CN113184850A - Method and device for purifying high-purity carbon dioxide gas - Google Patents
Method and device for purifying high-purity carbon dioxide gas Download PDFInfo
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- CN113184850A CN113184850A CN202110531940.3A CN202110531940A CN113184850A CN 113184850 A CN113184850 A CN 113184850A CN 202110531940 A CN202110531940 A CN 202110531940A CN 113184850 A CN113184850 A CN 113184850A
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 235
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 121
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 116
- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000007789 gas Substances 0.000 claims abstract description 248
- 238000001179 sorption measurement Methods 0.000 claims abstract description 161
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910001868 water Inorganic materials 0.000 claims abstract description 42
- 239000003463 adsorbent Substances 0.000 claims abstract description 37
- 238000000926 separation method Methods 0.000 claims abstract description 30
- 239000002912 waste gas Substances 0.000 claims abstract description 28
- 238000005057 refrigeration Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 230000007246 mechanism Effects 0.000 claims abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 230000008569 process Effects 0.000 claims description 32
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 20
- 239000001301 oxygen Substances 0.000 claims description 20
- 229910052760 oxygen Inorganic materials 0.000 claims description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims description 17
- 238000000746 purification Methods 0.000 claims description 17
- 239000003507 refrigerant Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 12
- 238000003795 desorption Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 9
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 7
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- 239000012530 fluid Substances 0.000 claims description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 5
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- 239000000741 silica gel Substances 0.000 claims description 5
- 229910002027 silica gel Inorganic materials 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 230000003139 buffering effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
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- 230000001172 regenerating effect Effects 0.000 claims 1
- 239000000047 product Substances 0.000 description 42
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000012071 phase Substances 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
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- 238000002485 combustion reaction Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
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- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
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- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/50—Carbon dioxide
-
- 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
- B01D53/047—Pressure swing adsorption
- B01D53/053—Pressure swing adsorption with storage or buffer vessel
-
- 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
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
-
- 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
- C01B2210/0046—Nitrogen
-
- 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
- C01B2210/0062—Water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Abstract
The invention belongs to the technical field of gas separation, and particularly relates to a method and a device for purifying high-purity carbon dioxide gas. The invention adopts the pressure swing adsorption technology of the carbon dioxide adsorbent with the equilibrium adsorption mechanism, obtains high-purity carbon dioxide from an adsorption phase under lower pressure, and couples pressurization, refrigeration, water removal and carbon dioxide liquefaction to obtain high-purity liquid carbon dioxide as product gas; wherein, the gas phase component in the bed layer is replaced by the recycle feeding carbon dioxide product gas, so as to obtain the mixed gas of carbon dioxide and water vapor with higher purity; a gas recovery loop is designed between two or more groups of beds which run symmetrically, and a part of waste gas generated in the adsorption separation process flows back to the symmetric separation beds so as to improve the recovery rate of the system; a portion of the product gas will be refluxed to the feed end of the adsorbent bed to displace the impure gas in the gas phase. The method can purify the mixed gas containing about 15% of carbon dioxide to obtain 60-99.9% of carbon dioxide gas.
Description
Technical Field
The invention belongs to the technical field of gas separation, and particularly relates to a method and a device for purifying low-partial-pressure carbon dioxide mixed gas.
Background
Pressure Swing Adsorption (PSA) is an important and widely used gas separation process, such as pressure swing adsorption drying, pressure swing adsorption oxygen production, nitrogen production, etc., and generally, different adsorbents are used to separate different mixed gases to obtain desired components based on pressure swing adsorption with equilibrium adsorption or kinetic separation characteristics.
Carbon dioxide (CO)2) Is the main greenhouse gas, CO, responsible for global climate change2The capture, utilization and sequestration of (a) has become one of the hot issues of international social concern. The industrial fields of steel making, cement, chemical industry (such as ammonia synthesis, hydrogen production, natural gas purification) and the like all have a large amount of CO2And (5) discharging. At present, China generates CO in flue gas generated by combustion2The recovery measure is to use chemical absorption and temperature-changing regeneration method to recover CO in flue gas2Separating, and compressing, liquefying, and refining to obtain industrial grade or food grade CO2The product, the system technology is complicated, the investment is large, the equipment occupies a large area, especially a miniaturized system, and no simple, feasible and effective solution is provided.
Disclosure of Invention
In view of the above situation, the present invention provides a method and an apparatus for obtaining high purity carbon dioxide by removing nitrogen, oxygen and moisture in flue gas generated in a combustion chemical reaction process, wherein the background gas usually contains nitrogen, oxygen and moisture, and is a carbon dioxide mixed gas containing nitrogen, oxygen and moisture.
