WO2014148937A1 - Procédé de production d'un concentré de xénon à partir d'oxygène contenant du xénon et installation correspondante - Google Patents

Procédé de production d'un concentré de xénon à partir d'oxygène contenant du xénon et installation correspondante Download PDF

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Publication number
WO2014148937A1
WO2014148937A1 PCT/RU2013/000223 RU2013000223W WO2014148937A1 WO 2014148937 A1 WO2014148937 A1 WO 2014148937A1 RU 2013000223 W RU2013000223 W RU 2013000223W WO 2014148937 A1 WO2014148937 A1 WO 2014148937A1
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WIPO (PCT)
Prior art keywords
xenon
adsorber
valve
output
radon
Prior art date
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PCT/RU2013/000223
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English (en)
Russian (ru)
Inventor
Виталий Леонидович БОНДАРЕНКО
Николай Петрович ЛОСЯКОВ
Валерий Борисович ВОРОТЫНЦЕВ
Александр Петрович ГРАФОВ
Валентин Иванович ЧЕРЕПАНОВ
Владислав Васильевич АЛЕКСАХИН
Original Assignee
Bondarenko Vitaly Leonidovich
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Application filed by Bondarenko Vitaly Leonidovich filed Critical Bondarenko Vitaly Leonidovich
Priority to PCT/RU2013/000223 priority Critical patent/WO2014148937A1/fr
Publication of WO2014148937A1 publication Critical patent/WO2014148937A1/fr

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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
    • B01D53/02—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof
    • C01B23/001—Purification or separation processes of noble gases
    • C01B23/0036—Physical processing only
    • C01B23/0052—Physical processing only by adsorption in solids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/18—Noble gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/104—Oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/11—Noble gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40086—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by using a purge gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0029—Obtaining noble gases
    • C01B2210/0037—Xenon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0045—Oxygen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0078—Noble gases
    • C01B2210/0087—Radon

