CN110006216B - Cryogenic and membrane coupled process for separating and recovering noncondensable exhaust gas of ethylene circulating refrigeration system - Google Patents
Cryogenic and membrane coupled process for separating and recovering noncondensable exhaust gas of ethylene circulating refrigeration system Download PDFInfo
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- CN110006216B CN110006216B CN201910247722.XA CN201910247722A CN110006216B CN 110006216 B CN110006216 B CN 110006216B CN 201910247722 A CN201910247722 A CN 201910247722A CN 110006216 B CN110006216 B CN 110006216B
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- refrigeration system
- circulating refrigeration
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- cryogenic
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000005977 Ethylene Substances 0.000 title claims abstract description 103
- 238000005057 refrigeration Methods 0.000 title claims abstract description 46
- 239000012528 membrane Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 76
- 238000000926 separation method Methods 0.000 claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 239000001301 oxygen Substances 0.000 claims abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 7
- 238000009834 vaporization Methods 0.000 claims description 7
- 230000008016 vaporization Effects 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 12
- 238000009825 accumulation Methods 0.000 abstract description 5
- 229920005549 butyl rubber Polymers 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000012465 retentate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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
- B01D53/22—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 diffusion
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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
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B43/00—Arrangements for separating or purifying gases or liquids; Arrangements for vaporising the residuum of liquid refrigerant, e.g. by heat
- F25B43/04—Arrangements for separating or purifying gases or liquids; Arrangements for vaporising the residuum of liquid refrigerant, e.g. by heat for withdrawing non-condensible gases
- F25B43/043—Arrangements for separating or purifying gases or liquids; Arrangements for vaporising the residuum of liquid refrigerant, e.g. by heat for withdrawing non-condensible gases for compression type systems
-
- 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
- F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
-
- 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
- F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
-
- 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
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/62—Ethane or ethylene
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- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- Analytical Chemistry (AREA)
- Power Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
The invention provides a process for separating and recovering noncondensable exhaust gas of a cryogenic and membrane coupled ethylene circulating refrigeration system, belonging to the technical field of petrochemical industry. The process starts from the characteristics of an ethylene circulating refrigeration system, firstly, the non-condensable exhaust gas is liquefied and rectified by utilizing the cryogenic condition formed by ethylene throttling expansion, most of ethylene is recovered in a liquid state, then, residual ethylene in the enriched cryogenic tail gas is separated through a gas membrane, and low-pressure ethylene-rich gas obtained at a permeation side returns to a compressor of the ethylene circulating refrigeration system. Through the coupled treatment of deep cooling and membrane separation, the noncondensable exhaust gas can avoid the accumulation of oxygen and nitrogen and obviously reduce the loss of ethylene. By taking a butyl rubber device of 6 ten thousand tons per year as an example, the high-efficiency separation and recovery process of the noncondensable exhaust gas provided by the invention has the advantages that the content of ethylene in the tail gas discharged to a torch is lower than 5.0 vol%, the recovery rate of ethylene reaches 99%, about 210 tons of ethylene can be recovered every year, and the annual economic benefit exceeds 200 ten thousand yuan.
Description
Technical Field
The invention relates to a process for separating and recovering noncondensable exhaust gas of a cryogenic and membrane coupled ethylene circulating refrigeration system, belonging to the technical field of petrochemical industry. The process comprises the steps of firstly liquefying and rectifying noncondensable exhaust gas by utilizing the cryogenic condition formed by ethylene throttling expansion, recovering most ethylene in a liquid state, then separating and enriching residual ethylene in cryogenic tail gas through a gas membrane, and returning low-pressure ethylene-rich gas obtained at a permeation side to a compressor of an ethylene circulating refrigeration system. Through the coupled treatment of deep cooling and membrane separation, the noncondensable exhaust gas can avoid the accumulation of oxygen and nitrogen and obviously reduce the loss of ethylene.
Background
Ethylene is an important basic chemical raw material and is widely applied to various fields. In the butyl unit, ethylene was used as a refrigerant to provide cold at-76, -97, and-110 ℃ at different throttling pressures. In order to meet the production requirement of a butyl rubber device and provide cold at the temperature of-110 ℃, an ethylene circulating refrigeration system needs to be operated under negative pressure, so that air enters the refrigeration system to form non-condensable gas. To ensure safe operation, the noncondensable gases must be periodically vented from the ethylene recycle refrigeration system. During the discharge process, a large amount of ethylene enters the flare system along with the non-condensable gas, causing huge waste. According to the production data of a 6-ten-thousand-ton butyl rubber device of a certain enterprise, if the noncondensable exhaust gas of an ethylene refrigeration system is directly discharged to a torch, about 212 tons of ethylene is lost every year, and the economic loss exceeds 200 ten thousand yuan/year.
