CN113952823B - C after recovery 4 F 7 N/CO 2 Device and method for separating and purifying mixed gas - Google Patents
C after recovery 4 F 7 N/CO 2 Device and method for separating and purifying mixed gas Download PDFInfo
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- 238000010521 absorption reaction Methods 0.000 claims abstract description 133
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims description 80
- 238000000746 purification Methods 0.000 claims description 37
- 238000003795 desorption Methods 0.000 claims description 27
- 238000001179 sorption measurement Methods 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 5
- 238000005057 refrigeration Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 8
- 238000009413 insulation Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 141
- 230000006872 improvement Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 4
- 230000008929 regeneration Effects 0.000 description 4
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- 229920006395 saturated elastomer Polymers 0.000 description 3
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- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- 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
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
- F25J3/0266—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon dioxide
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- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
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- 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
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Abstract
C after recovery 4 F 7 N/CO 2 Device and method for separating and purifying mixed gas, belonging to C 4 F 7 N/CO 2 The technical field of mixed gas recovery relates to the technical field of solving the problem of how to recover C in gas insulation equipment 4 F 7 N/CO 2 The mixed gas is separated and purified; c after recovery 4 F 7 N/CO 2 The mixed gas is absorbed CO through an absorption tower 2 Enrichment of C 4 F 7 N, high concentration C after enrichment 4 F 7 Compressing the N mixed gas into a rectifying and purifying tower for pressurizing and cooling, wherein C 4 F 7 N is easy to liquefy, and liquid C 4 F 7 N is transferred to a storage tank, CO 2 Partially vaporised C 4 F 7 N gas is input into a mixed tail gas treatment pipeline through a gas outlet at the top of the rectifying and purifying tower to be adsorbed, and residual C in the N gas is adsorbed 4 F 7 N, CO removal 2 The device can not only lead C to be contained in the gas 4 F 7 N and CO 2 Gas separation, and can remove impurities in the mixed gas, and C after treatment 4 F 7 The purity of N is more than 95%, the flow of the device is simple, and the energy consumption is low.
Description
Technical Field
The invention belongs to C 4 F 7 N/CO 2 The technical field of mixed gas recovery, and relates to a recovered C 4 F 7 N/CO 2 A device and a method for separating and purifying mixed gas.
Background
The gas insulation device is one of key power transmission and transformation devices which cannot be replaced by a modern power grid, and has the advantages of compact structure, small influence by environmental factors, high operation safety and reliability and the like. Due to SF 6 Gases have extremely strong greenhouse effects, and one of six greenhouse gases is limited by the kyoto protocol in 1997. At present, overseas products free of SF have been developed 6 Is an environment-friendly insulating medium C 4 F 7 N, considered as currently replacing SF 6 The gas is applied to a hot spot medium for insulation of power equipment.
C 4 F 7 The insulating property of N is SF 6 More than 2.2 times of the gas, the Global Warming Potential (GWP) is SF only 6 One tenth of the gas. However C 4 F 7 The N liquefaction temperature is higher (one atmosphere pressureabout-4.7deg.C below), and is used with a buffer gas (such as CO) at a certain ratio 2 ) Mixing. Research shows that C 4 F 7 N/CO 2 C in the mixed gas 4 F 7 The N content is 5-15%, and the electric performance requirement can be met. C in order not to cause new environmental pollution 4 F 7 N/CO 2 After the mixed gas is recovered, the mixed gas needs to be separated and purified. However, C 4 F 7 Study and application of N just started, C 4 F 7 N/CO 2 The separation and purification technology of the mixed gas is more blank.
In the prior art, the Chinese patent application C with the application publication number of CN112516746A and the application publication date of 2021, 03 and 19 4 F 7 N/CO 2 Mixed gas recovery and purification device discloses: comprises a recovery purifying gas circuit and a tank charging gas circuit; the air inlet end of the recovery purification air circuit is provided with an air inlet interface, the air outlet end of the recovery purification air circuit is connected with the air inlet end of the tank air charging circuit, and a first pressure sensor, a first electromagnetic valve and an adsorption module are sequentially arranged from the air inlet end to the air outlet end; the air outlet end of the tank air charging path is provided with an air outlet interface, and the tank air charging path is sequentially provided with a first pressure reducing and stabilizing valve, a compressor, a one-way valve and a second pressure sensor from the air inlet end to the air outlet end, and the air outlet of the one-way valve is connected with the air outlet interface. The device also comprises a tail gas recovery branch, an online sampling branch and a mixed gas concentration correction gas circuit, wherein the tail gas recovery branch releases high-pressure gas reserved in the connecting pipeline into a built-in storage tank, and the online sampling branch is matched with the mixed gas concentration correction gas circuit to correct the concentration of the mixed gas so as to enable the mixed gas to be recycled. However, the technical proposal of the Chinese patent application does not give how to separate and purify C 4 F 7 N/CO 2 And (3) mixing the gases.
Disclosure of Invention
The technical problem to be solved by the invention is how to recover C in gas insulation equipment 4 F 7 N/CO 2 And (5) separating and purifying the mixed gas.
