CN106461323B - Cryogenic purincation method with heat absorption - Google Patents

Cryogenic purincation method with heat absorption Download PDF

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Publication number
CN106461323B
CN106461323B CN201580033220.7A CN201580033220A CN106461323B CN 106461323 B CN106461323 B CN 106461323B CN 201580033220 A CN201580033220 A CN 201580033220A CN 106461323 B CN106461323 B CN 106461323B
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air
temperature
flow
exchanger
impurity
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CN106461323A (en
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伯诺瓦·达维迪安
伯纳德·索尼耶
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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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
    • F25J3/04—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 for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04242—Cold end purification of the feed air
    • 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
    • F25J3/04—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 for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/04054—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of air
    • 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
    • F25J3/04—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 for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/0406—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of nitrogen
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • F25J2205/70—Heating the adsorption vessel

Abstract

A method of carrying out purified gases feeding flow in the at a temperature of absorbing unit for containing at least two absorber, cryogenic distillation unit, exchanger and the compressor that run less than or equal to -50 DEG C for using, wherein being at least part for being at least partly originated from the heat generated in the compression process of fluid by the compressor for heat needed for regenerating these absorbers.

Description

Cryogenic purincation method with heat absorption
Technical field
The present invention relates to a kind of methods for purifying feed stream using absorbing unit and cryogenic distillation unit.
Background technique
Absorption is the phenomenon that generally promotion by low temperature.For example, for ASU (air separation equipment), CO2In molecular sieve On stop at it is up to 5 times bigger than at 20 DEG C and about 3 times or so bigger than the stopping for propane at -100 DEG C.
Regeneration requires supplementation with heat, which has upset the freezing balance of equipment, if absorption occurs in negative temperature Under talking about.Its energy cost may be even more big, because temperature is low.
It in method according to prior art, is adsorbed at positive temperature and carries out, and be used for regenerated heat (extra heat Amount) it is discharged into atmosphere, the freezing without will affect the low temperature part balances.
From there, suffering from a problem that is that cryogenic purincation is provided in low temperature separating methods, the cryogenic separation side Method already knows how to manage the thermal enhancement required for the regeneration at least equal to these absorbers when it reaches freezing balance.
Summary of the invention
A solution of the invention be it is a kind of for use less than or equal to -50 DEG C at a temperature of run include Absorbing unit, cryogenic distillation unit, exchanger and the compressor of at least two absorber are come the method that purifies feed stream, wherein It is at least partly to be originated to be generated in the compression process of fluid by the compressor for heat needed for regenerating these absorbers Heat at least part.
It depends on the circumstances, can have according to the method for the present invention one or more in following characteristics:
The adsorption step that the method includes being implemented by the absorbing unit, wherein the adsorption step under negative temperature into Row；
The method includes, according to the first alternative solution, following consecutive steps (Fig. 1):
A) feed stream 1 is cooled to the temperature lower than -50 DEG C, preferably shorter than -100 DEG C in exchanger 2；
B) cooling air-flow 3 being sent in absorbing unit 4, at least one impurity X is at least partly adsorbed herein, with Just the air-flow 5 of poor impurity X is recycled；
C) air-flow 5 of poor impurity X is introduced into exchanger 2 to be cool below -50 DEG C, preferably shorter than -150 DEG C Temperature；
D) by the poor impurity X and cooled air-flow 5 is sent in cryogenic distillation unit 7, the air-flow is separated herein At at least two stream 8 and 9；
E) a part for flowing 9 is introduced into the exchanger so as to be heated to be higher than -150 DEG C, preferably higher than -100 DEG C, More preferably higher than -50 DEG C of temperature ideally arrives the temperature close to the temperature of feed stream 1 at the end of step a),
It is compressed later in compressor 10 with the compression ratio greater than 1.2；
F) compression stream 9 is sent in absorbing unit 4, to regenerate one of the two absorbers；
Wherein the compression in step e) causes at least 20 DEG C of temperature of stream 9 to rise, and regenerates these to provide Heat input needed at least one of absorber；
The method includes, according to the second alternative solution, following consecutive steps (Fig. 2):
A) feed stream 1 is cooled to the temperature lower than -50 DEG C, preferably shorter than -100 DEG C in exchanger 2；
B) cooling air-flow 3 being sent in absorbing unit 4, at least one impurity X is at least partly adsorbed herein, with Just first-class the 5 of poor impurity X are recycled；
C) air-flow 5 of poor impurity X is compressed in compressor 10 with the compression ratio greater than 1.2, later in exchanger 2 In be cooled to lower than -50 DEG C, preferably shorter than -150 DEG C of temperature；
D) by the poor impurity X, compressed and cooled air-flow 5 is sent in cryogenic distillation unit 7, herein should Air-flow is separated at least two stream 8 and 9；
