WO2006068531A1 - Procede de purification et de division d'un melange a composants multiples, et dispositif permettant sa mise en oeuvre - Google Patents

Procede de purification et de division d'un melange a composants multiples, et dispositif permettant sa mise en oeuvre Download PDF

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Publication number
WO2006068531A1
WO2006068531A1 PCT/RU2004/000508 RU2004000508W WO2006068531A1 WO 2006068531 A1 WO2006068531 A1 WO 2006068531A1 RU 2004000508 W RU2004000508 W RU 2004000508W WO 2006068531 A1 WO2006068531 A1 WO 2006068531A1
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WIPO (PCT)
Prior art keywords
production
column
stream
flow
target component
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Application number
PCT/RU2004/000508
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English (en)
Russian (ru)
Inventor
Mikhail Yurievich Savinov
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Mikhail Yurievich Savinov
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Priority to PCT/RU2004/000508 priority Critical patent/WO2006068531A1/fr
Publication of WO2006068531A1 publication Critical patent/WO2006068531A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/028—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of noble gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/34—Krypton
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/36—Xenon

Definitions

  • the invention relates to cryogenic technology, in particular, to the purification and separation of multicomponent mixtures containing inert gases obtained in air separation plants, and can be used in the chemical and oil and gas industry.
  • a known method of separating a krypton-xenon concentrate purified from hydrocarbons comprising supplying and separating a krypton-xenon concentrate in a preliminary distillation column to form a stream of krypton fraction and a stream of xenon fraction, feeding and separating a stream of xenon fraction in a distillation column for separating high boiling impurities to form a stream of purified xenon fraction, supply and separation of the stream of purified xenon fraction in the production xenon column with the formation xenon production stream, feeding and separating the krypton fraction stream in the intermediate impurity recovery column to form a purified krypton fraction stream and intermediate impurities stream, feeding and separating the purified krypton fraction stream in the production krypton column to form the production krypton stream (see RF patent 2213609, B01D53 / 00).
  • the aim of the invention is to reduce the metal consumption, increase purity and reduce the loss of production gases with a complete processing scheme of a multicomponent mixture.
  • a device for the separation of krypton-xenon concentrate, purified from hydrocarbons includes a preliminary distillation column for separating a krypton-xenon concentrate into krypton and xenon fractions, a column for separating high-boiling impurities and a column for separating intermediate impurities for separating higher boiling impurities from the xenon and krypton fractions, respectively, production xenon and production krypton columns connected by lines with supply to the columns of power flows and the removal of the upper and lower product (see RF patent 2213609, B01D53 / 00).
  • the disadvantages of the known device are significant metal consumption, significant losses and insufficient purity of production gases.
  • the aim of the invention is to reduce the metal consumption, increase purity and reduce losses of production gases with a complete processing scheme of a multicomponent mixture.
  • This goal is achieved by the fact that in the device for cleaning and separating a multicomponent mixture containing two target components with different volatility, including a supply and filling ramps, a physicochemical cleaning unit with a flow line of a multicomponent mixture connected to a flow ramp and with a purified multicomponent flow line mixtures, a column for separating high-boiling impurities, containing an evaporator in the cube, a column for separating intermediate impurities, a production column for a less volatile target component, auction column of a more volatile target component, each of which contains a supply pipe for supplying a stream, a pipe for outputting a bottoms product and a pipe for outputting a top product, a gasifier, flow stimulators, a vacuum unit, a device for collecting blow-offs, supply and discharge lines for gas (liquids) flows with dead
  • the inventive method of purification and separation of a multicomponent mixture can be implemented in the inventive device, schematically shown in the drawing.
