US20170138665A1 - Cryogenic purification with heat uptake - Google Patents
Cryogenic purification with heat uptake Download PDFInfo
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- US20170138665A1 US20170138665A1 US15/318,801 US201515318801A US2017138665A1 US 20170138665 A1 US20170138665 A1 US 20170138665A1 US 201515318801 A US201515318801 A US 201515318801A US 2017138665 A1 US2017138665 A1 US 2017138665A1
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- Prior art keywords
- gas stream
- stream
- impurity
- exchanger
- adsorbers
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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
- F25J3/04006—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
- 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
- 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
Definitions
- the present invention relates to a process for purifying a feed gas stream using an adsorption unit and a cryogenic distillation unit.
- Adsorption is a phenomenon generally promoted by a low temperature.
- ASU Air Separation Unit
- the stopping of CO 2 on a molecular sieve is up to 5 times greater at ⁇ 100° C. than at 20° C., and around 3 times greater for the stopping of propane.
- the regeneration requires make-up heat which disturbs the refrigeration balance of the equipment, if the adsorption took place at a negative temperature. Its energy cost may be even greater since the temperature is low.
- the adsorption is carried out at a positive temperature and the heat for regenerating (the excess heat) is discharged to the atmosphere without impacting the refrigeration balance of the cryogenic portion.
- One solution of the present invention is a process for purifying a feed gas stream using an adsorption unit comprising at least 2 adsorbers, a cryogenic distillation unit, an exchanger and a compressor operating at a temperature below or equal to ⁇ 50° C., wherein the heat needed for the regeneration of the adsorbers is derived, at least in part, from at least one portion of the heat generated by the compressor, during the compression of a fluid.
- the process according to the invention may have one or more of the following features:
- the invention will be illustrated on an ASU with a cold compressor.
- the cold compressor introduces into the cold box a thermal gain that reheats the compressed gas.
- the natural refrigeration balance of the equipment makes it possible to manage this thermal gain.
- a portion of the hot gas will be used directly or indirectly via a heat exchange with another fluid in order to carry out the heating phase of the regeneration. This takes place with no real energy penalty, since it does not disturb (or barely disturbs) the refrigeration balance of the equipment.
- FIG. 1 represents the first alternative of the solution according to the invention.
- FIG. 2 represents the second alternative of the solution according to the invention.
- the air 1 is cooled in the exchange line 2 (for example, down to ⁇ 120° C.), then passes through a bed of adsorbent 4 at low temperature ( ⁇ 120° C.), then is reintroduced (optionally slightly hotter, due to the adsorption) into the exchange line 2 for final cooling before being sent to the distillation portion 7 .
- a portion of the residual nitrogen 9 is drawn off around ⁇ 120° C. from the exchange line, then compressed in a cold compressor 10 where it is heated up to a temperature of ⁇ 80° C. for example, then sent to a bed of adsorbent being regenerated.
- the heat provided by the compression constitutes the heat input needed for the heating phase of the regeneration.
- the nitrogen is cooled in the bed of adsorbent 4 , and is then sent at a temperature around ⁇ 120° C. to the exchange line 2 for additional reheating up to ambient temperature.
- the adsorption temperature may be preferentially close to the “natural” inlet temperature in the cold booster, that is to say the temperature dictated by the process, as though having a conventional ambient temperature purification.
- the heating phase of the regeneration does not disturb (or barely disturbs) the refrigeration balance of the equipment, this heating phase being carried out by the natural heat input provided by the cold compression. There is therefore no energy penalty in carrying out a cryogenic purification.
- a portion of the residual nitrogen is drawn off around ⁇ 120° C. from the exchange line, then passes firstly into the bed being regenerated (cooling phase), before being compressed, then sent to the exchange line for additional reheating up to ambient temperature.
- heating and cooling phase is carried out at a different pressure requiring an intermediate phase of adapting the bed to the correct pressure.
- the air 1 is partially cooled down to ⁇ 120° C., then passes through a bed of adsorbent 4 before being cold compressed 10 where it is heated up to a temperature of ⁇ 80° C., then sent back to the hotter exchange line 2 for final cooling before being sent to the distillation portion 7 .
- a portion of the residual nitrogen 9 is reheated in the exchange line 2 , up to a temperature close to that of the cold-compressed air, for example ⁇ 80° C., thus indirectly recovering the heat introduced by the compression of the air.