E) a part for flowing 9 is introduced into the exchanger so as to be heated to be higher than -150 DEG C, preferably higher than -100 DEG C, More preferably higher than -50 DEG C of temperature ideally arrives the temperature close to the temperature of feed stream 5 at the end of compression step c),
F) stream of reheating 9 is sent in absorbing unit 4, to regenerate at least one of the two absorbers；
Wherein the compression in step c) causes at least 20 DEG C of temperature of the air-flow 5 of poor impurity X to rise, and between Ground connection provides a part of required of reheating stream 9 via exchanger 2 and therefore regenerates the two absorbers in step f) At least one of needed for heat input；
These absorbers include single, preferred molecular sieve；
The feed stream is air, and impurity X is selected from H2O、CO2、N2O、CnHm, NOx；
The feed stream includes water and the method includes before step a), by the step of the feed stream prepurification Suddenly, which makes it possible to eliminate at least part of the water.
The prepurification step is by adsorbing progress at ambient temperature；
The absorption of the prepurification step is the single upper progress in aluminium oxide, silica gel or molecular sieve type.
The present invention will be illustrated on the ASU with cold compressor.The cold compressor will reheat the heat of compressed gas Gain is introduced into ice chest.The natural freezing balance of the equipment makes it possible to manage the thermal enhancement.A part of hot gas will Via with another fluid heat exchange and by direct or indirect use to carry out the regenerated heating period.This is occurred without really Energy loss because it does not interfere the freezing balance of (or the hardly interfere) equipment.
Detailed description of the invention
Fig. 1 shows the first alternative solution according to the solution of the present invention.
Fig. 2 shows the second alternative solutions according to the solution of the present invention.
Specific embodiment
Fig. 1 shows the first alternative solutions according to the solution of the present invention.
By air 1 in exchange pipeline 2 cooling (for example, down to -120 DEG C), then pass through under low temperature (- 120 DEG C) Then the bed of adsorbent 4 is reintroduced back to (optionally slightly hot, due to absorption) and is finally cooled down into exchange pipeline 2, is sent to later In distillation fraction 7.
By a part of remaining nitrogen 9, about -120 DEG C of extractions from the exchange pipeline, then compress in cold compressor 10, It is heated to such as -80 DEG C of temperature herein, is then delivered in the adsorbent bed being reproduced.The heat structure provided by compression At heat input needed for the regenerated heating period.The nitrogen is cooling in the bed of adsorbent 4, then in about -120 DEG C of temperature It is sent under degree to exchange pipeline 2 to be additionally again heated to environment temperature.
Adsorption temp can be determined preferentially close to " natural " inlet temperature in cold booster by this method Temperature, as have conventional environment temperature purifying.
As can be seen that the regenerated heating period does not interfere the freezing balance of (or the hardly interfering) equipment, the heating Stage is carried out by the natural heat input provided by cold compression.Therefore, energy loss is not present in carrying out cryogenic purincation.
About in the regenerated cooling stage according to the method for first alternative solution, by a part of remaining nitrogen from this About -120 DEG C of extractions in pipeline are exchanged, (cooling stage) is then initially entered in the bed being reproduced, is compressed later, then sent Into the exchange pipeline to be additionally again heated to environment temperature.
Observe that the heating and cooling stage carry out at various pressures, it is desirable that this bed is made to adapt to the centre of correct pressure Stage.
Fig. 2 indicates the second alternative solution according to the solution of the present invention.
1 part of air is cooled to -120 DEG C, then passes through the bed of adsorbent 4, later cold compression 10, herein by the sky Gas is heated to -80 DEG C of temperature, is then returned to more heat exchange pipeline 2 and is finally cooled down, is sent in distillation fraction 7 later.
A part of remaining nitrogen 9 is reheated in exchange pipeline 2, up to the temperature close to cold compression air themperature Degree, such as -80 DEG C, to recycle the heat introduced by the compression of air indirectly.Thus -80 DEG C of nitrogen is heated to pass through Bed across adsorbent 4 carries out the regenerated heating period, and the nitrogen is cooled to -120 DEG C in the adsorbent bed, is then delivered to It exchanges in pipeline 2 to be additionally again heated to environment temperature.
Adsorption temp can be preferentially close to " natural " inlet temperature in cold booster, the typically about steaming of oxygen The temperature of platform (plateau) is sent out, such as conventional single machine layout with cold booster (for pressurizeing at 40bar Oxygen be about -120 DEG C).
Again it is seen that the regenerated heating period does not interfere the freezing balance of (or the hardly interfering) equipment, it should Heating period is carried out by the natural heat input provided by cold compression (in this case indirectly).Therefore, it is carrying out Energy loss is not present in cryogenic purincation.
About the regenerated cooling stage according to the method for second alternative solution, by a part of remaining nitrogen close The exchange pipeline is left at the temperature (about -120 DEG C) of the entrance of cold compressor, across adsorbent bed to be cooled to, so After be sent in the exchange pipeline to be additionally again heated to environment temperature.In this case, heating and cooling stage are in identical pressure It is carried out under power.