The invention provides a purification method of high-purity carbon dioxide, which adopts a pressure swing adsorption technology of a carbon dioxide adsorbent based on a balanced adsorption mechanism, obtains high-purity carbon dioxide from an adsorption phase under lower pressure, and couples pressurization, refrigeration, water removal and carbon dioxide liquefaction to obtain high-purity liquid carbon dioxide as product gas, wherein:
the pressure swing adsorption technology based on the equilibrium adsorption mechanism is characterized in that a carbon dioxide adsorbent is filled in an adsorption bed layer, the adsorbent has stronger adsorption capacity on moisture and carbon dioxide in raw material gas relative to nitrogen and oxygen components, and high-purity carbon dioxide and water vapor mixed gas is obtained through desorption after the adsorption saturation of the bed layer;
in addition, the gas phase component in the bed layer is replaced by the carbon dioxide product gas with higher purity through circulating feeding, and the mixed gas of the carbon dioxide and the water vapor with higher purity can be obtained through desorption after the adsorption saturation of the bed layer;
in addition, in the invention, a gas recovery loop is designed between two or more groups of beds which run symmetrically, so that the loss of target gas is reduced to the maximum extent, and the recovery rate is improved;
in addition, in the invention, at least one part of the waste gas generated in the adsorption and separation process flows back to the symmetrical separation bed layer, which is beneficial to the boosting process of the symmetrical separation bed layer and the reduction of the power consumption in the desorption process, and improves the recovery rate of the system;
also, in the present invention, at least a portion of the product gas will be refluxed to the feed end of the adsorbent bed to displace impure gas in the gas phase;
in addition, by adopting the purification process, the purity of 60-99.9% of carbon dioxide is preferably obtained by purification from the carbon dioxide mixed gas containing about 15% of typical flue gas, and the purity of 60-85% of carbon dioxide is more preferably obtained;
in addition, in the invention, the subsequent coupled product carbon dioxide gas pressurization process adopts two-stage refrigeration to respectively achieve the purposes of removing water and liquefying carbon dioxide, wherein the water in the product carbon dioxide gas is preferably removed by the first-stage refrigeration (typically, a freeze dryer) under the pressure of 3-7.5 MPa so as to achieve the process purpose of normal pressure dew point of-65 ℃, which is different from the traditional technology that the dehydration process of firstly carrying out raw material gas at the front end is combined with the pressure boosting process required by carbon dioxide to remove water at the station;
in addition, in the invention, in the subsequent pressurization process of the coupled product carbon dioxide gas, two-stage refrigeration is adopted to respectively achieve the purposes of removing water and liquefying carbon dioxide, wherein the process purpose of liquefying the mixed gas with the purity of 60-85% of carbon dioxide obtained by a purification system is preferably carried out under the conditions of 1-15 ℃ and 3-7.5 MPa by secondary refrigeration (typically, refrigerant water heat exchange) under the pressure of 3-7.5 MPa, and the non-condensable gas is discharged out of the system.
Based on the method, the device for purifying the high-purity carbon dioxide provided by the invention comprises the following steps:
(1) at least one compression device for providing necessary raw gas with pressure, preferably but not necessarily comprising a device (not shown in the figure) required for pretreatment, for example, the mixed gas of carbon dioxide containing oxygen, nitrogen and water has the pressure of 15-100 kpa (gauge pressure) and does not need to be matched;
(2) at least one set of pressure swing adsorption device in the known technology, which at least comprises an adsorption tower, wherein a carbon dioxide adsorbent is arranged in the adsorption tower; typically, 13X or other modified regenerable carbon dioxide sorbents with equilibrium adsorption characteristics are used. One or more of molecular sieves for adsorbing water, such as activated alumina, silica gel and the like, can be compositely filled at the gas inlet end of the raw gas to remove impurity gases, such as water, total hydrocarbon and the like, contained in the mixed gas; the system also comprises an air inlet valve for raw material gas to enter each adsorption tower and a necessary connecting pipeline thereof, an exhaust valve for waste gas to enter the waste gas buffer tank and a necessary connecting pipeline thereof, and a gas production valve for product gas to enter the product gas buffer tank and a necessary connecting pipeline thereof; control valves for fluid exchange between symmetrically operating towers and necessary pipelines thereof for regulating and cutting off gas flow between the adsorption towers; the product gas enters the gas inlet valve of each adsorption tower and necessary pipelines thereof;
(3) at least one waste gas buffer tank connected with the exhaust end of each separator through a control valve and a necessary connecting pipeline for receiving waste gas from the separator and sending the temporarily stored waste gas into the separator which is in the process of pre-charging at the exhaust end of the separator;
(4) at least one product gas buffer tank, which is connected with the feed end of each separator through a control valve and a necessary connecting pipeline thereof by a desorption vacuum pump, is used for receiving the product gas from the separator, and sending the product gas in the product buffer tank into the gas inlet end of the separator through the control valve and the necessary connecting pipeline thereof to repressurize the separator which is in the adsorption process;
(5) at least one product gas booster for boosting the product gas in the product gas buffer tank to a predetermined pressure;
(6) at least one refrigerant heat exchanger and a filter, the gas is cooled, the moisture in the gas is condensed into liquid state, and the liquid state is removed through the filter and discharged out of the system;
(7) the at least one heat exchanger is used for cooling the carbon dioxide mixed gas from which the moisture is removed to a liquefaction triple point of the mixed gas, liquefying the carbon dioxide in the mixed gas as a product and outputting the product, and discharging the non-condensable gas out of the system;
(8) and the complete set of control components is used for carrying out necessary operation control on the valves on the loop and carrying out necessary control operation on equipment such as compression equipment, a vacuum pump, refrigeration equipment, a heat exchanger and the like.