The ethylene recovery methods commonly used at present mainly comprise cryogenic separation and gas membrane separation. Simple cryogenic separation has mainly the following limitations: the influence of the cryogenic temperature fluctuation is large, when the cryogenic temperature is not low enough, the recovery effect is not obvious, when the cryogenic temperature is too low, the full condensation phenomenon easily occurs, and the discharge of non-condensable gas is not facilitated. Simple gas membrane separation is also limited: the concentration of ethylene in the non-condensable exhaust gas reaches up to 97%, the membrane separation and enrichment effect is not obvious, and the phenomenon of obvious non-condensable gas accumulation also exists. Due to the defects of the prior art, a more reasonable and efficient noncondensable exhaust gas separation and recovery process is urgently needed for an ethylene circulating refrigeration system, so that the ethylene loss is obviously reduced while the accumulation of oxygen and nitrogen is avoided.
Disclosure of Invention
The invention relates to a process for separating and recovering noncondensable exhaust gas of a cryogenic and membrane coupled ethylene circulating refrigeration system. The process comprises the steps of firstly liquefying and rectifying noncondensable exhaust gas by utilizing the cryogenic condition formed by ethylene throttling expansion, recovering most ethylene in a liquid state, then separating and enriching residual ethylene in cryogenic tail gas through a gas membrane, and returning low-pressure ethylene-rich gas obtained at a permeation side to a compressor of an ethylene circulating refrigeration system.
The technical scheme of the invention is as follows:
a cryogenic and membrane coupled noncondensable exhaust gas separation and recovery process of an ethylene circulating refrigeration system, wherein the system used by the noncondensable exhaust gas separation and recovery process of the ethylene circulating refrigeration system comprises 1 an ethylene circulating refrigeration system 1, a rectifying tower 2, a heat exchanger 3 and a membrane separation unit 4;
noncondensable exhaust gas S-1 discharged from the ethylene circulating refrigeration system 1 firstly enters the rectifying tower 2 from the bottom of the rectifying tower 2 and is in countercurrent contact with the cryogenic condensate refluxed from the top of the rectifying tower, heavy component ethylene in a gas phase is cooled and liquefied, and oxygen and nitrogen of the noncondensable gas dissolved and absorbed in the cryogenic condensate are desorbed; the liquid ethylene S-2 obtained by separation in the rectifying tower 2 returns to the ethylene circulating refrigeration system 1 from the bottom of the tower;
the low-temperature liquid ethylene S-4 extracted from the ethylene circulating refrigeration system 1 enters a heat exchanger at the top of a rectifying tower 2, cold energy is provided by vaporization, the noncondensable exhaust gas S-1 rising in the rectifying tower 2 is partially liquefied, and the ethylene S-5 after low-temperature vaporization returns to a compressor of the ethylene circulating refrigeration system 1;
the cryogenic tail gas S-3 discharged from the top of the rectifying tower 2 exchanges heat with high-pressure normal-temperature ethylene S-7 output by a compressor in the ethylene circulating refrigeration system 1 in the heat exchanger 3, the high-pressure temperature-reducing liquefied ethylene S-8 is sent to a liquid ethylene tank of the ethylene circulating refrigeration system 1, and the cryogenic tail gas S-6 after heat exchange, the temperature of which is higher than the dew point, enters a membrane separation unit 4 as a raw material; the low pressure side of the membrane separation unit 4 obtains membrane separation permeation gas S-10 enriched with ethylene, the membrane separation permeation gas is sent to the inlet of a compressor of the ethylene circulating refrigeration system 1, the high pressure side of the membrane obtains membrane separation permeation residual gas S-9 without most of the ethylene, and the membrane separation permeation residual gas S-9 is discharged to a torch.
The invention has the beneficial effects that: the invention provides a high-efficiency cryogenic and membrane-coupled separation and recovery process for noncondensable exhaust gas of an ethylene circulating refrigeration system, which comprises the steps of firstly liquefying and rectifying the noncondensable exhaust gas by utilizing a cryogenic condition formed by throttling and expanding ethylene, recovering most of ethylene in a liquid state, then separating and enriching residual ethylene in cryogenic tail gas through a gas membrane, and returning low-pressure ethylene-rich gas obtained at a permeation side to a compressor of the ethylene circulating refrigeration system. By coupling cryogenic rectification and membrane separation, 99% of ethylene in the non-condensable exhaust gas can be recovered on the premise of avoiding the accumulation of oxygen and nitrogen. By taking a butyl rubber device of 6 ten thousand tons per year as an example, the high-efficiency separation and recovery process of the noncondensable exhaust gas provided by the invention can recover about 210 tons of ethylene every year, and the annual economic benefit exceeds 200 ten thousand yuan.