Definitions

  • the invention relates to processes for producing inert gases and can be used to obtain xenon concentrate from a xenon-containing oxygen stream.
  • xenon is obtained from a concentrate containing 0.2% Kg and Xe and which is successively passed through two layers of adsorbent until krypton is saturated with the second layer along the concentrate, then the eluent is fed into the second layer for desorption by heating krypton, blocking the message between the layers, moreover, the concentrate after the first layer is switched to the second layer of a parallel adsorber until xenon appears at the outlet of the first layer, after which xenon is desorbed [SU 1369771, A1, B01D53 / 02, 01.30.1988].
  • the disadvantage of this method is also a relatively narrow scope, since it can also be used only in the preliminary preparation of xenon and krypton concentrate in oxygen.
  • a method for producing xenon from a gas mixture in which the initial gas mixture containing xenon is sent for adsorption to a contact apparatus, which is filled with at least one adsorbent layer having an absorption capacity for xenon of 8-10 times higher absorption capacity in relation to other components of the gas mixture, the adsorption process is continued until xenon appears in the gas mixture, the adsorbent is regenerated with constant heat input at temperatures e, ranging from 333 to 353 ° K, the desorption process is continued until the cessation of xenon release from the adsorbent [RU 2259522, CI, F25J3 / 00, B01D53 / 02, 08/27/2005].
  • the disadvantage of this method is the relatively high radiation factor in the output useful product, caused by the relatively high presence of radon in it.
  • the closest in technical essence is a method for producing xenon concentrate in air separation plants, including the separation of the main and expandable air flows in the lower and upper columns into flows, the flow of a gaseous stream from the lower column to the main condenser unit, the condensation of a gaseous nitrogen stream and a liquid stream nitrogen from the block of main capacitors to the lower column, the output of the main stream of liquid oxygen from the upper column, which is carried out with the subsequent feeding it to the block of main condensers, where partial evaporation of the main stream of liquid oxygen is carried out, while part of the main stream of liquid oxygen is removed from the block of main capacitors in the form of a circulation stream of liquid oxygen, then part of the circulation stream of liquid oxygen is fed to the evaporator-condenser, where partial evaporation of the last stream with the formation of two streams - a stream of purified gaseous oxygen and a stream of oxygen that removes explosive impurities from the air separating installation, and the flow of oxygen outputting explosive impurities from
  • the disadvantage of the closest technical solution regarding the method is its relatively low safety, caused by a high radiation factor in the output useful product due to the relatively high presence of radon in it.
  • the required technical result in relation to the method is to increase the safety of the method.
  • One of the known devices contains a block of xenon adsorbents, which is connected via a pipe to a block of krypton adsorbents through a first heat exchanger, as well as a first and second gas blower, which are connected via pipes to a block of xenon adsorbents and a block of krypton adsorbents, respectively, and a second heat exchanger, which connected to at least one of the adsorbents of additional purification, which is connected via a labor pipe to the xenon adsorbent block [SU 1745313, A2, B01D53 / 02, 07.07.1992 ].
  • the disadvantage of this device is the relatively narrow functionality, since it can be used to obtain a xenon concentrate only from a mixture of xenon and krypton.
  • the closest in technical essence to the proposed device for producing xenon concentrate from xenon oxygen according to the method proposed above is a device for producing xenon from a gas mixture containing at least one contact apparatus filled with an adsorbent, a gas holder, a first contact furnace for catalytic burning of hydrocarbons , a second contact furnace for the catalytic burning of fluorochloride derivatives of saturated hydrocarbons, a gas cooler, a gas drying and purification unit, including containing two alternately working adsorber-desiccants, and a unit for low-temperature separation of components of gas mixtures, including the corresponding equipment (regenerative heat exchangers, distillation columns, separators, expanders, filters, etc.), moreover, the device can have several contact devices with the ability to turn them off and switch to the appropriate operating modes, namely the adsorption or regeneration (desorption) of the adsorbent [RU 2259522 , CI, F25J3 / 00, B01D53 / 02
  • the disadvantage of the closest technical solution is the relatively narrow functionality, since although it allows you to get xenon from the gas mixture, it does not provide a low radiation factor in the output useful product, caused by the relatively high presence of radon in it.
  • the required technical result with respect to the device is to expand the functionality by additionally providing a low radiation factor in a useful product.
  • the required technical result with respect to the method is achieved in that, in the method according to which the initial gas mixture, which uses xenon-containing oxygen, is subjected to cooling beforehand, the initial gas mixture is sent to the xenon-containing adsorber, from which the xenon concentrate is subsequently extracted, radon is preliminarily removed from the initial gas mixture by directing it to a cooled sorbent of a radon-retaining adsorber, and extracting xenon concentrate ksenonozaderzhivayuschego of the adsorber is carried out by creating a temperature gradient in the sorbent ksenonozaderzhivayuschego canister from its input to output before the desorption wave of xenon at the output, after which produce output xenon fraction.
  • the required technical result regarding the device is achieved by the fact that, in the installation containing the xenon adsorber, a heat exchanger and a filling ramp, a radar-retaining adsorber, an electric heater, a membrane compressor, an ejector are introduced, the flowmeter and valves from the first to the fifteenth, moreover, the filling ramp through the eleventh valve is connected to the ejector by a pipe connected to the outlet of the membrane compressor, the ejector through the tenth valve is connected to the inlet of the flowmeter by a pipe, which through the ninth valve is connected to the input of the heated nitrogen supply, the output of the flowmeter is connected with the input of an electric heater, the output of which is connected to the pipeline between the seventh valve and the input of the xenon adsorber, the output of which through the twelfth valve is connected to the through the eighth valve is connected to the inlet of the membrane compressor, and through the fifteenth and fourth valves in series, it is connected to the first output of the heat exchanger, the
  • the required technical result is achieved by the fact that, as a xenon-retaining sorbent, silica gel or alumina or NaX zeolite is used.
  • activated carbon or silica gel or alumina or NaX zeolite is used as a radon-retaining sorbent.
  • the drawing shows a functional diagram of the installation for implementing the proposed method for producing xenon concentrate from xenon-containing oxygen.
  • Installation for implementing the proposed method for producing xenon concentrate from xenon-containing oxygen contains a radar-holding adsorber 1, a xenon adsorber 2, a heat exchanger 3, a membrane compressor 4, an ejector 5, a filling ramp 6, a xenon-containing sorbent 7, placed in a xenon adsorber 2, and a radon-containing sorbent 8 radon holding adsorber 1, electric heater 9, flow meter 10 and valves from the first to the fifteenth 1 1 ... 25, respectively.
  • the filling ramp 6 through the eleventh valve 21 is connected to the ejector 5 by a pipe connected to the output of the membrane compressor 4.
  • the ejector 5 through the tenth valve 20 is connected to the input of the flowmeter 10 by a pipe, which through the ninth valve 19 is connected to the input of the heated nitrogen supply, the output of the flowmeter 10 is connected to the input of the electric heater 9, the output of which is connected to the pipeline between the seventh valve 17 and the input of the adsorber 2 xenon, the output of which through the twelfth valve 22 is connected to the atmosphere, through the eighth valve 18 is connected to the input of the membrane compressor 4, and through the fifteenth 25 and fourth 14 valves in series, with p the first input of the heat exchanger 3, the first output of which through the first 1 1 valve is connected to the output of the return oxygen.