- the nitrogen thus reheated to ⁇ 80° C. carries out the heating phase of the regeneration by passing through a bed of adsorbent 4 where it is cooled down to ⁇ 120° C., then is sent to the exchange line 2 for additional reheating up to ambient temperature.
- the adsorption temperature may be preferentially close to the “natural” inlet temperature in the cold booster, typically around the temperature of the vaporization plateau of the oxygen, for example for the conventional single-machine layouts with cold booster (around ⁇ 120° C. for oxygen pressurized at 40 bar).
- the heating phase of the regeneration does not disturb (or barely disturbs) the refrigeration balance of the equipment, this heating phase being carried out by the natural heat input provided by the cold compression, indirectly in this case. There is therefore no energy penalty in carrying out a cryogenic purification.
- a portion of the residual nitrogen leaves the exchange line at a temperature close to the inlet of the cold compressor (around ⁇ 120° C.), passes through the adsorbent bed in order to cool it, then is sent to the exchange line for additional reheating up to ambient temperature.
- the heating and cooling phases are carried out at the same pressure.
Abstract
Description
- This application is a 371 of International PCT Application PCT/FR2016/051567, filed Jun. 12, 2015, which claims priority to French Patent Application No. 1455985, filed Jun. 26, 2014, the entire contents of which are incorporated herein by reference.
- The present invention relates to a process for purifying a feed gas stream using an adsorption unit and a cryogenic distillation unit.
- Adsorption is a phenomenon generally promoted by a low temperature. For example, for an ASU (Air Separation Unit), the stopping of CO2 on a molecular sieve is up to 5 times greater at −100° C. than at 20° C., and around 3 times greater for the stopping of propane.
- The regeneration requires make-up heat which disturbs the refrigeration balance of the equipment, if the adsorption took place at a negative temperature. Its energy cost may be even greater since the temperature is low.
- In the processes according to the prior art, the adsorption is carried out at a positive temperature and the heat for regenerating (the excess heat) is discharged to the atmosphere without impacting the refrigeration balance of the cryogenic portion.
- Starting from there, one problem that is faced is that of providing a cryogenic purification in a cryogenic separation process that already knows how to manage, when it comes to the refrigeration balance, a heat gain at least equal to that needed for the regeneration of the adsorbers.
- One solution of the present invention is a process for purifying a feed gas stream using an adsorption unit comprising at least 2 adsorbers, a cryogenic distillation unit, an exchanger and a compressor operating at a temperature below or equal to −50° C., wherein the heat needed for the regeneration of the adsorbers is derived, at least in part, from at least one portion of the heat generated by the compressor, during the compression of a fluid.
- Depending on the case, the process according to the invention may have one or more of the following features:
-
- said process comprises an adsorption step implemented by the adsorption unit, with the adsorption step performed at a negative temperature;
- said process comprises, according to a first alternative, the following successive steps (
FIG. 1 ): - a) the
feed gas stream 1 is cooled in theexchanger 2 to a temperature below −50° C., preferably below −100° C.; - b) the cooled
gas stream 3 is sent to theadsorption unit 4 where at least one impurity X is at least partly adsorbed so as to recover agas stream 5 depleted in impurity X; - c) the gas stream depleted in
impurity X 5 is introduced into theexchanger 2 in order to be cooled to a temperature below −50° C., preferably below −150° C.; - d) the
gas stream 5 depleted in impurity X and cooled is sent to thecryogenic distillation unit 7 where it is separated into at least 2streams - e) a portion of the
stream 9 is introduced into the exchanger in order to be reheated to a temperature above −150° C., preferably above −100° C., more preferentially above −50° C., ideally to a temperature close to that of thefeed gas stream 1 at the end of step a) before being compressed in thecompressor 10 with a compression ratio greater than 1.2; - f) the
compressed stream 9 is sent to theadsorption unit 4 in order to regenerate one of the two adsorbers;
with the compression in step e) leading to a temperature increase of thestream 9 of at least 20° C. and thus providing the heat input needed for the regeneration of at least one of the adsorbers; - said process comprises, according to a second alternative, the following successive steps (
FIG. 2 ): - a) the
feed gas stream 1 is cooled in theexchanger 2 to a temperature below −50° C., preferably below −100° C.; - b) the cooled
gas stream 3 is sent to theadsorption unit 4 where at least one impurity X is at least partly adsorbed so as to recover a first stream depleted inimpurity X 5; - c) the
gas stream 5 depleted in impurity X is compressed in thecompressor 10 with a compression ratio greater than 1.2 before being cooled in theexchanger 2 to a temperature below −50° C., preferably below −150° C.; - d) the
