion valve not shown in the Figure, protects the line downstream of the safety valve 8 after closing thereof.
  • the device 1 further comprises an inerting gas feed line, which in this case is gaseous CO 2 ; the line is constituted in the order of one vaporizer 10, an expander 11, a manually-controlled flow valve 12, a flowmeter with transmitter 13 and a non-return valve 14.
  • an inerting gas feed line which in this case is gaseous CO 2 ; the line is constituted in the order of one vaporizer 10, an expander 11, a manually-controlled flow valve 12, a flowmeter with transmitter 13 and a non-return valve 14.
  • a tee 15, fed in upper part with two- phase CO 2 coming from the ejector situated at the outlet of the valve 6, on the side of inerting gas (CO 2 gas) is connected at the bottom to an injector 16 ensuring the injecting the two- phase CO 2 mixture into the gaseous medium 2 by transfer under pressure into the chamber 3.
  • the injector 16 carries out the transfer of the CO 2 towards the center of the transfer channel of the gaseous medium.
  • the inside of the tee 15 and the injector 16 are protected from the medium to be treated thanks to a low but permanent flow of the inerting gas.
  • a control-regulating unit of the parameter "A” ensures the measurement of the value of the parameter "A” in the transfer line, processes -via the control member 9- the signal received from “A” as well as the signals which come from the various safety parameters monitored (temperature and pressure of the gaseous medium to be treated, etc.). It controls according to “A” the opening level of the variable rate cryogenic valve 6 to maintain the "A” parameter at its set point; it also controls the closing of the cryogenic safety valve 8 in the event of a major defect affecting a safety parameter, or in the event of refusal of treatment authorization by the operator, as well as the opening or closing of the vent valve according to the operating mode, generally synchronous with the other valves.
  • This control of the control unit is ensured on the basis of information communicated by the measurement transmitters AIT (measurement of the "A” parameter), PIT (measurement of the pressure in the gaseous medium 2), TT (measurement of the temperature middle 2) not referenced.
  • AIT measurement of the "A” parameter
  • PIT measurement of the pressure in the gaseous medium 2
  • TT measurement of the temperature middle 2
  • the Figure 2 represents in more detail an example of an injector according to the invention.
  • the injector 16 is supplied with two- phase CO 2 coming from the ejector 17 at the outlet of the valve 6 and inerting gas consisting of gaseous CO 2 . This feed is performed via the tee 15 which receives CO 2 inerting at the side entry 18 and the two- phase CO 2 from 17 in the upper part.
  • the injector 16 made of a thermo-insulating material, for example polysulfone, conducts the "gas + solid" mixture towards the center of the channel 3 for transfer of the gaseous medium 2.
  • the method of the invention is implemented for the enrichment in CO 2 of natural gas combustion fumes.
  • the "A" parameter to be regulated is the CO 2 content of these fumes. Initially at about 8% CO 2 , the fumes are enriched by the process of the invention to levels of between 12 and 18% for subsequent use in a papermaking process. The flow of smoke is of the order of 12 000 m 3 / h. The amount of CO 2 used is about 1200 m 3 / h CO 2 (gas equivalent) to reach 16% CO 2 in the flue gases. The fumes thus enriched are intended in particular for the manufacture of calcium carbonate.
  • the process of the invention is particularly applicable in many fields using CO 2 as raw material.
  • the enrichment implemented according to the invention does not milling using CO 2 gas emerges sizing constraints and disadvantages related thereto.
  • the invention is thus particularly suitable for industrial installations with fumes containing CO 2 , polluting agent in the state, and also using CO 2 as raw material.
  • the process of the invention can also be used in cases where it is desired to treat a transfer gas medium with CO 2 .
  • the process of the invention can thus advantageously be applied to the enrichment of CO 2 with fumes for the manufacture of calcium carbonate for the paper industry.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Catalysts (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
EP03763931A 2002-07-11 2003-07-07 Procede et dispositif d'injection de co2 diphasique dans un milieu gazeux en transfert Expired - Lifetime EP1534414B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0208734A FR2842123B1 (fr) 2002-07-11 2002-07-11 Procede et dispositif d'injection de co2 diphasique dans un milieu gazeux en transfert
FR0208734 2002-07-11
PCT/FR2003/002097 WO2004007061A2 (fr) 2002-07-11 2003-07-07 Procede et dispositif d’injection de co2 diphasique dans un milieu gazeux en transfert