The invention can be used for separating gas which is not easy to be adsorbed, component which is easy to be adsorbed/permeated or component which is difficult to be adsorbed/permeated from gas which is difficult to be adsorbed/permeated by adopting one or more adsorbents, and the components can be used as required product gas independently or simultaneously. The present invention is preferably applied to PSA processes based on equilibrium adsorption theory rather than kinetic separation theory, but it is not excluded that PSA processes based on kinetic separation theory may employ the present invention for the purposes of the present invention. The basic principles disclosed can be applied to many other separation applications. Typical examples of separations that can be achieved by the present invention include:
by selective adsorption of N2To recover N from air2；
By selective adsorption of O2For recovering O from the air2；
Enriching CO from the carbon monoxide mixed gas by using an adsorbing material for selectively adsorbing CO;
by selective adsorption of CO2For enriching CO from carbon dioxide gas mixture2；
Realization of CO2/CH4Separation of, CO2/N2Separation of (A) from (B), H2/N2Separation of olefins/alkanes, etc.
From containing O2Separation of O from a gas mixture of Ar (e.g. obtained by separation of air by pressure swing adsorption coupled membrane separation)2Or Ar;
any combination of one or more suitable adsorbents may also be used for separation, for example, CaA zeolite, LiX zeolite, or any other specific separation material to recover oxygen or nitrogen; gases that are difficult to adsorb/permeate are enriched from the non-feed end while components that are more readily selectively adsorbed/permeate are enriched from the other end.
In the present invention, the product gas refers to a gas that is difficult to be adsorbed by the adsorbent, for example, nitrogen is easy to be adsorbed by the nitrogen adsorbent, oxygen and argon are difficult to be adsorbed by the nitrogen adsorbent, oxygen is easy to be adsorbed by the oxygen adsorbent, and argon is difficult to be adsorbed by the argon adsorbent.
In the present invention, the exhaust gas refers to a gas which is relatively easily adsorbed by an adsorbent with respect to a product gas, and for example, nitrogen, oxygen, and the like are relatively easily adsorbed by a nitrogen adsorbent and an oxygen adsorbent with respect to argon.
In the present invention, the adsorbent, also called molecular sieve, is used for pressure swing adsorption of dried molecular sieves such as 13X, activated alumina, silica gel, etc., and conventional PSA processes for producing oxygen from an air stream typically employ nitrogen adsorbents such as CaA, CaX, NaX, LiX types, etc., to produce oxygen based on equilibrium adsorption theory.
In the present invention, the adsorption column, which may be referred to as an adsorber, an adsorption bed or a separator, means a container filled with at least one adsorbent having a strong adsorption ability to a component which is easily adsorbed in a mixed gas, such as the above-mentioned adsorbent.
In the present invention, the terms Pressure Swing Adsorption, Adsorption separation, PSA, etc. are well known to those skilled in the art, and these refer not only to PSA methods, but also to methods similar thereto, such as Vacuum Swing Adsorption (VSA) or Mixed Pressure Swing Adsorption (MPSA), etc., and are to be understood in a broader sense, that is, for the Adsorption Pressure of the periodic cycle, a higher Pressure relative to the desorption step, may include a Pressure greater than or equal to atmospheric Pressure, and for the desorption Pressure of the periodic cycle, a lower Pressure relative to the Adsorption step, may include a Pressure less than or equal to atmospheric Pressure.
The method and the device of the invention do not exclude the use of a plurality of groups of adsorption separators which are arranged in parallel for separation, and the gas flow form of the adsorption separators can be axial flow, radial flow, lateral flow or other forms. Those skilled in the art will appreciate that even three or more of various types of separators may be used for separation, by providing the necessary additional lines and switching valves.
The product gas buffer vessel, such as described in the known art, may be filled with the necessary packing to achieve a more economical buffer volume.
The method and the device of the invention can arrange necessary gas detection equipment at the feed gas inlet, the intermediate process and the product gas outlet end, and install necessary pressure detection, dew point detection and purity detection equipment on the separator and the buffer tank, thereby forming a system which completely operates according to the required pressure and purity and being controlled by an intelligent control program. The method is not difficult to realize in the technical field, and experienced technicians know that the debugging process of the equipment is almost the process from system self-adaptation to stability, and in the fault judgment, a control program gives more sufficient information to maintenance and repair personnel and even directly specifies a fault point.