Drawings
FIG. 1 is a schematic flow diagram of the process for the separation and recovery of the non-condensed vent gas of a cryogenic membrane coupled ethylene cycle refrigeration system.
In the figure: 1 an ethylene circulating refrigeration system; 2, a rectifying tower; 3, a heat exchanger; 4 a membrane separation unit; s-1, noncondensable exhaust gas; s-2 liquid ethylene; s-3, deep cooling tail gas; s-4, low-temperature liquid ethylene; s-5 ethylene after low-temperature vaporization; s-6, carrying out heat exchange on the cryogenic tail gas; s-7, high-pressure normal-temperature ethylene; s-8, cooling liquefied ethylene under high pressure; s-9, separating the residual gas by a membrane; s-10 ethylene-enriched membrane separation permeate gas.
Detailed Description
The following detailed description of the invention refers to the accompanying drawings.
Examples
The separation and recovery process provided by the invention is used for treating noncondensable exhaust gas generated by an ethylene circulating refrigeration system of a 6 ten thousand ton/year butyl rubber device. The pressure of the uncondensed off-gas was 1.64MPaG, the temperature was-38 ℃ and the ethylene content was about 97 mol%, so that the amount of ethylene lost per year was about 212 tons of ethylene.
Noncondensable exhaust gas S-1 discharged from the ethylene circulating refrigeration system 1 firstly enters the bottom of a rectifying tower 2 and is in countercurrent contact with the cryogenic condensate refluxed from the top of the tower, heavy component ethylene in a gas phase is cooled and liquefied, and oxygen and nitrogen of the noncondensable gas dissolved and absorbed in the cryogenic condensate are desorbed; the liquid ethylene S-2 obtained by separation in the rectifying tower 2 returns to the ethylene circulating refrigeration system 1 from the bottom of the tower; the low-temperature liquid ethylene S-4 extracted from the ethylene circulating refrigeration system 1 enters a heat exchanger at the top of the rectifying tower 2, cold energy is provided by vaporization, the noncondensable exhaust gas rising in the rectifying tower 2 is partially liquefied, and the ethylene S-5 after low-temperature vaporization returns to a compressor of the ethylene circulating refrigeration system 1; the cryogenic tail gas S-3 discharged from the top of the rectifying tower 2 exchanges heat with high-pressure normal-temperature ethylene S-7 output by a compressor in the ethylene circulating refrigeration system 1 in a heat exchanger 3, the high-pressure normal-temperature ethylene S-8 is sent to a liquid ethylene tank of the ethylene circulating refrigeration system 1 after being cooled and liquefied, the cryogenic tail gas S-6 after heat exchange has the temperature higher than the dew point and is used as a raw material to enter a membrane separation unit 4, membrane separation permeation gas S-10 enriched with ethylene is obtained at the low-pressure side of a membrane and is sent to the compressor inlet of the ethylene circulating refrigeration system 1, and membrane separation permeation residual gas S-9 for removing most of ethylene is obtained at the high-pressure side of the membrane and is discharged to a torch.
The diameter of the rectifying tower 2 is 0.20 meter, the height of the filler is 0.8 meter, and the heat exchange area at the top of the tower is 0.3 square meter; the membrane area was 0.1 square meter.
Conditions of the rectifying tower 2: the pressure at the bottom of the tower is 1.64MPaG, and the temperature is-38 ℃; the overhead pressure was 1.61MPaG at-100 ℃.
Membrane separation conditions: the pressure of the raw material is 1.60MPaG, and the temperature is 30 ℃; osmotic pressure 5kPaG, temperature 27 ℃; residual pressure 1.58MPaG and temperature 29 ℃.
In this example, the membrane separation retentate discharged to the flare had an ethylene content of about 4.6 mol% and an ethylene recovery of 99.0%. 210 tons of ethylene can be recovered every year, and the annual economic benefit can reach 200 ten thousand yuan.