gas stream 5 depleted in impurity X, compressed and cooled is sent to thecryogenic distillation unit 7 where it is separated into at least 2streams - e) a portion of the
stream 9 is introduced into the exchanger in order to be reheated to a temperature above −150° C., preferably above −100° C., more preferentially above −50° C., ideally to a temperature close to that of thefeed gas stream 5 at the end of the compression of step c); - f) the reheated
stream 9 is sent to theadsorption unit 4 in order to regenerate at least one of the two adsorbers;
with the compression in step c) leading to a temperature increase of thegas stream 5 depleted in impurity X of at least 20° C. and thus providing, indirectly via theexchanger 2, the heat input needed for the reheating of a portion of thestream 9 and therefore for the regeneration of at least one of the two adsorbers in step f); - the adsorbers comprise a monobed, preferably a molecular sieve;
- the feed gas stream is air and the impurity X is selected from H2O, CO2, N2O, CnHm, NOx;
- the feed gas stream comprises water and said process comprises, before step a), a step of pre-purification of the feed gas stream that makes it possible to eliminate at least one portion of the water;
- the pre-purification step is carried out by adsorption at ambient temperature;
- the adsorption of the pre-purification step is carried out on a monobed of alumina, silica gel or molecular sieve type.
- The invention will be illustrated on an ASU with a cold compressor. The cold compressor introduces into the cold box a thermal gain that reheats the compressed gas. The natural refrigeration balance of the equipment makes it possible to manage this thermal gain. A portion of the hot gas will be used directly or indirectly via a heat exchange with another fluid in order to carry out the heating phase of the regeneration. This takes place with no real energy penalty, since it does not disturb (or barely disturbs) the refrigeration balance of the equipment.
- For a further understanding of the nature and objects for the present invention, reference should be made to the following detailed description, taken in conjunction with the accompanying drawings, in which like elements are given the same or analogous reference numbers and wherein:
-
FIG. 1 represents the first alternative of the solution according to the invention. -
FIG. 2 represents the second alternative of the solution according to the invention. - The
air 1 is cooled in the exchange line 2 (for example, down to −120° C.), then passes through a bed of adsorbent 4 at low temperature (−120° C.), then is reintroduced (optionally slightly hotter, due to the adsorption) into theexchange line 2 for final cooling before being sent to thedistillation portion 7. - A portion of the
residual nitrogen 9 is drawn off around −120° C. from the exchange line, then compressed in acold compressor 10 where it is heated up to a temperature of −80° C. for example, then sent to a bed of adsorbent being regenerated. The heat provided by the compression constitutes the heat input needed for the heating phase of the regeneration. The nitrogen is cooled in the bed of adsorbent 4, and is then sent at a temperature around −120° C. to theexchange line 2 for additional reheating up to ambient temperature. - The adsorption temperature may be preferentially close to the “natural” inlet temperature in the cold booster, that is to say the temperature dictated by the process, as though having a conventional ambient temperature purification.
- It is seen that the heating phase of the regeneration does not disturb (or barely disturbs) the refrigeration balance of the equipment, this heating phase being carried out by the natural heat input provided by the cold compression. There is therefore no energy penalty in carrying out a cryogenic purification.
- Regarding the cooling phase of the regeneration of the process according to the first alternative, a portion of the residual nitrogen is drawn off around −120° C. from the exchange line, then passes firstly into the bed being regenerated (cooling phase), before being compressed, then sent to the exchange line for additional reheating up to ambient temperature.
- It is observed that the heating and cooling phase is carried out at a different pressure requiring an intermediate phase of adapting the bed to the correct pressure.
- The
air 1 is partially cooled down to −120° C., then passes through a bed of adsorbent 4 before being cold compressed 10 where it is heated up to a temperature of −80° C., then sent back to thehotter exchange line 2 for final cooling before being sent to thedistillation portion 7. A portion of theresidual nitrogen 9 is reheated in theexchange line 2, up to a temperature close to that of the cold-compressed air, for example −80° C., thus indirectly recovering the heat introduced by the compression of the air. The nitrogen thus reheated to −80° C. carries out the heating phase of the regeneration by passing through a bed of adsorbent 4 where it is cooled down to −120° C., then is sent to theexchange line 2 for additional reheating up to ambient temperature. - The adsorption temperature may be preferentially close to the “natural” inlet temperature in the cold booster, typically around the temperature of the vaporization plateau of the oxygen, for example for the conventional single-machine layouts with cold booster (around −120° C. for oxygen pressurized at 40 bar).