  • the output of the radon holding adsorber 1 through the seventh valve 17 is connected to the pipeline between the seventh valve 17 and the xenon adsorber 2, and through in series installed thirteenth valve 23 and sixth valve 16, interconnected by a chilled nitrogen supply pipe, is connected to the third input of the heat exchanger 3, the third output of which is connected through the third valve 13 to the atmosphere.
  • the proposed method for producing xenon concentrate from xenon-containing oxygen is implemented in the proposed installation as follows.
  • the main purpose of the proposed method and its installation is to extract xenon from the so-called "safety stream", which is liquid oxygen taken from the tail of the air separation plants (VRU), from which explosive impurities (primarily hydrocarbons) are removed from them. Typically, this liquid-like stream is converted to gaseous in the ASU itself.
  • safety stream liquid oxygen taken from the tail of the air separation plants (VRU)
  • explosive impurities primarily hydrocarbons
  • the essence of the present invention lies in the fact that the process of adsorption of xenon from a gaseous "safety stream" occurs in one adsorber, the dimensions of which are selected so that its operating time at the application stage (absorption of xenon from oxygen) is approximately 3 months. Moreover, the duration of the desorption and delivery of the product is about 2 days. This allows you to significantly reduce the capital costs and dimensions of the means of concentration, in comparison with known installations, with minimal product losses associated with the shutdown of the adsorber to desorption and delivery of the target product.
  • an ejector 5 is introduced into the installation, which allows a 3-4-fold increase in the flow of gas xenon circulating through the adsorber 2, in comparison with the known installations, with the same compressor performance.
  • the radon-trapping adsorber 1 the dimensions of which are much smaller than the xenon adsorber 2 and which is designed to practically completely radon retard, are included in the technological scheme of the installation in front of the xenon adsorber 2. It is advisable to choose the dimensions of this adsorber in such a way that the advance of the radon adsorption front is limited by the length of the layer of the radon-retaining sorbent 8.
  • the adsorption proper which determines the dynamics of the radon absorption process
  • the radiation power in the xenon concentrate taken from the main adsorber is at the level of the natural background.
  • the claimed method for producing xenon concentrate can be implemented on the installation, schematically shown in the drawing and containing two technologically sequentially connected adsorbers (radon-retaining adsorber 1 and xenon adsorber 2) connected to a single technological scheme using valves, pipelines, and also including a heat exchanger 3 , compressor 4, ejector 5 and filling ramp 6 with cylinders.
  • the installation has connections with an air separation device to obtain the necessary amount of refrigerants from it and return oxygen purified from impurities to it.
  • An electric heater 9 is included in the circuit, which allows desorption of the sorbent and its regeneration.
  • the installation is equipped with the necessary instrumentation, for example, a flowmeter 10. An example implementation of the inventive method on the installation for its implementation.
  • the oxygen stream with xenon contained in it from an external air separation device is directed through a second valve 12 to a heat exchanger 3, where it is cooled to operating temperature due to the cold going countercurrent through the sixth 16 and third 13 valves, for example, nitrogen gas taken from the air separation device, and also due to the cold returned to the air separation device through the fourth 14 and first 1 1 valves of the oxygen stream purified from xenon .
  • an external air separation device for example, from a liquid oxygen evaporator
  • Cooled oxygen containing xenon through the fifth valve 15 is directed to a radon-retaining adsorber 1 filled with a radon-retaining sorbent 8, where radon is completely extracted from it, and partially heavy hydrocarbons, such as ethane, are extracted. Then, the oxygen flow with xenon inside it through the seventh valve 17 is directed to the input of the xenon adsorber 2, filled with xenon-retaining sorbent 7, where xenon, part of krypton and methane, as well as part of oxygen are adsorbed. This stage continues until xenon slip occurs at the output of the adsorber 2 (based on the size of the adsorber and the technological mode, the stage lasts from 60 to 90 days).
  • a replacement operation is carried out in the xenon adsorber 2, with the aim of replacing the explosive oxygen atmosphere in the presence of methane with a safe nitrogen.
  • the seventh 17 and fifteenth 25 valves are closed and nitrogen is supplied to the input of the xenon adsorber 2 through the ninth valve 19 with an oxygen content of less than 0.1%.
  • Nitrogen, passing adsorber 2, through the twelfth valve 22 is discharged into the atmosphere.
  • the required nitrogen flow rate is controlled by a flow meter 10.
  • substitution stage continues until the residual oxygen content at the point at the outlet of the xenon adsorber 2 drops to 0.1-1-0.5%, otherwise hazardous oxygen concentrations in the mixture may occur at the subsequent separation stage (in particular, in the absence of nitrogen injection in circuit) leading to explosive situations.
  • a moving temperature field is created in the xenon adsorber 2 from its input to the output, which is formed using the circulating circuit included in the operation.
  • Ninth 19 and the twelfth 22th valves are closed, and the eighth 18th and tenth 20 are opened.
  • the electric heater 9 is switched on, providing the necessary high temperature at the inlet to the xenon adsorber 2.
  • the xenon adsorbed on the xenon-retaining sorbent 7 will shift in the exit direction, while concentrating in the underlying layers of the xenon-retaining sorbent 7.
  • the production xenon concentrate is injected into the cylinders of the filling ramp 6 through the eleventh valve 21.
  • opening the ninth valve 19 nitrogen is supplied, so that the pressure in the circuit is kept constant.
  • the circulation circuit is opened by closing the tenth valve 20.
  • the ejector 5 is also closed, the electric heater 9 is turned off and the remaining on the xenon-containing sorbent 7 and in it intergranular space, the concentrate is pumped into the cylinders of the filling ramp 6 by displacing it with nitrogen from xenon adsorber 2, for which nitrogen is supplied through the ninth valve 19.
  • the concentrate is stopped pumping into the filling ramp 6, the membrane compressor 4 is stopped and all valves are closed.
  • the ninth 19 and twelfth 22 valves are opened, the necessary nitrogen flow rate at the inlet to the xenon adsorber 2 is established by the flowmeter 10 and the electric heater 9 is turned on, raising the temperature of the regenerating gas at the inlet to a predetermined limit (control is carried out by the temperature at the outlet of the xenon adsorber 2.
  • the regeneration of the xenon-retaining sorbent 7 ends upon reaching a predetermined temperature at the outlet of the xenon adsorber 2. After that, turn off the electric heater 9 and close the ninth 19 and twelfth 22 valves. Then, xenon adsorber 2 is cooled to operating temperature by supplying cold nitrogen through the fourteenth valve 24 from an air separation device. Past adsorber
  • Regeneration and cooling of the sorbent in the radon-retaining adsorber 1 is carried out simultaneously with similar operations in the adsorber 2.
  • the seventh 17 and fourteenth 24 valves are provided in the installation.
  • the required technical result is achieved, which consists in increasing the level of safety of their application and use, since the level of the radiation factor in the useful product decreases and the oxygen concentration in the presence of methane decreases.
  • the improvement of the known device allows to expand its functionality by providing a reduction in the radiation factor in the output useful product and at the same time reduce the duration of separation operations, in particular, due to the introduction of an ejector in the device, which allows several times increase the intensity of circulation through the adsorber stripping gas stream.
  • K Pads / Pdes, where Pads is the duration of the adsorption step, days, Pdes is the duration of the step desorption, day. Due to the exclusion of a separate substitution stage, by combining it with the concentration and separation stage, the value of Pdes decreases significantly and, therefore, K. increases.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