The invention solves the technical problems through the following technical scheme:
c after recovery 4 F 7 N/CO 2 The device for separating and purifying the mixed gas comprises: CO 2 Gas adsorption pipeline and CO 2 Desorption pipeline of gas C 4 F 7 A purifying and recycling pipeline of N gas and a mixed tail gas treatment pipeline;
said CO 2 The gas adsorption pipeline includes: a first electromagnetic valve (V1), a third electromagnetic valve (V3), a first absorption tower (1) and a fifth electromagnetic valve (V5); a second electromagnetic valve (V2), a fourth electromagnetic valve (V4), a second absorption tower (2) and a sixth electromagnetic valve (V6);
said CO 2 The desorption pipeline of gas includes: the device comprises a first three-way electromagnetic valve (VT 1), a first diaphragm pump (3), a second three-way electromagnetic valve (VT 2), a third absorption tower (4) and a seventh electromagnetic valve (V7);
the C is 4 F 7 The purification recovery pipeline of N gas includes: a ball valve (V10), a second diaphragm pump (5), a rectifying and purifying tower (6) and a V-shaped storage tank (7);
one end of a first electromagnetic valve (V1) is used as an input end of mixed gas, the other end of the first electromagnetic valve (V1) is in sealing connection with a bottom port of a first absorption tower (1), a top port of the first absorption tower (1) is in sealing connection with one end of a fifth electromagnetic valve (V5), the other end of the fifth electromagnetic valve (V5) is in sealing connection with one end of a ball valve (V10), the other end of the ball valve (V10) is in sealing connection with an input end of a second diaphragm pump (5), an output end of the second diaphragm pump (5) is in sealing connection with an air inlet of a rectification purification tower (6), an air outlet of the rectification purification tower (6) is in sealing connection with a V-shaped storage tank (7), an air outlet of the rectification purification tower (6) is in sealing connection with an input end of a mixed tail gas treatment pipeline, and a first output end of the mixed tail gas treatment pipeline is used as an emptying port; one end of the second electromagnetic valve (V2) is in sealing connection with the input end of the mixed gas, the other end of the second electromagnetic valve (V2) is in sealing connection with the bottom port of the second absorption tower (2), the top port of the second absorption tower (2) is in sealing connection with one end of the sixth electromagnetic valve (V6), and the other end of the sixth electromagnetic valve (V6) is in sealing connection between the fifth electromagnetic valve (V5) and the ball valve (V10); one end of the fourth electromagnetic valve (V4) is connected between the third electromagnetic valve (V3) and the 1# port of the first three-way electromagnetic valve (VT 1) in a sealing way, and the other end of the fourth electromagnetic valve (V4) is connected between the second electromagnetic valve (V2) and the bottom port of the second absorption tower (2) in a sealing way;
one end of the third electromagnetic valve (V3) is connected between the bottom port of the first absorption tower (1) and the first electromagnetic valve (V1) in a sealing way, the other end of the third electromagnetic valve (V3) is connected with the 1# port of the first three-way electromagnetic valve (VT 1) in a sealing way, the 2# port of the first three-way electromagnetic valve (VT 1) is connected with the air inlet of the third absorption tower (4) in a sealing way, the 3# port of the first three-way electromagnetic valve (VT 1) is connected with the input end of the first diaphragm pump (3) in a sealing way, the output end of the first diaphragm pump (3) is connected with the 3# port of the second three-way electromagnetic valve (VT 2) in a sealing way, the 1# port of the second three-way electromagnetic valve (VT 2) is connected with the air inlet of the third absorption tower (4) in a sealing way, the air outlet of the third absorption tower (4) is connected with one end of the seventh electromagnetic valve (V7) in a sealing way, and the other end of the seventh electromagnetic valve (V7) is used as an emptying port.
The device of the invention recovers C 4 F 7 N/CO 2 The mixed gas is absorbed CO through an absorption tower 2 Enrichment of C 4 F 7 N, high concentration C after enrichment 4 F 7 Compressing the N mixed gas into a rectifying and purifying tower (6) for pressurizing and cooling, wherein C 4 F 7 N is easy to liquefy, and liquid C 4 F 7 N is transferred to a storage tank (7), CO 2 Partially vaporised C 4 F 7 N gas is input into a mixed tail gas treatment pipeline through a gas outlet at the top of a rectifying and purifying tower (6) for adsorption, and residual C in the N gas is adsorbed 4 F 7 N, CO removal 2 The device can not only lead C to be contained in the gas 4 F 7 N and CO 2 Gas separation, and can remove impurities in the mixed gas, and C after treatment 4 F 7 The purity of N is more than 95%, the flow of the device is simple, and the energy consumption is low.
As a further improvement of the technical scheme of the invention, the C 4 F 7 The purification recovery pipeline of N gas still includes: the refrigerator (8), the refrigerator (8) is arranged in the rectifying and purifying tower(6) Is used for cooling the rectification and purification tower (6).