Publications (2)

Publication Number Publication Date
EP1534414A2 EP1534414A2 (fr) 2005-06-01
EP1534414B1 true EP1534414B1 (fr) 2009-09-02

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EP03763931A Expired - Lifetime EP1534414B1 (fr) 2002-07-11 2003-07-07 Procede et dispositif d'injection de co2 diphasique dans un milieu gazeux en transfert

Country Status (10)

Country Link
US (1) US7648569B2 (ja)
EP (1) EP1534414B1 (ja)
JP (1) JP2005532161A (ja)
AT (1) ATE441472T1 (ja)
AU (1) AU2003263267A1 (ja)
BR (1) BR0312329B1 (ja)
CA (1) CA2490662C (ja)
DE (1) DE60329111D1 (ja)
FR (1) FR2842123B1 (ja)
WO (1) WO2004007061A2 (ja)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100443739C (zh) * 2005-12-16 2008-12-17 中海石油研究中心 一种气固、液固、液液引射加料的系统及配比输运方法
DE102008052802A1 (de) * 2008-10-22 2010-04-29 Messer France S.A.S Anordnung zum Eintragen von flüssigem Kohlendioxid in ein Medium
US20110265492A1 (en) * 2010-04-28 2011-11-03 Newman Michael D Freezer with cryogen injection control system
US20130074936A1 (en) * 2011-09-27 2013-03-28 Caterpillar Inc. Mis-fill prevention system
ITUB20160983A1 (it) 2016-02-23 2017-08-23 Soc It Acetilene E Derivati S I A D S P A In Breve Siad S P A Dispositivo e corrispondente metodo per l’erogazione di co2 liquida in ambienti a pressione inferiore a quella del suo punto triplo
US20230140807A1 (en) * 2021-11-03 2023-05-04 Biosenta Inc. Method and Apparatus for Producing Core-Shell Calcium Hydroxide-Calcium Carbonate Particles

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE791663A (fr) 1972-09-11 1973-03-16 Kohlensaurewerke C G Rommenholler Gmbh Procede et appareillage pour la production de composants gazeuxde reaction pour la preparation de moules et noyaux de fonderie
US4389820A (en) * 1980-12-29 1983-06-28 Lockheed Corporation Blasting machine utilizing sublimable particles
US4747421A (en) * 1985-03-13 1988-05-31 Research Development Corporation Of Japan Apparatus for removing covering film
US4806171A (en) * 1987-04-22 1989-02-21 The Boc Group, Inc. Apparatus and method for removing minute particles from a substrate
DE4034076A1 (de) * 1990-10-26 1992-04-30 Linde Ag Vorrichtung zur expansion verfluessigter gase
US5486132A (en) * 1993-06-14 1996-01-23 International Business Machines Corporation Mounting apparatus for cryogenic aerosol cleaning
US5378312A (en) * 1993-12-07 1995-01-03 International Business Machines Corporation Process for fabricating a semiconductor structure having sidewalls
FR2787862B1 (fr) * 1998-12-29 2001-01-26 Carboxyque Francaise Procede et dispositif d'injection regulee de dioxyde de carbone liquide dans un liquide sous pression
KR100385432B1 (ko) * 2000-09-19 2003-05-27 주식회사 케이씨텍 표면 세정용 에어로졸 생성 시스템

Also Published As

Publication number Publication date
DE60329111D1 (de) 2009-10-15
WO2004007061A2 (fr) 2004-01-22
FR2842123B1 (fr) 2004-08-27
JP2005532161A (ja) 2005-10-27
ATE441472T1 (de) 2009-09-15
CA2490662C (fr) 2012-01-24
BR0312329A (pt) 2005-04-12
FR2842123A1 (fr) 2004-01-16
EP1534414A2 (fr) 2005-06-01
CA2490662A1 (fr) 2004-01-22
US20050268786A1 (en) 2005-12-08
BR0312329B1 (pt) 2011-08-23
WO2004007061A3 (fr) 2004-04-08
AU2003263267A1 (en) 2004-02-02
US7648569B2 (en) 2010-01-19

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