- Again, it is seen that the heating phase of the regeneration does not disturb (or barely disturbs) the refrigeration balance of the equipment, this heating phase being carried out by the natural heat input provided by the cold compression, indirectly in this case. There is therefore no energy penalty in carrying out a cryogenic purification.
- Regarding the cooling phase of the regeneration of the process according to the second alternative, a portion of the residual nitrogen leaves the exchange line at a temperature close to the inlet of the cold compressor (around −120° C.), passes through the adsorbent bed in order to cool it, then is sent to the exchange line for additional reheating up to ambient temperature. In this case, the heating and cooling phases are carried out at the same pressure.
- It will be understood that many additional changes in the details, materials, steps and arrangement of parts, which have been herein described in order to explain the nature of the invention, may be made by those skilled in the art within the principle and scope of the invention as expressed in the appended claims. Thus, the present invention is not intended to be limited to the specific embodiments in the examples given above.
Claims (9)
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 |
Publications (1)
Publication Number | Publication Date |
---|---|
US20170138665A1 true US20170138665A1 (en) | 2017-05-18 |
Family
ID=51519043
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US15/318,801 Abandoned US20170138665A1 (en) | 2014-06-26 | 2015-06-12 | Cryogenic purification with heat uptake |
Country Status (5)
Country | Link |
---|---|
US (1) | US20170138665A1 (en) |
EP (1) | EP3161399B1 (en) |
CN (1) | CN106461323B (en) |
FR (1) | FR3022993A1 (en) |
WO (1) | WO2015197940A1 (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3236059A (en) * | 1962-08-29 | 1966-02-22 | Air Prod & Chem | Separation of gaseous mixtures |
US4746332A (en) * | 1985-09-27 | 1988-05-24 | Hitachi, Ltd. | Process for producing high purity nitrogen |
EP0590946A1 (en) * | 1992-10-01 | 1994-04-06 | The Boc Group, Inc. | Production of nitrogen |
Family Cites Families (5)
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 |
FR2766735B1 (en) * | 1997-07-31 | 1999-09-03 | Air Liquide | PROCESS AND DEVICE FOR THE PRODUCTION OF ULTRA-PUR INERT GAS |
CN100363699C (en) * | 2005-04-25 | 2008-01-23 | 林福粦 | Air separation system for recycling cold energy of liquified natural gas |
JP5005894B2 (en) * | 2005-06-23 | 2012-08-22 | エア・ウォーター株式会社 | Nitrogen generation method and apparatus used therefor |
CN201265997Y (en) * | 2008-09-05 | 2009-07-01 | 苏州制氧机有限责任公司 | Liquid air separation plant |
-
2014
- 2014-06-26 FR FR1455985A patent/FR3022993A1/en active Pending
-
2015
- 2015-06-12 US US15/318,801 patent/US20170138665A1/en not_active Abandoned
- 2015-06-12 EP EP15733826.0A patent/EP3161399B1/en active Active
- 2015-06-12 CN CN201580033220.7A patent/CN106461323B/en active Active
- 2015-06-12 WO PCT/FR2015/051567 patent/WO2015197940A1/en active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3236059A (en) * | 1962-08-29 | 1966-02-22 | Air Prod & Chem | Separation of gaseous mixtures |
US4746332A (en) * | 1985-09-27 | 1988-05-24 | Hitachi, Ltd. | Process for producing high purity nitrogen |
EP0590946A1 (en) * | 1992-10-01 | 1994-04-06 | The Boc Group, Inc. | Production of nitrogen |
Also Published As
Publication number | Publication date |
---|---|
FR3022993A1 (en) | 2016-01-01 |
EP3161399A1 (en) | 2017-05-03 |
EP3161399B1 (en) | 2018-08-15 |
CN106461323A (en) | 2017-02-22 |
WO2015197940A1 (en) | 2015-12-30 |
CN106461323B (en) | 2019-08-06 |
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