As a further improvement of the technical scheme of the present invention, the mixed tail gas treatment pipeline includes: a fourth absorption tower (9), an eighth electromagnetic valve (V8), a ninth electromagnetic valve (V9) and an eleventh electromagnetic valve (V11); one end of an eleventh electromagnetic valve (V11) is in sealing connection with an air outlet of the rectifying and purifying tower (6), the other end of the eleventh electromagnetic valve (V11) is in sealing connection with an air inlet of a fourth absorption tower (9), an air outlet of the fourth absorption tower (9) is in sealing connection with one end of an eighth electromagnetic valve (V8), and the other end of the eighth electromagnetic valve (V8) is used as an emptying port; one end of the ninth electromagnetic valve (V9) is connected between the air outlet of the fourth absorption tower (9) and the eighth electromagnetic valve (V8) in a sealing way, and the other end of the ninth electromagnetic valve (V9) is connected between the fifth electromagnetic valve (V5) and the ball valve (V10) in a sealing way.
As a further improvement of the technical proposal of the invention, the CO 2 The gas adsorption line further comprises: a first pressure gauge (P1); the first pressure gauge (P1) is arranged on the first absorption tower (1) in a sealing mode and is used for detecting the internal pressure of the first absorption tower (1).
As a further improvement of the technical proposal of the invention, the CO 2 The gas adsorption line further comprises: a second pressure gauge (P2); the second pressure gauge (P2) is arranged on the second absorption tower (2) in a sealing mode and is used for detecting the internal pressure of the second absorption tower (2).
As a further improvement of the technical proposal of the invention, the CO 2 The desorption pipeline of gas still includes: a third pressure gauge (P3); the third pressure gauge (P3) is hermetically arranged on the third absorption tower (4) and is used for detecting the internal pressure of the third absorption tower (4); a measuring port A is arranged between the air outlet of the third absorption tower (4) and the seventh electromagnetic valve (V7) and is used for detecting the components and the purity of the mixed gas.
As a further improvement of the technical scheme of the invention, the mixed tail gas treatment pipeline further comprises: the fourth pressure gauge (P4) is hermetically arranged on the fourth absorption tower (9) and is used for detecting the internal pressure of the fourth absorption tower (9); a measuring port B is arranged between the air outlet of the fourth absorption tower (9) and the eighth electromagnetic valve (V8) and is used for detecting the components and the purity of the mixed gas.
As a further improvement of the technical scheme of the invention, the C 4 F 7 The purification recovery pipeline of N gas still includes: and the fifth pressure gauge (P4) is hermetically arranged on the V-shaped storage tank (7) and is used for detecting the internal pressure of the V-shaped storage tank (7).
C after being recovered and applied to 4 F 7 N/CO 2 The method of the separation and purification device of the mixed gas is characterized by comprising the following steps:
s1, adsorb C 4 F 7 N/CO 2 CO in mixed gas 2 The gas is specifically as follows: opening a first electromagnetic valve (V1), C 4 F 7 N/CO 2 The mixed gas enters a first absorption tower (1) through a first electromagnetic valve (V1), and the first absorption tower (1) absorbs C 4 F 7 N/CO 2 Most of CO in the mixed gas 2 The gas, at this time, opens the fifth electromagnetic valve (V5), the ball valve (V10) and the second diaphragm pump (5), and the gas contains a small amount of CO after being absorbed by the first absorption tower (1) 2 The mixed gas of (2) is compressed into a rectifying and purifying tower (6) through a second diaphragm pump (5) to be separated and purified;
S2、CO 2 the desorption of the gas is specifically as follows: closing the first electromagnetic valve (V1) and the fifth electromagnetic valve (V5), opening the third electromagnetic valve (V3), communicating a 1# port and a 3# port of the first three-way electromagnetic valve (VT 1), communicating a 3# port and a 1# port of the second three-way electromagnetic valve (VT 2), starting the first diaphragm pump (3) to carry out negative pressure pumping desorption on the first absorption tower (1), and carrying out a large amount of CO generated by desorption 2 Trace C 4 F 7 The N gas is absorbed with C in the third absorption tower (4) 4 F 7 N gas, then opening a seventh electromagnetic valve (V7), and discharging CO through the seventh electromagnetic valve (V7) 2 A gas;
S3、C 4 F 7 the purification and recovery of N gas are specifically as follows: opening a ball valve (V10), starting a second diaphragm pump (5), compressing the mixed gas absorbed by the first absorption tower (1) into a rectification purification tower (6) for pressurization, refrigeration and liquefaction, opening a V-shaped storage tank (7), and liquefying C 4 F 7 N streamsInto a V-type tank (7), while the gaseous CO 2 Micro-vaporized C 4 F 7 And the N tail gas enters a mixed tail gas treatment pipeline for treatment.
The invention has the advantages that:
(1) The device of the invention recovers C 4 F 7 N/CO 2 The mixed gas is absorbed CO through an absorption tower 2 Enrichment of C 4 F 7 N, high concentration C after enrichment 4 F 7 Compressing the N mixed gas into a rectifying and purifying tower (6) for pressurizing and cooling, wherein C 4 F 7 N is easy to liquefy, and liquid C 4 F 7 N is transferred to a storage tank (7), CO 2 Partially vaporised C 4 F 7 N gas is input into a mixed tail gas treatment pipeline through a gas outlet at the top of a rectifying and purifying tower (6) for adsorption, and residual C in the N gas is adsorbed 4 F 7 N, CO removal 2 The device can not only lead C to be contained in the gas 4 F 7 N and CO 2 Gas separation, and can remove impurities in the mixed gas, and C after treatment 4 F 7 The purity of N is more than 95%, the flow of the device is simple, and the energy consumption is low.