Claims (9)

1. it is a kind of for use less than or equal to -50 DEG C at a temperature of run the absorbing unit comprising at least two absorber, Cryogenic distillation unit, exchanger and compressor are come the method that purifies feed stream, wherein for regenerating needed for these absorbers Heat is at least partly to be originated from at least part of heat generated in the compression process of fluid by the compressor, and institute The method of stating includes the adsorption step implemented by the absorbing unit, and wherein the adsorption step carries out under negative temperature.
2. the method as described in claim 1, which is characterized in that the method includes following consecutive steps:
The feed stream (1) a) is cooled to the temperature lower than -50 DEG C in exchanger (2)；
B) air-flow of the cooling (3) is sent in the absorbing unit (4), at least one impurity X is at least partly inhaled herein It is attached, to recycle the air-flow (5) of poor impurity X；
C) air-flow (5) of the poor impurity X is introduced into and is cool below -50 DEG C of temperature in the exchanger (2)；
D) by the poor impurity X and cooled air-flow (5) is sent in the cryogenic distillation unit (7), herein by the air-flow point From at least first-class (8) and second (9)；
E) a part of the second (9) is introduced into be heated to the temperature for being higher than -150 DEG C in the exchanger, later It is compressed in compressor (10) with the compression ratio greater than 1.2；
F) compressed second (9) is sent in the absorbing unit (4), to regenerate one of the two absorbers；
Wherein the compression in step e) causes at least 20 DEG C of temperature of the second (9) to rise, and to provide regeneration Heat input needed at least one of these absorbers.
3. the method as described in claim 1, which is characterized in that the method includes following consecutive steps:
The feed stream (1) a) is cooled to the temperature lower than -50 DEG C in exchanger (2)；
B) air-flow of the cooling (3) is sent in the absorbing unit (4), at least one impurity X is at least partly inhaled herein It is attached, to recycle the air-flow (5) of poor impurity X；
C) air-flow (5) of the poor impurity X is compressed in the compressor (10) with the compression ratio greater than 1.2, later at this The temperature lower than -50 DEG C is cooled in exchanger (2)；
D) by the poor impurity X, compressed and cooled air-flow (5) is sent in the cryogenic distillation unit (7), herein should Air-flow is separated at least first-class (8) and second (9)；
E) a part of the second (9) is introduced into the exchanger to be heated to the temperature for being higher than -150 DEG C；
F) second of the reheating (9) is sent in the absorbing unit (4), to regenerate at least one in the two absorbers It is a；
Wherein the compression in step c) causes 20 DEG C of temperature of the air-flow (5) of the poor impurity X to rise, and to indirectly There is provided via the exchanger (2) reheat the second (9) a part of required and therefore in step f) regeneration this two Heat input needed at least one of a absorber.
4. the method as described in one of claims 1 to 3, which is characterized in that these absorbers include single.
5. method as claimed in claim 4, which is characterized in that these absorbers include molecular sieve.
6. method as claimed in claim 2 or claim 3, which is characterized in that the feed stream is air, and impurity X is selected from H2O、 CO2、N2O、CnHm、NOx。
7. method as claimed in claim 2 or claim 3, which is characterized in that the feed stream include water and the method includes, Before step a), the step of by the feed stream prepurification, which makes it possible to eliminate at least one of the water Point.
8. the method for claim 7, which is characterized in that the prepurification step is carried out by adsorbing at ambient temperature 's.
9. method according to claim 8, which is characterized in that the absorption of the prepurification step is in aluminium oxide, silica gel or to divide Single upper progress of son sieve type.
CN201580033220.7A 2014-06-26 2015-06-12 Cryogenic purincation method with heat absorption Active CN106461323B (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR1455985 2014-06-26
FR1455985A FR3022993A1 (en) 2014-06-26 2014-06-26 CRYOGENIC CLEANING WITH HEAT INPUT
PCT/FR2015/051567 WO2015197940A1 (en) 2014-06-26 2015-06-12 Cryogenic purification with heat uptake

