CN115540499A - Device and method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas - Google Patents

Device and method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas Download PDF

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CN115540499A
CN115540499A CN202211171362.8A CN202211171362A CN115540499A CN 115540499 A CN115540499 A CN 115540499A CN 202211171362 A CN202211171362 A CN 202211171362A CN 115540499 A CN115540499 A CN 115540499A
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tower
oxygen
pipeline
nitrogen
flash
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汤雁婷
郭泉辉
于欣
申文静
王文浩
蒋安琪
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Henan University
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Henan University
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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
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • 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
    • F25J3/0257—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 nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • 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
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/52—One fluid being oxygen enriched compared to air, e.g. "crude oxygen"

Abstract

The invention discloses a device and a method for producing high-purity nitrogen and ultrapure oxygen by flash evaporation waste gas low-temperature pressurization circulation. The invention aims to solve the problems that in the prior art, the single-tower rectification extraction rate is low, the energy consumption is high, and the conventional oxygen product cannot meet the purity requirement of ultrapure oxygen. The technology of recycling the nitrogen component in the flash evaporation waste gas and the compression work thereof by utilizing the low-temperature pressurization recycling of the flash evaporation waste gas reduces the energy consumption of nitrogen production. By utilizing the multistage rectification technology, high-purity nitrogen and ultrapure oxygen are simultaneously produced on the premise of not additionally increasing energy consumption. The device and the method for obtaining high-purity nitrogen and ultrapure oxygen through cryogenic separation have the advantages of low energy consumption, less investment, small occupied area, economy and reasonableness.