(2) Setting two groups of CO which are mutually backed up 2 Absorption tower, a group of absorption CO 2 And the other group is desorbed, so that the separation efficiency is further improved.
(3) The bottom V-shaped design of the V-shaped storage tank (7) can be used for liquid C 4 F 7 N gathers bottom, conveniently fills, can furthest reduce C simultaneously 4 F 7 And N is converted into gas phase and liquid phase, so that the purification efficiency is improved.
Drawings
FIG. 1 shows a recovered C according to a first embodiment of the present invention 4 F 7 N/CO 2 A structure diagram of a device for separating and purifying mixed gas;
FIG. 2 shows a recovered C according to a second embodiment of the present invention 4 F 7 N/CO 2 A flow chart of a method for separating and purifying mixed gas.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The technical scheme of the invention is further described below with reference to the attached drawings and specific embodiments:
example 1
As shown in FIG. 1, a recovered C 4 F 7 N/CO 2 The device for separating and purifying the mixed gas comprises: the device comprises a first absorption tower 1, a second absorption tower 2, a first diaphragm pump 3, a third absorption tower 4, a second diaphragm pump 5, a rectification and purification tower 6, a V-shaped storage tank 7, a refrigerator 8 and a fourth absorption tower 9; a first electromagnetic valve V1, a second electromagnetic valve V2, a third electromagnetic valve V3, a fourth electromagnetic valve V4, a fifth electromagnetic valve V5, a sixth electromagnetic valve V6, a seventh electromagnetic valve V7, an eighth electromagnetic valve V8, a ninth electromagnetic valve V9, a ball valve V10, an eleventh electromagnetic valve V11, a first three-way electromagnetic valve VT1 and a second three-way electromagnetic valve VT2; a first pressure gauge P1, a second pressure gauge P2, a third pressure gauge P3, a fourth pressure gauge P4, and a fifth pressure gauge P5.
One end of the first electromagnetic valve V1 is used as an input end of mixed gas, the other end of the first electromagnetic valve V1 is in sealing connection with a bottom port of the first absorption tower 1, a top port of the first absorption tower 1 is in sealing connection with one end of a fifth electromagnetic valve V5, the other end of the fifth electromagnetic valve V5 is in sealing connection with one end of a ball valve V10, the other end of the ball valve V10 is in sealing connection with an input end of a second diaphragm pump 5, an output end of the second diaphragm pump 5 is in sealing connection with an air inlet of a rectifying and purifying tower 6, a liquid outlet of the rectifying and purifying tower 6 is in sealing connection with a V-shaped storage tank 7, an air outlet of the rectifying and purifying tower 6 is in sealing connection with one end of an eleventh electromagnetic valve V11, the other end of the eleventh electromagnetic valve V11 is in sealing connection with an air inlet of a fourth absorption tower 9, a refrigerator 8 is arranged outside the rectifying and purifying tower 6 for cooling the rectifying and purifying tower 6, an air outlet of the fourth absorption tower 9 is in sealing connection with one end of an eighth electromagnetic valve V8, and the other end of the eighth electromagnetic valve V8 is used as an emptying port; one end of the ninth electromagnetic valve V9 is connected between the air outlet of the fourth absorption tower 9 and the eighth electromagnetic valve V8 in a sealing mode, and the other end of the ninth electromagnetic valve V9 is connected between the fifth electromagnetic valve V5 and the ball valve V10 in a sealing mode.
One end of the second electromagnetic valve V2 is used as an input end of the mixed gas, the other end of the second electromagnetic valve V2 is in sealing connection with the bottom port of the second absorption tower 2, the top port of the second absorption tower 2 is in sealing connection with one end of the sixth electromagnetic valve V6, and the other end of the sixth electromagnetic valve V6 is in sealing connection between the fifth electromagnetic valve V5 and the ball valve V10.
The third electromagnetic valve V3 and the fourth electromagnetic valve V4 are connected in series in a sealing manner, wherein the non-serial end of the third electromagnetic valve V3 is connected between the bottom port of the first absorption tower 1 and the first electromagnetic valve V1 in a sealing manner, the non-serial end of the fourth electromagnetic valve V4 is connected between the bottom port of the second absorption tower 2 and the second electromagnetic valve V2 in a sealing manner, the serial common point of the third electromagnetic valve V3 and the fourth electromagnetic valve V4 is connected with the 1# port of the first three-way electromagnetic valve VT1 in a sealing manner, the 2# port of the first three-way electromagnetic valve VT1 is connected with the air inlet of the third absorption tower 4 in a sealing manner, the 3# port of the first three-way electromagnetic valve VT1 is connected with the input end of the first diaphragm pump 3 in a sealing manner, the output end of the first diaphragm pump 3 is connected with the 3# port of the second three-way electromagnetic valve VT2 in a sealing manner, the 1# port of the second three-way electromagnetic valve VT2 is connected with the air inlet of the third absorption tower 4 in a sealing manner, the 2# port of the second three-way electromagnetic valve VT2 is connected between the sixth electromagnetic valve V6 and the ball valve V10 in a sealing manner, and the air outlet of the third absorption tower 4 is connected with one end of the seventh electromagnetic valve V7 in a sealing manner.