Claims (1)
1. A cryogenic and membrane coupled technology for separating and recovering noncondensable exhaust gas of an ethylene circulating refrigeration system is characterized in that the system used by the technology for separating and recovering the noncondensable exhaust gas of the ethylene circulating refrigeration system comprises an ethylene circulating refrigeration system (1), a rectifying tower (2), a heat exchanger (3) and a membrane separation unit (4);
noncondensable exhaust gas (S-1) discharged from an ethylene circulating refrigeration system (1) firstly enters a rectifying tower (2) from the bottom of the rectifying tower (2) and is in countercurrent contact with a cryogenic condensate refluxed from the top of the rectifying tower, heavy component ethylene in a gas phase is cooled and liquefied, and oxygen and nitrogen of the noncondensable gas dissolved and absorbed in the cryogenic condensate are desorbed; separating the obtained liquid ethylene (S-2) in a rectifying tower (2), and returning the liquid ethylene (S-2) to an ethylene circulating refrigeration system (1) from the bottom of the tower;
low-temperature liquid ethylene (S-4) extracted from the ethylene circulating refrigeration system (1) enters a heat exchanger at the top of a rectifying tower (2), cold energy is provided by vaporization, noncondensable exhaust gas (S-1) rising in the rectifying tower (2) is partially liquefied, and ethylene (S-5) after low-temperature vaporization returns to a compressor of the ethylene circulating refrigeration system (1);
the cryogenic tail gas (S-3) discharged from the top of the rectifying tower (2) exchanges heat with high-pressure normal-temperature ethylene (S-7) output by a compressor in the ethylene circulating refrigeration system (1) in the heat exchanger (3), the high-pressure temperature-reducing liquefied ethylene (S-8) is sent to a liquid ethylene tank of the ethylene circulating refrigeration system (1), and the cryogenic tail gas (S-6) after heat exchange has the temperature higher than the dew point and is used as a raw material to enter a membrane separation unit (4); membrane separation permeation gas (S-10) enriched in ethylene is obtained at the low-pressure side of the membrane separation unit (4) and is sent to the inlet of a compressor of the ethylene circulating refrigeration system (1), membrane separation permeation gas (S-9) with most of the ethylene removed is obtained at the high-pressure side of the membrane, and the membrane separation permeation gas is discharged to a flare.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910247722.XA CN110006216B (en) | 2019-03-29 | 2019-03-29 | Cryogenic and membrane coupled process for separating and recovering noncondensable exhaust gas of ethylene circulating refrigeration system |
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| CN201910247722.XA CN110006216B (en) | 2019-03-29 | 2019-03-29 | Cryogenic and membrane coupled process for separating and recovering noncondensable exhaust gas of ethylene circulating refrigeration system |
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| CN110006216B true CN110006216B (en) | 2020-01-24 |
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| CN114471090B (en) * | 2022-02-07 | 2022-10-04 | 大连理工大学 | Membrane coupling separation process for comprehensively utilizing ethylene device torch gas |
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| US4832718A (en) * | 1982-05-03 | 1989-05-23 | Advanced Extraction Technologies, Inc. | Processing nitrogen-rich, hydrogen-rich, and olefin-rich gases with physical solvents |
| US5372009A (en) * | 1993-11-09 | 1994-12-13 | Mobil Oil Corporation | Cryogenic distillation |
| US5960643A (en) * | 1996-12-31 | 1999-10-05 | Exxon Chemical Patents Inc. | Production of ethylene using high temperature demethanization |
| CN2606739Y (en) * | 2003-03-14 | 2004-03-17 | 大连理工大学 | CO2 purifying device by adsorptive fine disstillation |
| WO2007018509A1 (en) * | 2005-07-28 | 2007-02-15 | Innovene Usa Llc | Cryogenic fractionation process |
| EP2926882A1 (en) * | 2014-04-01 | 2015-10-07 | Linde Aktiengesellschaft | Method and assembly for separating a gas mixture and method for retrofitting a separating system |
| CN104030875B (en) * | 2014-05-23 | 2016-10-05 | 四川天采科技有限责任公司 | High yield highly purified catalytic cracked dry gas sharp separation process for purification and device |
| CN105276924B (en) * | 2014-07-04 | 2017-09-01 | 中国石化工程建设有限公司 | A kind of lighter hydrocarbons cryogenic separation retracting device and method |
| CN104826445B (en) * | 2015-05-15 | 2017-05-03 | 大连理工大学 | Separating process for recycling start-up tail gas of ethylene compression refrigerating system |
| US20170176097A1 (en) * | 2015-12-18 | 2017-06-22 | Bechtel Hydrocarbon Technology Solutions, Inc. | Systems and Methods for Recovering Desired Light Hydrocarbons from Refinery Waste Gas Using a Back-End Turboexpander |
| US10533794B2 (en) * | 2016-08-26 | 2020-01-14 | Ortloff Engineers, Ltd. | Hydrocarbon gas processing |
| CN108641750B (en) * | 2018-05-09 | 2023-04-25 | 天津市天地创智科技发展有限公司 | Dry gas separation system and separation method based on argon circulation refrigeration |
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