Regarding liquefaction of carbon dioxide as a product gas, basic physical property data of carbon dioxide are shown in table 1 below:
TABLE 1 basic physical data of carbon dioxide
Obviously, the lower the temperature is, the lower the pressure required by the gas-liquid phase change is, but the achievement of the temperature and the pressure needs to consume a large amount of refrigeration and compression energy, refrigerant water is preferably adopted as a cold source in the invention, and the cold source is usually easy to obtain at low cost, for example, the typical upper water temperature is 3 ℃ (if the temperature can be lower, the better, and the return water temperature is 10 ℃ for liquefaction, so that the compression power consumption of the liquefaction can be reduced to the maximum extent, and the effects of low-temperature liquefaction and storage are comprehensively considered.
In addition, as shown in the following table 2, at 10 ℃, the pressure required by the condensation of carbon dioxide is respectively 15MPa and 6.5MPa when the content of carbon dioxide is 30 percent and 70 percent, and the difference is very large; with the increase of the concentration of the carbon dioxide, the liquefaction pressure of typical 70 percent carbon dioxide is close to that of pure component carbon dioxide, and the liquefaction pressure is respectively 6.5/4.5MPa, the purification system has high purity as much as possible, the liquefaction operation pressure can be greatly reduced, the 6.5MPa type is selected for liquefaction, and the effects of low-temperature refrigeration and high-pressure compression are considered.
TABLE 2 carbon dioxide concentration to operating pressure comparison table
Therefore, the preferable purification system firstly obtains the mixed gas with the carbon dioxide purity of 60-85%, and the mixed gas is liquefied under the conditions of 1-15 ℃ and 3-7.5 MPa, so that good economical efficiency can be obtained.
Various changes may be made in the above-described apparatus without departing from the scope of the invention.
Drawings
FIG. 1 is a schematic flow diagram of a method and apparatus for purifying a low partial pressure carbon dioxide gas mixture according to the present invention.
The symbols in the figure are as follows: 101A and 101B are adsorption towers, B01 is a pressure boosting device, C01 is a pressure boosting device, and PV01 is a product gas buffer tank; PV02 is a waste gas surge tank; TC01 is a refrigerant heat exchanger, and F01 is a filter; YHQ01 is a liquefier, XYQ01 is a silencer, 01A, 02A, 03A, 04A, 01B, 02B, 03B, 04B are automatic control valves, and TV01 is an automatic control valve with flow control regulation capability.
Detailed Description
A typical purification device for carbon dioxide mixed gas with low partial pressure has a structure shown in fig. 1. The method comprises the following steps:
two groups of pressure swing adsorption devices (also called adsorption towers and separators) 101A and 101B are connected in parallel to form two groups of adsorption components which run symmetrically; the two groups of pressure swing adsorption devices are filled with carbon dioxide adsorbents, typically 13X, other modified regenerable carbon dioxide adsorbents with balanced adsorption characteristics;
in addition, water adsorbents (such as one or more of activated alumina, silica gel and other molecular sieves for adsorbing water) are compositely filled at the gas inlet ends of the raw material gases of the two pressure swing adsorption devices so as to remove impurity gases such as water, total hydrocarbons and the like contained in the raw material gas mixture;
the pressure boosting device B01 is used for extracting gas in the adsorption tower and sending the gas into a product gas buffer tank PV 01; the pressure boosting device B01 may be a vacuum pump;
the pressure boosting equipment C01 is used for boosting the pressure of the product carbon dioxide mixed gas to the pressure required by the three phase points of water removal and liquefaction;
a product gas buffer tank PV01 for buffering carbon dioxide product gas;
the exhaust buffer tank PV02 is used for buffering and discharging exhaust gas;
the refrigerant heat exchanger TC01 can be various types of refrigeration equipment and is used for cooling the mixed gas to reduce the water content in the gas;
a filter F01 for removing liquid water droplets contained in the gas phase and discharging the same out of the system;
the liquefier YHQ01 can be various types of refrigeration equipment and heat exchange equipment, is used for cooling gas, meets the requirement of a liquefaction triple point of carbon dioxide mixed gas, and typically adopts a pressure-bearing container (containing heat preservation) for heat exchange by refrigerant water; the liquefier YHQ01 comprises an air inlet, a liquefied carbon dioxide outlet, a non-condensable gas outlet, refrigerant water on-water and a water outlet, and also comprises necessary temperature and pressure monitoring;
the silencer XYQ01 is used for eliminating fluid discharge noise and can be any type of silencer;
still include the control flap: 01A, 02A, 03A, 04A, 01B, 02B, 03B, 04B, and automatic control valves with flow control regulation: TV 01. Wherein:
the raw material gas pipeline is respectively connected with the gas inlets of the adsorption devices 101A and 101B through pipelines, and the control valves 01A and 01B are correspondingly arranged on the two connecting pipelines;
the pressure boosting device B01 is respectively connected with the product air ports of the adsorption devices 101A and 101B through pipelines, and the control valves 02A and 02B are correspondingly arranged on the two connecting pipelines; the other end of the pressure boosting device B01 is connected with the inlet end of a product gas buffer tank PV01 through a pipeline;
the inlet end of the product gas buffer tank PV01 is respectively connected with the product gas ports of the adsorption devices 101A and 101B through pipelines, and the control valves 04A and 04B are correspondingly arranged on the two connecting pipelines;
the inlet end of the exhaust gas buffer tank PV02 is respectively connected with the exhaust gas outlets of the adsorption devices 101A and 101B through pipelines, and the control valves 03A and 03B are correspondingly arranged on the two connecting pipelines; the outlet end of the exhaust buffer tank PV02 is connected with a silencer XYQ01 for discharging the exhaust gas;
the automatic control valve TV01 is arranged on a connecting pipeline of the waste gas outlets of the adsorption devices 101A and 101B;
the inlet end of the refrigerant heat exchanger TC01 is connected with the outlet end of the product gas buffer tank PV01 through a pipeline, and the boosting equipment C01 is arranged on the connecting pipeline; the outlet end of the refrigerant heat exchanger TC01 is sequentially connected with a filter F01 and a liquefier YHQ01 through pipelines.