  • the device (installation) contains a discharge ramp 1 with cylinders 2 of a multicomponent mixture, a physicochemical treatment unit 3, consisting of a recuperative heat exchanger 4, an electric heater 5, a reactor 6 and an adsorber 7, a filter 8, a low-temperature rectification unit 9, a gasifier 14, a blow-off collecting device 15, flow drivers 16, 17, 18, a filling ramp 19 of a production gas of a less volatile target component with cylinders 20 pre-inflated with a production gas of a less volatile target component, a filling ramp 21 of a production gas of a more volatile target component with cylinders 22 pre-inflated with production gas of a more volatile target component, receiver 23, vacuum unit 24, which contains one or more, for example, vacuum mechanical pumps or vacuum jet pumps 25 and at least one vacuum cryosorption pump 26, a cylinder 27 with a gas having a high sorption capacity with respect to the target components
  • Block low-temperature distillation 9 includes a column for the allocation of high-boiling impurities 10, a production column for a less volatile target component 11, a column for the separation of intermediate impurities 12, a production column for a more volatile target component 13.
  • Each column in the head has a condenser-evaporator, cooled by refrigerant, with a closed cavity filled with a working fluid, and at the bottom there is a cube equipped with an electric heating element.
  • the cube of the high-boiling impurity separation column 10 also contains an evaporator 29 with an additional heater, made, for example, of pipe-in-pipe type heat exchange elements with a coolant supply through line 30 to the central pipes.
  • Consumption ramp 1 by line 31 of the stream of the multicomponent mixture (stream A) is connected to the inlet pipe of the physicochemical treatment unit 3, the outlet pipe of which is connected by line 32 of the stream of the purified multicomponent mixture (stream B) through a heated evaporator 29 with a pipe for supplying a column of high-boiling impurities 10.
  • the multicomponent mixture flow line 31 is connected by a line 33 to a gas cylinder 27 having a high sorption capacity with respect to the target components, and the cleaned multicomponent mixture flow line 32 can be communicated via a line 34 to a blower collection device 15 or via a 35 s line a nozzle located in the middle of the contact space of the high-boiling impurity recovery column 10.
  • the filter 8 installed on the line 32 of the stream of the purified multicomponent mixture is located directly in front of the ok low temperature rectification 9.
  • the high-boiling impurity separation column 10 in the upper zone of the concentration part has an outlet pipe for the upper product, which is connected by a stream line 36 of the purified fraction of both target components (stream B) to the pipe in the middle part of the production column of the less volatile target component 11, and in the lower part in the cube, a nozzle connected by a line 37 of a stream of high-boiling impurities (stream G) through a gasifier 14 with an exit from the device or line 47 with a device for collecting blow-offs 15.
  • the head of the column for separating high-boiling impurities 10 in the cap condenser-evaporator has a branch pipe, connected by a line 38 with flow line B.
  • the production column of the less volatile target component 11 in the upper zone of the concentration part has an outlet pipe for the upper product, which is connected by a line 39 of the mixed flow fraction of the more volatile target component (stream D) with a pipe in the middle of the intermediate separation column 12, and in the lower part in the cube - a pipe connected by a line 40 of a production stream of a less volatile target component (stream E) through a gasifier 14 and a flow inducer 17 with a filling ramp 19 of a production gas of a less volatile target component.
  • the column head of the less volatile target component 11 in the cap of the condenser-evaporator has a pipe connected by line 41 to the flow line D.
  • the column for the separation of intermediate impurities 12 in the head in the lid of the condenser-evaporator has a nozzle connected by a line 42 of the stream of the purified fraction of the more volatile target component (stream G) to the nozzle in the middle part of the production column of the more volatile target component 13, and in the lower part in the cube there is a nozzle connected by a line 43 of the stream of intermediate impurities (stream 3) through the gasifier 14 with the exit from the device or through line 44 with the device for collecting blowers 15.
  • the production column of the more volatile target component 13 in the head in the cap of the condenser-evaporator has a pipe connected by a flow line 45 low boiling impurities (stream I) with the exit from the device, and in the lower part in the cube, a pipe connected by a line 46 of the production stream of a more volatile target component (stream K) through a gasifier 14 and a flow inducer 16 with a filling ramp 21 of the production gas of a more volatile target component .
  • the purge collection device 15 line 48 through the flow rate 18 is connected to the outlet of the device or line 49 is communicated with a pipe located in the lower part of the contact space of the high-boiling impurity separation column 10.