L'invention concerne des processus technologiques pour produire des gaz inertes. Pour produire un concentré de xénon, le mélange gazeux constitué d'oxygène contenant du xénon est préalablement refroidi, le radon en est évacué au moyen d'un sorbant refroidi et d'un adsorbant de rétention de radon, puis il est dirigé dans un adsorbant de rétention de xénon à partir duquel on extrait ensuite le concentré de xénon. L'oxygène dans l'adsorbant de rétention de xénon est périodiquement remplacé par un milieu inerte par la coupure d'alimentation en mélange gazeux et par l'acheminement dans l'adsorbant de rétention de xénon d'un gaz de remplacement jusqu'à l'obtention à la sortie d'une concentration résiduelle d'oxygène à un seuil inférieur ou égal au seuil prédéterminé. Le concentré de xénon est extrait par la création d'un gradient de température dans le sorbant de l'adsorbant de rétention de xénon de son entrée à sa sortie, jusqu'à la formation d'une vague de désorption de xénon à la sortie, après quoi on extrait la fraction de xénon. L'installation pour mettre en oeuvre le procédé comprend un adsorbant de xénon, un échangeur de chaleur, un adsorbant de rétention de radon, un réchauffeur électrique, un compresseur à membrane, un éjecteur, un débitmètre, des robinets et des conduites. L'invention permet de réduire le facteur de rayonnement dans le produit obtenu.
PCT/RU2013/000223 2013-03-19 2013-03-19 Procédé de production d'un concentré de xénon à partir d'oxygène contenant du xénon et installation correspondante WO2014148937A1 (fr)