The first pressure gauge P1 is arranged on the first absorption tower 1 in a sealing way and is used for detecting the internal pressure of the first absorption tower 1; the second pressure gauge P2 is arranged on the second absorption tower 2 in a sealing way and is used for detecting the internal pressure of the second absorption tower 2; the third pressure gauge P3 is hermetically arranged on the third absorption tower 4 and is used for detecting the internal pressure of the third absorption tower 4; the fourth pressure gauge P4 is hermetically arranged on the fourth absorption tower 9 and is used for detecting the internal pressure of the fourth absorption tower 9; the fifth pressure gauge P4 is hermetically provided on the V-tank 7 for detecting the internal pressure of the V-tank 7.
A measuring port A is arranged between the air outlet of the third absorption tower 4 and a seventh electromagnetic valve V7 and is used for detecting the components and the purity of the mixed gas; a measuring port B is arranged between the air outlet of the fourth absorption tower 9 and the eighth electromagnetic valve V8 and is used for detecting the components and the purity of the mixed gas, and the gas purity is detected as a special purpose C 4 F 7 The chromatograph for detecting N can detect each component and content in the gas at the same time.
Operation of the device
1. Adsorption C 4 F 7 N/CO 2 CO in mixed gas 2 Gas and its preparation method
The first absorption tower 1 and the second absorption tower 2 are filled with a selective adsorbent for selectively adsorbing CO 2 Molecules, not adsorbing C 4 F 7 N molecule.
Opening the first electromagnetic valve V1, closing the second electromagnetic valve V2, C 4 F 7 N/CO 2 The mixed gas enters the first absorption tower 1 through the first electromagnetic valve V1, and the first absorption tower 1 absorbs C 4 F 7 N/CO 2 Most of CO in the mixed gas 2 The gas, at this time, the fifth electromagnetic valve V5 and the ball valve V10 are opened, the second diaphragm pump 5 is opened, and a small amount of CO is contained after being absorbed by the first absorption tower 1 2 The mixed gas of (2) is compressed into a rectifying and purifying tower 6 through a second diaphragm pump 5 for separation and purification.
When the first absorption tower 1 is saturated in adsorption, the first electromagnetic valve V1 and the fifth electromagnetic valve V5 are closed, the second electromagnetic valve V2 and the sixth electromagnetic valve V6 are opened, and the second absorption tower 2 is started for C 4 F 7 N/CO 2 CO in mixed gas 2 The gas is adsorbed.
2、CO 2 Desorption of gases
2.1 first absorption column Desorption Process
Closing the first electromagnetic valve V1, the fourth electromagnetic valve V4 and the fifth electromagnetic valve V5, opening the third electromagnetic valve V3, communicating the 1# port and the 3# port of the first three-way electromagnetic valve VT1, communicating the 3# port and the 1# port of the second three-way electromagnetic valve VT2, starting the first diaphragm pump 3 to pump negative pressure to the first absorption tower 1, and pumping negative pressure to the first absorption tower 1In the environment, CO adsorbed in the adsorbent 2 Can release and a small amount of C can be present in the desorption process 4 F 7 N gas is mixed therein, and a large amount of CO generated by desorption is mixed therein 2 Trace C 4 F 7 The N gas is absorbed by C in the third absorption tower 4 4 F 7 N gas (the third absorption tower is internally filled with a special C 4 F 7 N molecular adsorbent for CO 2 Non-adsorption of molecules), measurement port A detects C 4 F 7 After the content of N gas is lower than 500 mu L/L, opening a seventh electromagnetic valve V7, and discharging CO through the seventh electromagnetic valve V7 2 When the gas pressure gauge P1 is smaller than 10kPa (absolute pressure), the desorption process of the first absorption tower 1 is finished.
2.2 Desorption Process of the second absorption column
Closing the second electromagnetic valve V2, the third electromagnetic valve V3 and the sixth electromagnetic valve V6, opening the fourth electromagnetic valve V4, communicating the 1# port and the 3# port of the first three-way electromagnetic valve VT1, communicating the 3# port and the 1# port of the second three-way electromagnetic valve VT2, starting the first diaphragm pump 3 to pump negative pressure to the second absorption tower 2, and adsorbing CO in the adsorbent under the negative pressure environment 2 Can release and a small amount of C can be present in the desorption process 4 F 7 N gas is mixed therein, and a large amount of CO generated by desorption is mixed therein 2 Trace C 4 F 7 The N gas is absorbed by C in the third absorption tower 4 4 F 7 N gas, measuring port A detects C 4 F 7 After the content of N gas is lower than 500 mu L/L, opening a seventh electromagnetic valve V7, and discharging CO through the seventh electromagnetic valve V7 2 And when the gas pressure gauge P2 is smaller than 10kPa (absolute pressure), the desorption process of the second absorption tower 2 is finished.