  • Both branches of the filling ramps 19, 21 are connected by production gas return lines 50, 51 with nozzles located respectively in the cube of the production column of the less volatile target component 11 and in the cube of the production column of the more volatile target component 13, and cylinders 20, 22 connected to the filling ramps filling them with production gas is pre-inflated with the same production gas.
  • Both branches of the consumable 1 and filling ramps 19, 21 contain Al, A2, AZ fittings connected to the analysis lines and are connected by separate lines 52-l ⁇ 52-3 with a vacuum manifold 52, and lines 53-1 ⁇ 53-3 with a vacuum collector 53.
  • the vacuum manifold 52 is connected by a pipe 54 to a mechanical (jet) vacuum pump 25 included in the vacuum unit 24, and the vacuum collector 53 through a receiver 23 is connected by a pipe 55 to a cryosorption vacuum pump 26, which is connected by a pipe 56 to line 48.
  • Contact space each column Yu ⁇ IZ pipelines dams 52-4 ⁇ 53-7 are connected to a vacuum manifold 52, and by pipelines 53-4 ⁇ 53-7 to a vacuum collector 53.
  • Each distillation column Yu ⁇ IZ contains a heater of the contact space 61-64, and the lines of production flows 40, 46 - heaters 65-1, 65-2, 66-1,66-2.
  • Filling ramps 19, 21, flow drivers 16 ⁇ 18 of the flow lines B, D, F, and others contain a number of dead-end pipelines, for example 58, which is a supply pipe to the safety valve 57 (other safety valves are not shown in the diagram). Such pipelines additionally contain a purge line 59.
  • the circuit provides a source of production gas of a more volatile target component 28, which is connected by line 60 to the high-boiling impurity recovery column 10.
  • the method of purification and separation of a multicomponent mixture using the example of a krypton-xenon mixture obtained in air separation plants is carried out as follows. In this case, xenon is the less volatile target component, and krypton is the more volatile target component.
  • Cylinders 2 with the original krypton-xenon mixture are installed on the supply ramp 1, cylinders 20 pre-pressurized with production xenon on the filling ramp 19 of production gas of a less volatile target component, and cylinders 22, previously pre-inflated by production xenon inflated with production krypton, a source 28 of production gas of a more volatile target component is filled with production krypton, in a cylinder 27 as a gas having a large sorption capacity To target components, carbon dioxide is used.
  • Consumption ramp 1 filling ramps 19, 21 with closed valves on cylinders, a regenerated physical and chemical cleaning unit 3, working cavities of distillation columns Yu ⁇ IZ of line 40, 46 of production streams with heaters 61-64, 65-1, 65-2 turned on , 66-1, 66-2, flow rate drivers 16 ⁇ 18 are evacuated by connecting through a vacuum manifold 52 to a mechanical vacuum pump 25. The exhaust of the mechanical vacuum pump 25 is vented to the atmosphere. Then, a krypton stream is fed through the line 60 from the source of production gas of a more volatile target component 28 into the contact spaces of distillation columns Yu ⁇ IZ.
  • the krypton-xenon mixture After supplying refrigerant (liquid nitrogen) to the condensers - evaporators, into the closed cavities of the working fluid evaporator-condensers (mixture of krypton and oxygen gases, nitrogen) and cooling the distillation columns, the krypton-xenon mixture is supplied.
  • a krypton-xenon mixture obtained in air separation plants containing krypton Kr, xenon Xe with impurities for example, hydrocarbons, nitrogen N 2 , oxygen O 2 , ozone O 3 , argon Ar, neon Ne, helium He, hydrogen H 2 , carbon monoxide CO, carbon dioxide CO 2 , tetrafluoromethane CO 4 , hexafluoroethane CF 4 , monofluorotrichloromethane CFCl 3 , difluorodichloromethane CF 2 Cl 2 and others.
  • impurities for example, hydrocarbons, nitrogen N 2 , oxygen O 2 , ozone O 3 , argon Ar, neon Ne, helium He, hydrogen H 2 , carbon monoxide CO, carbon dioxide CO 2 , tetrafluoromethane CO 4 , hexafluoroethane CF 4 , monofluorotrichloromethane CFCl 3 , difluo
  • the krypton-xenon mixture stream is heated in a recuperative heat exchanger 4 and an electric heater 5, catalytic oxidation of hydrocarbons in the reactor 6, cooling and absorption of water and carbon dioxide in the adsorber 7. In addition to water and carbon dioxide in the adsorber, and a significant amount of krypton and xenon is also retained in the reactor.
  • the krypton-xenon mixture is fed through line 32 of the stream of the purified multicomponent mixture through a filter 8 located directly in front of the low-temperature rectification unit 9, an evaporator 29 with additional heating to the middle part of the high-boiling impurity separation column 10, in which the condensate is condensate krypton.
  • a filter 8 located directly in front of the low-temperature rectification unit 9, an evaporator 29 with additional heating to the middle part of the high-boiling impurity separation column 10, in which the condensate is condensate krypton.