Generally, the apparatus receives a relatively clean feed gas that has been pretreated, typically after removal of entrained solid particulate impurities and total hydrocarbons such as oil; as is well known in the art, these are very essential to gas separation systems.
The treated raw gas enters a pressure swing adsorption separation device of the prior art described in the attached figure 1, and then carbon dioxide components which are easy to be adsorbed are output from an outlet of a vacuum pump B01, and carbon dioxide with higher purity is output from a product gas buffer tank PV 01.
This pressure swing adsorption device is typical double-tower adsorption system, nitrogen gas in the gas mixture is adsorbed and dispelled to adsorption tower 101A, the difficult gas of adsorbing such as oxygen, adsorption tower 101B is when then accomplishing the regeneration process of adsorbent, the carbon dioxide gas mixture of output enrichment is sent into product gas buffer tank PV01, when adsorption tower 101A adsorbs saturation, switch over promptly and carry out the process of dispelling oxygen, dispelling nitrogen for adsorption tower 101B who has accomplished regeneration, when adsorption tower 101A carries out the regeneration process, the carbon dioxide gas mixture of output enrichment is sent into product gas buffer tank PV01, this kind of pressure swing adsorption process based on balanced adsorption mechanism, heterogeneous order operation when adopting the double-tower device, its typical operation flow is:
(1) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 02A and 02B, boosting the pressure of the adsorption tower 101A, and reducing the pressure of the adsorption tower 101B;
(2) opening control valves 01A and 03A, simultaneously introducing the feed gas and the waste gas of the waste gas buffer tank PV102 into an adsorption tower 101A, and pre-pressurizing the adsorption tower 101A; meanwhile, the control valve 02B is opened, and the adsorption tower 101B starts to produce gas and sends the gas into a product gas buffer tank PV 101;
(3) opening a control valve 01A, and allowing feed gas to enter an adsorption tower 101A to continuously perform pre-pressurization; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(4) opening control valves 01A and 03A, feeding and adsorbing the adsorption tower 101A normally, and allowing the gas difficult to adsorb to enter a waste gas buffer tank PV102 and be discharged out of the system; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(5) opening control valves 04A and 03A, and allowing product gas in the buffer tank PV101 to enter 101A to replace the gas phase; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(6) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 01A and 03A, and feeding and adsorbing in an adsorption tower 101A; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(7) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 02A and 02B, decompressing the adsorption tower 101A, and boosting the pressure of the adsorption tower 101B;
(8) opening a control valve 02A, generating gas by an adsorption tower 101A and sending the gas into a product gas buffer tank PV 101; meanwhile, control valves 01B and 03B are opened, and the feed gas and the waste gas of the waste gas buffer tank PV102 enter the adsorption tower 101B for pre-pressurization;
(9) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, opening a control valve 01B, and allowing the feed gas to enter an adsorption tower 101B for continuous pre-pressurization;
(10) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, control valves 01B and 03B are opened, the adsorption tower 101B performs normal adsorption, and the gas difficult to adsorb enters the waste gas buffer tank PV102 and is discharged out of the system;
(11) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, control valves 04B and 03B are opened, and product gas in the buffer tank PV101 enters 101B to replace the gas phase;
(12) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, the control valve TV01 is opened and adjusted to a certain opening, and the control valves 01B and 03B are opened to perform feed adsorption, and the adsorption tower 101B performs feed adsorption.
In the above steps, except for the designated open valve, all the other valves are in a closed state, and the opening and flow rate can be controlled by adjusting the TV 01.