3. Regeneration of the third absorption column
When the third absorption tower 4 is saturated by adsorption, at the moment, the third electromagnetic valve V3, the fourth electromagnetic valve V4, the fifth electromagnetic valve V5, the sixth electromagnetic valve V6 and the seventh electromagnetic valve V7 are closed, the 2# port and the 3# port of the first three-way electromagnetic valve VT1 are communicated, the 3# port and the 2# port of the second three-way electromagnetic valve VT2 are communicated, the first diaphragm pump 3 is started to pump negative pressure to the third absorption tower 4, the third absorption tower 4 is subjected to negative pressure desorption, and at the moment, the ball valve V10 is opened and the valve V2 is startedThe second diaphragm pump 5 is moved to desorb C 4 F 7 And (3) compressing the N gas to a rectifying and purifying tower 6 for further purification, and ending the regeneration of the third absorption tower 4 when the internal pressure of the third absorption tower 4 is lower than 10kPa (absolute pressure).
4、C 4 F 7 Purification and recovery of N gas
The refrigerator 8 is started in advance to refrigerate the rectification and purification tower 6 for 10min in advance, at the moment, the ball valve V10 is opened, the second diaphragm pump 5 is started, the mixed gas absorbed by the first absorption tower 1 and the second absorption tower 2 is compressed into the rectification and purification tower 6 for pressurization, refrigeration and liquefaction, and the V-shaped storage tank 7 is opened due to C 4 F 7 The liquefaction temperature of N gas is-4.7 ℃, and C is liquefied after pressurization, refrigeration and liquefaction 4 F 7 N flows into the V-tank 7, while gaseous CO 2 Micro-vaporized C 4 F 7 N gas is positioned at the top of the rectifying and purifying tower 6, the refrigerator 8 only refrigerates the rectifying and purifying tower 6, and the lower V-shaped storage tank 7 is close to C 4 F 7 N is liquefied to cool, when the temperature of the V-shaped storage tank 7 is not reduced any more or is lower than 1 ℃/2min, the V-shaped storage tank 7 is closed, and an eleventh electromagnetic valve V11 is opened to exhaust for 30s; when the temperature of the V-shaped storage tank 7 reaches minus 10 ℃ and the internal pressure is lower than 100kPa (absolute pressure), closing an eleventh electromagnetic valve V11, opening a liquid outlet of the V-shaped storage tank 7, and leading the liquid C to be in a liquid state 4 F 7 The N tank is transferred to an external container.
C 4 F 7 N and CO 2 Is characterized by larger liquefaction temperature difference of C 4 F 7 N/CO 2 Introducing the mixed gas into a low-temperature rectification purification tower 6, reducing the temperature to a certain value, and liquefying C 4 F 7 N is liquefied and slowly discharged from the bottom of the rectifying and purifying tower 6 due to C 4 F 7 N/CO 2 C in the mixed gas 4 F 7 The N content is low, so the volume of the V-shaped storage tank 7 at the lower part of the rectifying and purifying tower 6 can not be too large, and the C is liquefied 4 F 7 The outlet pipeline of N is in a slender funnel shape, and the outlet is provided with a needle valve for controlling liquefaction C 4 F 7 Flow of N.
5. Mixed tail gas treatment of purifying tower
Rectifying and purifying towerCO in 6 2 Trace of gaseous C 4 F 7 N is intermittently discharged through an eleventh electromagnetic valve V11, and the discharged mixed gas passes through a fourth absorption tower 9 to obtain C in the mixed gas 4 F 7 N gas is adsorbed, and CO after adsorption 2 Gas (wherein C 4 F 7 N gas content below 500. Mu.L/L) is evacuated via an eighth solenoid valve V8, during which the evacuated CO is monitored via a measuring port B 2 Middle C 4 F 7 When the detected value is higher than 500. Mu.L/L, the fourth absorption column 9 needs to be regenerated.
6. Regeneration of the fourth absorption column
When the fourth absorption tower 9 is saturated, the fifth electromagnetic valve V5, the sixth electromagnetic valve V6, the eighth electromagnetic valve V8 and the eleventh electromagnetic valve V11 are closed, the ninth electromagnetic valve V9 and the ball valve V10 are opened, the second diaphragm pump 5 is started, the fourth absorption tower 9 is subjected to negative pressure desorption, and the desorbed C is subjected to negative pressure desorption 4 F 7 And (3) compressing the N gas to the rectifying and purifying tower 6 for further purification, and ending the regeneration of the fourth absorption tower 9 when the internal pressure of the fourth absorption tower 9 is lower than 10kPa (absolute pressure).