Priority Applications (1)

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PCT/RU2013/000223 WO2014148937A1 (fr) 2013-03-19 2013-03-19 Procédé de production d'un concentré de xénon à partir d'oxygène contenant du xénon et installation correspondante

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PCT/RU2013/000223 WO2014148937A1 (fr) 2013-03-19 2013-03-19 Procédé de production d'un concentré de xénon à partir d'oxygène contenant du xénon et installation correspondante

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112129040A (zh) * 2020-09-27 2020-12-25 杭州制氧机集团股份有限公司 一种液氙冷却、氙气再液化撬装装置及其方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5039500A (en) * 1988-11-18 1991-08-13 Kyodo Oxygen Co., Ltd. Process for producing xenon
RU2129904C1 (ru) * 1998-04-21 1999-05-10 Савинов Михаил Юрьевич Способ получения ксенонового концентрата на воздухоразделительных установках
WO2011163342A2 (fr) * 2010-06-25 2011-12-29 Advanced Technology Materials, Inc. Récupération de xe et d'autres composés de grande valeur
RU2011127527A (ru) * 2011-07-06 2013-01-20 Виталий Леонидович Бондаренко Способ получения ксенонового концентрата из ксеноносодержащего кислорода и установка для его реализации

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5039500A (en) * 1988-11-18 1991-08-13 Kyodo Oxygen Co., Ltd. Process for producing xenon
RU2129904C1 (ru) * 1998-04-21 1999-05-10 Савинов Михаил Юрьевич Способ получения ксенонового концентрата на воздухоразделительных установках
WO2011163342A2 (fr) * 2010-06-25 2011-12-29 Advanced Technology Materials, Inc. Récupération de xe et d'autres composés de grande valeur
RU2011127527A (ru) * 2011-07-06 2013-01-20 Виталий Леонидович Бондаренко Способ получения ксенонового концентрата из ксеноносодержащего кислорода и установка для его реализации

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112129040A (zh) * 2020-09-27 2020-12-25 杭州制氧机集团股份有限公司 一种液氙冷却、氙气再液化撬装装置及其方法
CN112129040B (zh) * 2020-09-27 2024-02-20 杭氧集团股份有限公司 一种液氙冷却、氙气再液化撬装装置及其方法

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