In the above steps, after a group of adsorption is saturated, the fluid control valve is controlled and switched to control the fluid to enter the symmetrical adsorption group, and the adsorption group with saturated adsorption is regenerated and gas-produced, and the above steps are repeated in a circulating way, so that the carbon dioxide gas mixture containing oxygen, nitrogen and moisture can be purified to high-purity carbon dioxide with purity of 99% or even more than 99.99%, and the high-purity carbon dioxide gas mixture is continuously sent to a post-stage system.
In addition, in the invention, the carbon dioxide purity of 60-99.9% is preferably obtained by purifying the mixed gas containing about 15% of carbon dioxide in typical flue gas, and the carbon dioxide purity of 60-85% is more preferably obtained and is continuously sent to a post-stage system.
In addition, the carbon dioxide gas continuously extracted through the steps is pressurized to 3-7.5 MPa by a supercharger C01, and the purposes of removing water and liquefying carbon dioxide are achieved through two-stage coupled refrigeration, wherein:
preferably, the water in the air is removed by primary refrigeration TC01 under the pressure of 3-7.5 MPa, so as to achieve the process aim of normal pressure dew point of-65 ℃.
The pipe filter F01 is arranged to trap particulates, liquid droplets, which may be present in the pipe and which are discharged from the system via the filter.
Preferably, the process aim of liquefying the mixed gas with the purity of 60-85% of carbon dioxide obtained by the purification system is fulfilled in YHQ01 with a second-stage cold source (second-stage refrigeration, typically, refrigerant water heat exchange) under the conditions of 1-15 ℃ and 3-7.5 MPa, and the non-condensable gas is discharged out of the system.
Therefore, the continuous extraction of the flue gas containing about 15% of carbon dioxide and the purification and liquefaction of the carbon dioxide into liquid carbon dioxide can be completed.
The embodiments described above illustrate only some of the important features of the invention and all other variations which do not depart from the gist of the invention are intended to be within the scope of the invention, which is limited only by the scope of the claims.
Claims (9)
1. A high-purity carbon dioxide gas purification method is characterized in that a pressure swing adsorption technology of a carbon dioxide adsorbent based on a balanced adsorption mechanism is adopted, high-purity carbon dioxide is obtained from an adsorption phase under a lower pressure, and pressurization, refrigeration, water removal and carbon dioxide liquefaction are coupled to obtain high-purity liquid carbon dioxide as a product gas, wherein:
the pressure swing adsorption technology based on the equilibrium adsorption mechanism is characterized in that a carbon dioxide adsorbent is filled in an adsorption bed layer, the adsorbent has stronger adsorption capacity on moisture and carbon dioxide in raw material gas relative to nitrogen and oxygen components, and high-purity carbon dioxide and water vapor mixed gas is obtained through desorption after the adsorption saturation of the bed layer;
in addition, gas phase components in the bed layer are replaced by circularly feeding carbon dioxide product gas with higher purity, and mixed gas of carbon dioxide and water vapor with higher purity is obtained by desorption after the adsorption saturation of the bed layer;
in addition, a gas recovery loop is designed between two or more groups of bed layers which run symmetrically, so that the loss of target gas is reduced to the maximum extent, and the recovery rate is improved;
at least one part of the waste gas generated in the adsorption and separation process flows back to the symmetrical separation bed layer, so that the pressure rise process of the symmetrical separation bed layer is facilitated, the power consumption in the desorption process is reduced, and the recovery rate of the system is improved;
and at least a portion of the product gas will be refluxed to the feed end of the adsorbent bed to displace impure gas in the gas phase.
2. The purification method of claim 1, wherein the subsequent coupled product carbon dioxide gas pressurization process adopts two-stage refrigeration to remove water and liquefied carbon dioxide respectively, wherein the water is removed by the first-stage refrigeration under the pressure of 3-7.5 MPa to realize the normal pressure dew point of-65 ℃; and (3) liquefying the mixed gas with the purity of 60-85% of carbon dioxide obtained by the purification system under the conditions of 1-15 ℃ and 3-7.5 MPa by secondary refrigeration.