  • high-boiling impurities with respect to xenon are collected in the cube, for example, C 2 F 6 , CFC lz, CF 2 Cl, etc., and a purified fraction of both target components containing xenon, krypton and volatile with respect to xenon impurities.
  • High boiling impurities from the cube of the column through line 37 of the flow of high boiling impurities through the gasifier 14 are removed from the unit or sent via line 47 to the purge collecting device 15.
  • the stream of the purified fraction of both target components is removed from the upper zone of the concentration part of the column, which allows the use of krypton condensate instead of xenon condensate in a known device, reduce the pressure of the working fluid in the closed cavity of the condenser-evaporator and the mass of the apparatus.
  • Line 38 is a purge line for the condensation cavity of the condenser-evaporator.
  • the purified fraction of both target components is sent via line 36 to the middle of the production column of the less volatile target component 11, where the krypton condensate is reflux.
  • production xenon is collected in the cube of the column, which is sent along the line 40 of the production stream of the less volatile target component through the gasifier 14 to the flow inducer 17 and then to the filling ramp 19, and the upper product contains krypton, all volatile with respect to xenon substances and traces of xenon.
  • the high-boiling impurity recovery column 10 it is withdrawn from the upper zone of the column concentration section and sent through the mixed stream stream 41 of a fraction of a more volatile target component to the middle of the intermediate-separation column 12.
  • Line 41 is a purge conduit for the condensation cavity condenser-evaporator.
  • each branch of the filling ramp 19 and the filling of the cylinders 20 is carried out in the following sequence: preliminary evacuation of the branch by connecting its line 52-1 to the vacuum manifold 52 of the mechanical vacuum pump 25, disconnecting it from the vacuum manifold 52 and connecting the line 53-1 to the cryosorption vacuum manifold 53 vacuum pump 26, - sequential short-term opening of valves on cylinders 20, previously pressurized with production xenon, blowing branches and connecting to a vacuum manifold ohm 52, final evacuation, pressurization of the ramp branch with production xenon from line 40, analysis of production xenon from fitting AI, - opening valves on cylinders 20 and filling them with production xenon, closing valves on cylinders and returning the remaining production xenon in the ramp branch on return line 50 production gas per cube column
  • tetrafluoromethane CF 4 and other impurities having a boiling point at the same pressure are higher than the boiling point of krypton and therefore are not volatile with respect to krypton, are concentrated in the cube of the column, whence they are passed through line 43 a stream of intermediate impurities (stream 3) through a gasifier 14 is removed from the device or sent via line 44 to a collector for blowing off 15.
  • a low-boiling impurity stream (stream I) is withdrawn and the low-boiling impurity line is removed from the device 45.
  • the low-boiling impurity stream consists of a mixture of N 2 , Ar, O 2 , O 3 , He, H 2 , CO, etc., and the content of krypton in it does not exceed 0.3% vol.
  • the sequence of operations and the preparation of the flow line K, the flow driver 16, the branches of the filling ramp 21 for production krypton are performed similarly to the above-described sequence of operations and the preparation for the production xenon of the flow line E, the flow stimulator 17, the branches of the filling ramp 19.
  • the contents of the cube of production columns 11, 13 are discharged into cylinders 20, 22, high-boiling and intermediate impurities from columns 10 and 12, and all remaining contents of the contact space of columns 10, 11, 13 after evaporation are transferred to column 12 , from where, through line 43, they are sent to a blow-off collecting device 15 and then, along line 48, through a flow inducer 17, they are taken out of the installation into storage for subsequent processing.
  • the gas remaining in the contact space of the columns, as well as in other apparatus and communications of the device is then transferred to the cryosorption vacuum pump 26 by communicating them with pipelines 53-1 ⁇ 53-13 with the vacuum manifold 53. After saturation of the cryosorption vacuum pump, it is regenerated, and the recovered the regeneration of the gas is sent through lines 56 and 48 to the device for collecting blowers 15.
  • cryosorption vacuum pump in the evacuation unit maximally eliminates the loss of the target components of the multicomponent mixture that occur, for example, when changing cylinders on the supply and filling ramps, when switching reactors and adsorbers in the physicochemical cleaning unit, and other operations associated with the continuous operation of the device .