Description

Device and method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas
Technical Field
The invention relates to the field of air separation, in particular to a device and a method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas.
Background
With the development of high and new technology industries, high-purity gas has wide application in the fields of research and production of large-scale integrated circuits such as chips, smelting and treatment of high-purity metal, solar photovoltaic industry and the like. Especially, electronic gas has a very important position in the chip industry and the like, the qualification rate and the production cost of the chip are directly influenced, and the demand is continuously increased. The demand for electronic gases is mainly high-purity nitrogen, and other gases such as ultra-pure oxygen are also demanded. The gas is characterized by high and stable purity.
For impurities in nitrogen, high-purity nitrogen produced by cryogenic rectification is generally required to be introduced into a purifier for impurity removal. If a conventional or previously existing cryogenic rectification plant is used to produce high purity nitrogen. The traditional single-tower rectification process has low extraction rate and high energy consumption. The double-tower rectification process has high investment and complex operation.
However, the oxygen obtained by the general cryogenic rectification method cannot meet the requirement of electronic grade oxygen because the oxygen contains impurities such as argon, nitrous oxide, carbon dioxide, hydrocarbon and the like. Generally, a purifier is required to be further added for removing impurities, extra energy consumption is increased, and more industrial fields are occupied.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a device and a method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas. The nitrogen rectification adopts a single rectification tower with waste gas circulation. A flash tower is added to recover flash waste gas with the nitrogen content of more than 80%, the flash waste gas is recovered by low-temperature pressurization of a pressurization end of an expansion machine, and the flash waste gas circularly enters the lower part of a rectifying tower to recover nitrogen components and compression work of the flash waste gas to produce high-purity nitrogen. Meanwhile, an oxygen tower and an ultra-pure oxygen tower are additionally arranged, and qualified ultra-pure oxygen is obtained by utilizing a multi-stage rectification method.
The technical scheme of the invention is realized as follows:
a device for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas comprises an air compressor, a purification system and a cold box, wherein the cold box comprises a main heat exchanger, an expansion machine, a rectifying tower, a flash evaporation tower, an oxygen tower, an ultrapure oxygen tower, a pressure reducing valve and a jet evaporator; the air compressor is connected with the purification system through a first pipeline, a gas outlet of the purification system is communicated with a second pipeline, and the second pipeline is connected with the rectifying tower after passing through the main heat exchanger; the liquid outlet at the bottom of the rectifying tower is connected with the flash tower through a third pipeline; a gas outlet at the top of the rectifying tower is communicated with a fourth pipeline, a fifth pipeline, a seventh pipeline and a sixteenth pipeline, the fourth pipeline extends out of the cold box after passing through the main heat exchanger, the fifth pipeline is connected with an evaporator at the lower part of the oxygen tower, a liquid outlet of the evaporator in the oxygen tower is connected with a sixth pipeline, the sixth pipeline is connected with the top of the rectifying tower, the seventh pipeline is connected with the evaporator at the lower part of the flash tower, a liquid outlet of the evaporator in the flash tower is communicated with an eighth pipeline, and the eighth pipeline is connected with the top of the rectifying tower; a liquid outlet at the bottom of the flash tower is communicated with a ninth pipeline, the ninth pipeline is connected with the upper part of the oxygen tower after passing through the pressure reducing valve, a gas outlet at the top of the oxygen tower is communicated with a tenth pipeline, the tenth pipeline is connected with the expansion end of the expansion machine after passing through the main heat exchanger, and the injection evaporator is arranged on the tenth pipeline; an outlet of an expansion end of the expansion machine is communicated with an eleventh pipeline, and the eleventh pipeline is connected with the purification system after passing through the main heat exchanger; the gas phase outlet of the flash tower is connected with the pressurization end of the expansion machine through a twelfth pipeline; an outlet of the pressurization end of the expansion machine is communicated with a thirteenth pipeline, and the thirteenth pipeline is connected with the lower part of the rectifying tower after passing through the main heat exchanger; a gas outlet at the middle lower part of the oxygen tower is connected with the middle part of the ultrapure oxygen tower through a fourteenth pipeline; the liquid outlet at the bottom of the oxygen tower is connected with the jet evaporator through a fifteenth pipeline, a sixteenth pipeline is connected with the evaporator at the lower part of the ultrapure oxygen tower, the outlet of the evaporator at the lower part of the ultrapure oxygen tower is communicated with a seventeenth pipeline, and the seventeenth pipeline is connected with the condenser at the upper part of the ultrapure oxygen tower; a liquid outlet of the evaporator at the lower part of the oxygen tower is connected with a condenser at the upper part of the ultrapure oxygen tower through an eighteenth pipeline; a condenser gas outlet at the upper part of the ultrapure oxygen tower is connected with an outlet at the expansion end of the expansion machine through a twentieth pipeline, and a top gas outlet of the ultrapure oxygen tower is communicated with the twentieth pipeline through a nineteenth pipeline; and a twenty-first pipeline is communicated with a gas outlet at the lower part of the ultrapure oxygen tower, and extends to the outside of the cold box after passing through the main heat exchanger.