3. A high purity carbon dioxide gas purification apparatus based on the purification method according to claim 1 or 2, comprising:
(1) at least one compression device for providing a pressurized feed gas;
(2) at least one set of pressure swing adsorption device, which at least comprises an adsorption tower, wherein a carbon dioxide adsorbent is filled in the adsorption tower; the system also comprises an air inlet valve for raw material gas to enter each adsorption tower and a necessary connecting pipeline thereof, an exhaust valve for waste gas to enter the waste gas buffer tank and a necessary connecting pipeline thereof, and a gas production valve for product gas to enter the product gas buffer tank and a necessary connecting pipeline thereof; control valves for fluid exchange between symmetrically operating towers and necessary pipelines thereof for regulating and cutting off gas flow between the adsorption towers; the product gas enters the gas inlet valve of each adsorption tower and necessary pipelines thereof;
(3) at least one waste gas buffer tank connected with the exhaust end of each separator through a control valve and a necessary connecting pipeline for receiving waste gas from the separator and sending the temporarily stored waste gas into the separator which is in the process of pre-charging at the exhaust end of the separator;
(4) at least one product gas buffer tank, which is connected with the feed end of each separator through a control valve and a necessary connecting pipeline thereof by a desorption vacuum pump, is used for receiving the product gas from the separator, and sending the product gas in the product buffer tank into the gas inlet end of the separator through the control valve and the necessary connecting pipeline thereof to repressurize the separator which is in the adsorption process;
(5) at least one product gas booster for boosting the product gas in the product gas buffer tank to a predetermined pressure;
(6) at least one refrigerant heat exchanger and a filter, the gas is cooled, the moisture in the gas is condensed into liquid state, and the liquid state is removed through the filter and discharged out of the system;
(7) the at least one heat exchanger is used for cooling the carbon dioxide mixed gas from which the moisture is removed to a liquefaction triple point of the mixed gas, liquefying the carbon dioxide in the mixed gas as a product and outputting the product, and discharging the non-condensable gas out of the system;
(8) and a complete set of control components is used for carrying out necessary operation control on the valves on the loop and carrying out necessary control operation on the compression equipment, the vacuum pump, the refrigeration equipment and the heat exchanger equipment.
4. The apparatus for purifying a high purity carbon dioxide gas as recited in claim 3, wherein the carbon dioxide adsorbent is 13X or other modified adsorbent having a regenerable equilibrium adsorption characteristic.
5. The apparatus for purifying high purity carbon dioxide according to claim 3, wherein a water adsorbent is compositely packed at the gas inlet end of the raw gas of the pressure swing adsorption apparatus for removing impurity gases such as water and total hydrocarbons contained in the mixed gas; the water adsorbent is one of activated alumina and a molecular sieve for adsorbing water by silica gel, or a combination of a plurality of the activated alumina and the silica gel.
6. The apparatus for purifying high purity carbon dioxide according to claim 3, wherein the pressure swing adsorption apparatus, also called adsorption tower or separator, has two groups, denoted as 101A, 101B, connected in parallel, to form two groups of symmetrically operated adsorption modules; the two groups of pressure swing adsorption devices are filled with carbon dioxide adsorbents; further comprising:
the pressure boosting device B01 is used for extracting gas in the adsorption tower and sending the gas into a product gas buffer tank PV 01;
the pressure boosting equipment C01 is used for boosting the pressure of the product carbon dioxide mixed gas to the pressure required by the three phase points of water removal and liquefaction;
a product gas buffer tank PV01 for buffering carbon dioxide product gas;
the exhaust buffer tank PV02 is used for buffering and discharging exhaust gas;
the refrigerant heat exchanger TC01 can be various types of refrigeration equipment and is used for cooling the mixed gas to reduce the water content in the gas;
a filter F01 for removing liquid water droplets contained in the gas phase and discharging the same out of the system;
the liquefier YHQ01 can be various types of refrigeration equipment and heat exchange equipment, is used for cooling gas, meets the requirement of a liquefaction triple point of carbon dioxide mixed gas, and typically adopts a pressure-bearing container (containing heat preservation) for heat exchange by refrigerant water; the liquefier YHQ01 comprises an air inlet, a liquefied carbon dioxide outlet, a non-condensable gas outlet, refrigerant water on-water and a water outlet, and also comprises necessary temperature and pressure monitoring;
a muffler XYQ01 for canceling fluid discharge noise;
the system also comprises control valves 01A, 02A, 03A, 04A, 01B, 02B, 03B and 04B and an automatic control valve TV01 with flow control and regulation performance; wherein:
the raw material gas pipeline is respectively connected with the gas inlets of the adsorption devices 101A and 101B through pipelines, and the control valves 01A and 01B are correspondingly arranged on the two connecting pipelines;
the pressure boosting device B01 is respectively connected with the product air ports of the adsorption devices 101A and 101B through pipelines, and the control valves 02A and 02B are correspondingly arranged on the two connecting pipelines; the other end of the pressure boosting device B01 is connected with the inlet end of a product gas buffer tank PV01 through a pipeline;
the inlet end of the product gas buffer tank PV01 is respectively connected with the product gas ports of the adsorption devices 101A and 101B through pipelines, and the control valves 04A and 04B are correspondingly arranged on the two connecting pipelines;
the inlet end of the exhaust gas buffer tank PV02 is respectively connected with the exhaust gas outlets of the adsorption devices 101A and 101B through pipelines, and the control valves 03A and 03B are correspondingly arranged on the two connecting pipelines; the outlet end of the exhaust buffer tank PV02 is connected with a silencer XYQ01 for discharging the exhaust gas;
the automatic control valve TV01 is arranged on a connecting pipeline of the waste gas outlets of the adsorption devices 101A and 101B;
the inlet end of the refrigerant heat exchanger TC01 is connected with the outlet end of the product gas buffer tank PV01 through a pipeline, and the boosting equipment C01 is arranged on the connecting pipeline; the outlet end of the refrigerant heat exchanger TC01 is sequentially connected with a filter F01 and a liquefier YHQ01 through pipelines.