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CN106461323A CN106461323A (en) 2017-02-22
CN106461323B true CN106461323B (en) 2019-08-06

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US (1) US20170138665A1 (en)
EP (1) EP3161399B1 (en)
CN (1) CN106461323B (en)
FR (1) FR3022993A1 (en)
WO (1) WO2015197940A1 (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4746332A (en) * 1985-09-27 1988-05-24 Hitachi, Ltd. Process for producing high purity nitrogen
EP0894522A1 (en) * 1997-07-31 1999-02-03 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and apparatus for the production of ultra-pure inert gas
CN101198834A (en) * 2005-06-23 2008-06-11 空气及水株式会社 Nitrogen generating device and apparatus for use therefor
CN201265997Y (en) * 2008-09-05 2009-07-01 苏州制氧机有限责任公司 Liquid air separation plant

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1189094B (en) * 1962-06-09 1965-03-18 Linde Eismasch Ag Process for removing carbon dioxide from gas mixtures
US3236059A (en) * 1962-08-29 1966-02-22 Air Prod & Chem Separation of gaseous mixtures
US5551257A (en) * 1992-10-01 1996-09-03 The Boc Group, Inc. Production of ultrahigh purity nitrogen
CN100363699C (en) * 2005-04-25 2008-01-23 林福粦 Air separation system for recycling cold energy of liquified natural gas

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4746332A (en) * 1985-09-27 1988-05-24 Hitachi, Ltd. Process for producing high purity nitrogen
EP0894522A1 (en) * 1997-07-31 1999-02-03 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and apparatus for the production of ultra-pure inert gas
CN101198834A (en) * 2005-06-23 2008-06-11 空气及水株式会社 Nitrogen generating device and apparatus for use therefor
CN201265997Y (en) * 2008-09-05 2009-07-01 苏州制氧机有限责任公司 Liquid air separation plant

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Publication number Publication date
CN106461323A (en) 2017-02-22
EP3161399B1 (en) 2018-08-15
WO2015197940A1 (en) 2015-12-30
FR3022993A1 (en) 2016-01-01
US20170138665A1 (en) 2017-05-18
EP3161399A1 (en) 2017-05-03

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