  • Another proposal of the present invention in terms of reducing the loss of target components is as follows. It was noted above that during the operation of the physicochemical purification unit, a significant amount of krypton and xenon is delayed in the adsorber and reactor. Therefore, immediately before regeneration from the cylinder 27, a stream of carbon dioxide is supplied to reactor 6 and adsorber 7 through line 33, which, adsorbing, displaces krypton and xenon from the contact mass of the adsorber and reactor, which are sent to mixtures with other gases through line 34 to the purge collecting device 15 .
  • the filter 8 located directly in front of the entrance to the low-temperature distillation unit prevents solid particles from contacting the contact mass of the reactor and adsorber and other particles capable of adsorbing impurities and impairing the purity of the production target components. Additional heating of the evaporator 29 prevents solid precipitation on the heat transfer surface of the evaporator from the side of the purified multicomponent medium, especially during the start-up of the device, when the temperature in the cube of the high-boiling impurity recovery column is close to the saturation temperature of the more volatile target component.
  • the proposed method and device for the purification and separation of a multicomponent mixture containing two target components with almost any impurities allows to achieve, with a full processing scheme in a continuous process, the extraction coefficient for the target components is not less than 0.99995 when the content of impurities in the production target components is not more than 10 * 10 "11 vol. Shares.
  • the metal consumption of the device is reduced in comparison with the known solution both by reducing the number of distillation columns and by reducing the mass of condensate ditch evaporators.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention se rapporte à un procédé permettant de traiter et de diviser un mélange à composants multiples. Le procédé selon l'invention consiste à diviser un mélange à composants multiples (écoulement B), qui contient deux composants cibles de volatilité différente, dans une colonne destinée à extraire les impuretés à haut point d'ébullition, de façon à produire une fraction traitée des deux composants cibles (écoulement C) et des impuretés semi-volatiles ; à diviser l'écoulement C en un composant cible moins volatil de production et en une fraction de mélange d'un composant cible plus volatil (écoulement D), dans une colonne destinée à produire un composant cible moins volatil ; à extraire de l'écoulement D les impuretés semi-volatiles dans une colonne destinée à extraire les impuretés intermédiaires, de façon à générer un écoulement D traité, lequel est divisé à l'aide d'un procédé connu ; à procéder à l'extraction de l'écoulement C et de l'écoulement D à partir de la zone supérieure de la partie de concentration de la colonne ; à filtrer l'écoulement B, à mettre sous vide les cavités des appareils et les communications, qui sont chauffées par une pompe mécanique avant leur mise en fonctionnement, et par une pompe cryogénique lors de leur arrêt ; à purger les bouts aveugles et les rampes, et à éliminer de l'adsorbeur et du réacteur les composants cibles avant la régénération. L'invention concerne aussi un dispositif permettant de mettre en oeuvre le procédé selon l'invention. L'invention permet d'améliorer la pureté d'un écoulement, de réduire les pertes de gaz de production et la consommation de métaux.
PCT/RU2004/000508 2004-12-17 2004-12-17 Procede de purification et de division d'un melange a composants multiples, et dispositif permettant sa mise en oeuvre WO2006068531A1 (fr)

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PCT/RU2004/000508 WO2006068531A1 (fr) 2004-12-17 2004-12-17 Procede de purification et de division d'un melange a composants multiples, et dispositif permettant sa mise en oeuvre

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PCT/RU2004/000508 WO2006068531A1 (fr) 2004-12-17 2004-12-17 Procede de purification et de division d'un melange a composants multiples, et dispositif permettant sa mise en oeuvre

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4417909A (en) * 1978-12-04 1983-11-29 Airco, Inc. Gas separation process
US6351970B1 (en) * 1998-05-26 2002-03-05 Linde Gas Aktiengesellschaft Method for extracting xenon
RU2213609C1 (ru) * 2002-11-15 2003-10-10 Савинов Михаил Юрьевич Способ разделения криптоно-ксенонового концентрата и устройство для его осуществления

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4417909A (en) * 1978-12-04 1983-11-29 Airco, Inc. Gas separation process
US6351970B1 (en) * 1998-05-26 2002-03-05 Linde Gas Aktiengesellschaft Method for extracting xenon
RU2213609C1 (ru) * 2002-11-15 2003-10-10 Савинов Михаил Юрьевич Способ разделения криптоно-ксенонового концентрата и устройство для его осуществления

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