Example two
As shown in FIG. 2, one is applied to the recovered C 4 F 7 N/CO 2 The method of the separation and purification device for the mixed gas comprises the following steps:
s1, adsorb C 4 F 7 N/CO 2 CO in mixed gas 2 The gas is specifically as follows: opening the first electromagnetic valve V1, C 4 F 7 N/CO 2 The mixed gas enters the first absorption tower 1 through the first electromagnetic valve V1, and the first absorption tower 1 absorbs C 4 F 7 N/CO 2 Most of CO in the mixed gas 2 The gas, at this time, the fifth electromagnetic valve V5 and the ball valve V10 are opened, the second diaphragm pump 5 is opened, and a small amount of CO is contained after being absorbed by the first absorption tower 1 2 The mixed gas of (2) is compressed into a rectifying and purifying tower 6 through a second diaphragm pump 5 to be separated and purified;
S2、CO 2 the desorption of the gas is specifically as follows: closing the first electromagnetic valve V1 and the fifth electromagnetic valve V5, opening the third electromagnetic valve V3 and the first three-way electric currentThe 1# port and the 3# port of the magnetic valve VT1 are communicated, the 3# port and the 1# port of the second three-way electromagnetic valve VT2 are communicated, the first diaphragm pump 3 is started to carry out negative pumping pressure desorption on the first absorption tower 1, and a large amount of CO generated by desorption is desorbed 2 Trace C 4 F 7 The N gas is absorbed by C in the third absorption tower 4 4 F 7 N gas, then opening the seventh electromagnetic valve V7, and discharging CO through the seventh electromagnetic valve V7 2 A gas;
S3、C 4 F 7 the purification and recovery of N gas are specifically as follows: opening a ball valve V10, starting a second diaphragm pump 5, compressing the mixed gas absorbed by the first absorption tower 1 into a rectification and purification tower 6 for pressurization, refrigeration and liquefaction, opening a V-shaped storage tank 7, and liquefying C 4 F 7 N flows into the V-tank 7, while gaseous CO 2 Micro-vaporized C 4 F 7 And the N tail gas enters a mixed tail gas treatment pipeline for treatment.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. C after recovery 4 F 7 N/CO 2 The separation and purification device of the mixed gas is characterized by comprising: CO 2 Gas adsorption pipeline and CO 2 Desorption pipeline of gas C 4 F 7 A purifying and recycling pipeline of N gas and a mixed tail gas treatment pipeline;
said CO 2 The gas adsorption pipeline includes: a first electromagnetic valve (V1), a second electromagnetic valve (V2), a third electromagnetic valve (V3), a fourth electromagnetic valve (V4), a first absorption tower (1), a second absorption tower (2), a fifth electromagnetic valve (V5) and a sixth electromagnetic valve (V6);
said CO 2 The desorption pipeline of gas includes: first oneA three-way electromagnetic valve (VT 1), a first diaphragm pump (3), a second three-way electromagnetic valve (VT 2), a third absorption tower (4) and a seventh electromagnetic valve (V7);
the C is 4 F 7 The purification recovery pipeline of N gas includes: a ball valve (V10), a second diaphragm pump (5), a rectifying and purifying tower (6) and a V-shaped storage tank (7);
one end of a first electromagnetic valve (V1) is used as an input end of mixed gas, the other end of the first electromagnetic valve (V1) is in sealing connection with a bottom port of a first absorption tower (1), a top port of the first absorption tower (1) is in sealing connection with one end of a fifth electromagnetic valve (V5), the other end of the fifth electromagnetic valve (V5) is in sealing connection with one end of a ball valve (V10), the other end of the ball valve (V10) is in sealing connection with an input end of a second diaphragm pump (5), an output end of the second diaphragm pump (5) is in sealing connection with an air inlet of a rectification purification tower (6), an air outlet of the rectification purification tower (6) is in sealing connection with a V-shaped storage tank (7), an air outlet of the rectification purification tower (6) is in sealing connection with an input end of a mixed tail gas treatment pipeline, and a first output end of the mixed tail gas treatment pipeline is used as an emptying port; one end of the second electromagnetic valve (V2) is in sealing connection with the input end of the mixed gas, the other end of the second electromagnetic valve (V2) is in sealing connection with the bottom port of the second absorption tower (2), the top port of the second absorption tower (2) is in sealing connection with one end of the sixth electromagnetic valve (V6), and the other end of the sixth electromagnetic valve (V6) is in sealing connection between the fifth electromagnetic valve (V5) and the ball valve (V10); one end of the fourth electromagnetic valve (V4) is connected between the third electromagnetic valve (V3) and the 1# port of the first three-way electromagnetic valve (VT 1) in a sealing way, and the other end of the fourth electromagnetic valve (V4) is connected between the second electromagnetic valve (V2) and the bottom port of the second absorption tower (2) in a sealing way;
one end of the third electromagnetic valve (V3) is connected between the bottom port of the first absorption tower (1) and the first electromagnetic valve (V1) in a sealing way, the other end of the third electromagnetic valve (V3) is connected with the 1# port of the first three-way electromagnetic valve (VT 1) in a sealing way, the 2# port of the first three-way electromagnetic valve (VT 1) is connected with the air inlet of the third absorption tower (4) in a sealing way, the 3# port of the first three-way electromagnetic valve (VT 1) is connected with the input end of the first diaphragm pump (3) in a sealing way, the output end of the first diaphragm pump (3) is connected with the 3# port of the second three-way electromagnetic valve (VT 2) in a sealing way, the 1# port of the second three-way electromagnetic valve (VT 2) is connected with the air inlet of the third absorption tower (4) in a sealing way, the air outlet of the third absorption tower (4) is connected with one end of the seventh electromagnetic valve (V7) in a sealing way, and the other end of the seventh electromagnetic valve (V7) is used as an emptying port.
2. A recovered C according to claim 1 4 F 7 N/CO 2 The device for separating and purifying the mixed gas is characterized in that the C 4 F 7 The purification recovery pipeline of N gas still includes: the refrigerator (8), refrigerator (8) set up in the outside of rectifying and purifying column (6), be used for cooling down rectifying and purifying column (6).