7. The apparatus for purifying high purity carbon dioxide according to claim 6, wherein the treated raw material gas is fed into a pressure swing adsorption separation apparatus, and then carbon dioxide enriched with carbon dioxide which is easily adsorbed is outputted from an outlet of a pressure boosting device B01, and carbon dioxide with higher purity is outputted from a product gas buffer tank PV 01; wherein, the adsorption tower 101A adsorbs and dispels the difficult gases of nitrogen gas, oxygen, etc. in the gas mixture, the adsorption tower 101B finishes the regeneration process of the adsorbent while, produce the carbon dioxide gas mixture enriched and send into the product gas buffer tank PV01, when the adsorption tower 101A adsorbs and is saturated, switch over to the adsorption tower 101B that has already finished regenerating and dispel the oxygen, dispel the process of the nitrogen, while the adsorption tower 101A carries on the regeneration process, produce the carbon dioxide gas mixture enriched and send into the product gas buffer tank PV01, this kind of pressure swing adsorption process based on equilibrium adsorption mechanism, the heterogeneous order when adopting the double-tower apparatus runs; the typical operation flow is as follows:
(1) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 02A and 02B, boosting the pressure of the adsorption tower 101A, and reducing the pressure of the adsorption tower 101B;
(2) opening control valves 01A and 03A, simultaneously introducing the feed gas and the waste gas of the waste gas buffer tank PV102 into an adsorption tower 101A, and pre-pressurizing the adsorption tower 101A; meanwhile, the control valve 02B is opened, and the adsorption tower 101B starts to produce gas and sends the gas into a product gas buffer tank PV 101;
(3) opening a control valve 01A, and allowing feed gas to enter an adsorption tower 101A to continuously perform pre-pressurization; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(4) opening control valves 01A and 03A, feeding and adsorbing the adsorption tower 101A normally, and allowing the gas difficult to adsorb to enter a waste gas buffer tank PV102 and be discharged out of the system; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(5) opening control valves 04A and 03A, and allowing product gas in the buffer tank PV101 to enter 101A to replace the gas phase; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(6) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 01A and 03A, and feeding and adsorbing in an adsorption tower 101A; meanwhile, opening a control valve 02B, and generating gas by an adsorption tower 101B;
(7) opening a control valve TV01, adjusting the opening degree to a certain degree, simultaneously opening control valves 02A and 02B, decompressing the adsorption tower 101A, and boosting the pressure of the adsorption tower 101B;
(8) opening a control valve 02A, generating gas by an adsorption tower 101A and sending the gas into a product gas buffer tank PV 101; meanwhile, control valves 01B and 03B are opened, and the feed gas and the waste gas of the waste gas buffer tank PV102 enter the adsorption tower 101B for pre-pressurization;
(9) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, opening a control valve 01B, and allowing the feed gas to enter an adsorption tower 101B for continuous pre-pressurization;
(10) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, control valves 01B and 03B are opened, the adsorption tower 101B performs normal adsorption, and the gas difficult to adsorb enters the waste gas buffer tank PV102 and is discharged out of the system;
(11) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, control valves 04B and 03B are opened, and product gas in the buffer tank PV101 enters 101B to replace the gas phase;
(12) opening a control valve 02A, and producing gas by an adsorption tower 101A; meanwhile, a control valve TV01 is opened and adjusted to a certain opening degree, meanwhile, control valves 01B and 03B are opened for feeding adsorption, and an adsorption tower 101B is opened for feeding adsorption;
in the above steps, except for the designated open valve, all the other valves are in a closed state, and the opening and flow rate thereof are controlled by adjusting the control valve TV 01.
8. The apparatus for purifying high purity carbon dioxide according to claim 7, wherein the purity of carbon dioxide is 60 to 99.9% by purifying the mixed gas containing about 15% of carbon dioxide in the flue gas in the above steps.
9. The purification device of high-purity carbon dioxide according to claim 7, wherein in the pressurization process of the subsequent coupled product carbon dioxide, two-stage refrigeration is adopted to remove water and liquefied carbon dioxide respectively, wherein the water in the product carbon dioxide is removed by one-stage refrigeration under the pressure of 3-7.5 MPa to realize the normal pressure dew point of-65 ℃; and (3) liquefying the mixed gas with the purity of 60-85% of carbon dioxide obtained by the purification system under the conditions of 1-15 ℃ and 3-7.5 MPa by secondary refrigeration.
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