3. A recovered C according to claim 1 4 F 7 N/CO 2 The mixed gas separation and purification device is characterized in that the mixed tail gas treatment pipeline comprises: a fourth absorption tower (9), an eighth electromagnetic valve (V8), a ninth electromagnetic valve (V9) and an eleventh electromagnetic valve (V11); one end of an eleventh electromagnetic valve (V11) is in sealing connection with an air outlet of the rectifying and purifying tower (6), the other end of the eleventh electromagnetic valve (V11) is in sealing connection with an air inlet of a fourth absorption tower (9), an air outlet of the fourth absorption tower (9) is in sealing connection with one end of an eighth electromagnetic valve (V8), and the other end of the eighth electromagnetic valve (V8) is used as an emptying port; one end of the ninth electromagnetic valve (V9) is connected between the air outlet of the fourth absorption tower (9) and the eighth electromagnetic valve (V8) in a sealing way, and the other end of the ninth electromagnetic valve (V9) is connected between the fifth electromagnetic valve (V5) and the ball valve (V10) in a sealing way.
4. A recovered C according to claim 1 4 F 7 N/CO 2 The device for separating and purifying the mixed gas is characterized in that the CO 2 The gas adsorption line further comprises: a first pressure gauge (P1); the first pressure gauge (P1) is arranged on the first absorption tower (1) in a sealing mode and is used for detecting the internal pressure of the first absorption tower (1).
5. A recovered C according to claim 1 4 F 7 N/CO 2 The device for separating and purifying the mixed gas is characterized in that the CO 2 The gas adsorption line further comprises: a second pressure gauge (P2); the second pressure gauge (P2) is arranged on the second absorption tower (2) in a sealing mode and is used for detecting the internal pressure of the second absorption tower (2).
6. A recovered C according to claim 1 4 F 7 N/CO 2 The device for separating and purifying the mixed gas is characterized in that the CO 2 The desorption pipeline of gas still includes: a third pressure gauge (P3); the third pressure gauge (P3) is hermetically arranged on the third absorption tower (4) and is used for detecting the internal pressure of the third absorption tower (4); a measuring port A is arranged between the air outlet of the third absorption tower (4) and the seventh electromagnetic valve (V7) and is used for detecting the components and the purity of the mixed gas.
7. A recovered C according to claim 3 4 F 7 N/CO 2 The mixed gas separating and purifying device is characterized in that the mixed tail gas treatment pipeline further comprises: the fourth pressure gauge (P4) is hermetically arranged on the fourth absorption tower (9) and is used for detecting the internal pressure of the fourth absorption tower (9); a measuring port B is arranged between the air outlet of the fourth absorption tower (9) and the eighth electromagnetic valve (V8) and is used for detecting the components and the purity of the mixed gas.
8. A recovered C according to claim 1 4 F 7 N/CO 2 The device for separating and purifying the mixed gas is characterized in that the C 4 F 7 The purification recovery pipeline of N gas still includes: and the fifth pressure gauge (P4) is hermetically arranged on the V-shaped storage tank (7) and is used for detecting the internal pressure of the V-shaped storage tank (7).
9. A post recovery C applied to any one of claims 1-8 4 F 7 N/CO 2 The method of the separation and purification device of the mixed gas is characterized by comprising the following steps:
s1, adsorb C 4 F 7 N/CO 2 CO in mixed gas 2 The gas is specifically as follows: opening a first electromagnetic valve (V1), C 4 F 7 N/CO 2 The mixed gas enters a first absorption tower (1) through a first electromagnetic valve (V1), and the first absorption tower (1) absorbs C 4 F 7 N/CO 2 Most of CO in the mixed gas 2 The gas, at this time, opens the fifth electromagnetic valve (V5), the ball valve (V10) and the second diaphragm pump (5), and the gas contains a small amount of CO after being absorbed by the first absorption tower (1) 2 The mixed gas of (2) is compressed into a rectifying and purifying tower (6) through a second diaphragm pump (5) to be separated and purified;
S2、CO 2 the desorption of the gas is specifically as follows: closing the first electromagnetic valve (V1) and the fifth electromagnetic valve (V5), opening the third electromagnetic valve (V3), communicating a 1# port and a 3# port of the first three-way electromagnetic valve (VT 1), communicating a 3# port and a 1# port of the second three-way electromagnetic valve (VT 2), starting the first diaphragm pump (3) to carry out negative pressure pumping desorption on the first absorption tower (1), and carrying out a large amount of CO generated by desorption 2 Trace C 4 F 7 The N gas is absorbed with C in the third absorption tower (4) 4 F 7 N gas, then opening a seventh electromagnetic valve (V7), and discharging CO through the seventh electromagnetic valve (V7) 2 A gas;
S3、C 4 F 7 the purification and recovery of N gas are specifically as follows: opening a ball valve (V10), starting a second diaphragm pump (5), compressing the mixed gas absorbed by the first absorption tower (1) into a rectification purification tower (6) for pressurization, refrigeration and liquefaction, opening a V-shaped storage tank (7), and liquefying C 4 F 7 N flows into a V-type storage tank (7), while gaseous CO 2 Micro-vaporized C 4 F 7 And the N tail gas enters a mixed tail gas treatment pipeline for treatment.
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