Further, the theoretical plate number of the rectifying tower is 35 to 50 or the corresponding actual plate number of the rectifying tower is 45 to 65.
Further, the theoretical plate number of the flash tower is 2~8 or the corresponding sieve plate tower with the actual tray number of 4-10 trays.
Further, the theoretical plate number of the oxygen tower is 20 to 30 or the corresponding actual plate number of the tower is 25 to 45, and the tower is a sieve plate tower or a structured packing tower.
Further, the theoretical plate number of the ultrapure oxygen tower is 20-30 or the corresponding actual plate number of the tower is 25-45 trays, and the tower is a sieve plate tower or a structured packing tower.
Further, the expander is a turbo expander.
A method for producing high-purity nitrogen and ultrapure oxygen by using the device comprises the following steps:
the compressed and purified air enters a main heat exchanger, is cooled by the return gas and then enters a rectifying tower; obtaining pure nitrogen at the top of the rectifying tower, reheating one part of the pure nitrogen as a nitrogen product by a main heat exchanger and then sending the nitrogen product out of a cold box, liquefying the second part of the nitrogen by an oxygen tower evaporator and then taking the liquefied nitrogen as reflux liquid to enter the rectifying tower, condensing and liquefying the third part of the nitrogen by a flash tower evaporator and then taking the nitrogen as reflux liquid to supplement the nitrogen into the rectifying tower, condensing and liquefying the fourth part of the nitrogen by a bottom evaporator of the ultra-pure oxygen tower, throttling and depressurizing the nitrogen to enter a top condenser of the ultra-pure oxygen tower, finally supplementing the nitrogen after being evaporated to enter a twentieth pipeline as regeneration waste gas, feeding oxygen-enriched liquid air at the bottom of the rectifying tower into the flash tower for flash evaporation, reducing the oxygen content of the liquid at the bottom of the flash tower and throttling the nitrogen by a pressure reducing valve to enter the oxygen tower as reflux liquid; the gas phase at the top of the oxygen tower enters the main heat exchanger for reheating and enters an expansion end of an expansion machine as expansion waste gas to provide cold energy for the whole device, and the expanded waste gas enters a purification system after being reheated by the main heat exchanger to serve as regeneration gas of the adsorbent; the gas phase at the top of the flash tower has high nitrogen content, enters a pressurizing end of an expander for pressurizing, and enters the lower part of the rectifying tower after being cooled by a main heat exchanger for directly recycling nitrogen components; the liquid at the bottom of the oxygen tower is vaporized by the waste gas at the top of the oxygen tower through the jet evaporator and enters the main heat exchanger to recover the cold energy of the liquid; leading out pure oxygen from the middle part of the oxygen tower and sending the pure oxygen into the middle part of the ultra-pure oxygen tower, wherein an evaporator heat source of the ultra-pure oxygen tower is from pressure nitrogen at the top of a rectifying tower, decompressing and sending the liquefied pure oxygen into a condenser at the top of the ultra-pure oxygen tower to be used as a cold source, and part of a supplementary cold source of the condenser of the ultra-pure oxygen tower is from liquefied liquid nitrogen of an evaporator at the bottom of the oxygen tower; the lower part of the ultra-pure oxygen tower leads out ultra-pure oxygen which is reheated by the main heat exchanger and then sent out of the cold box as a product.
Further, the working pressure of the rectifying tower is 0.4 to 1.5 MPa. The working pressure of the oxygen tower is 0.2 to 0.8 MPa. The working pressure of the ultrapure oxygen tower is 0.2 to 0.8 MPa. The working pressure of the flash tower is 0.3 to 1.2 MPa.
The technical scheme of the invention has the following positive effects:
the application utilizes the flash evaporation waste gas that comes out at the flash distillation tower top (current technology is as the direct discharge cold box of waste gas), utilizes the flash evaporation waste gas of expander pressure boost end low temperature pressure boost recovery high nitrogen content, and the circulation gets into the rectifying column and retrieves its nitrogen component and work of compression production high-purity nitrogen gas. Compared with the traditional single-tower low-temperature rectification flow: the extraction rate of nitrogen is improved by 10-15%, and the energy consumption is saved by 10-15%; the scale of the air compressor and the purification system is smaller than that of a single-tower process; the rectification part has complex structure; the whole investment is only slightly higher than that of a single-tower low-temperature rectification flow. High-purity nitrogen and ultra-pure oxygen are produced simultaneously on the premise of not increasing extra energy consumption.
Therefore, the process can not only maximally reduce investment and occupied area, reduce energy consumption and production cost, but also save human resources and investment, and is scientific and reasonable. The invention has important significance for improving economic benefits, and plays a positive role in saving social resources and creating a low-carbon and environment-friendly social environment.
Drawings
FIG. 1 is a schematic structural diagram of a device for producing high-purity nitrogen by low-temperature pressurization circulation of flash evaporation waste gas.
The labels in the figures are: 1. an air compressor; 2. a purification system; 3. a primary heat exchanger; 4. an expansion end of the turboexpander; 5. a turbo expander boost end; 6. a rectifying tower; 7. a flash column; 8. a pressure reducing valve; 9. an oxygen tower; 10. an ultra-pure oxygen column; 11. a jet evaporator; 12. a flash column evaporator; 13. an oxygen column evaporator; 14. an ultra-pure oxygen column evaporator; 15. an ultra-pure oxygen column condenser; 16. a cold box; 101. a first conduit; 102. a second conduit; 103. a third pipeline; 104. a fourth pipe; 105. a fifth pipeline; 106. a sixth pipeline; 107. a seventh pipe; 108. an eighth conduit; 109. a ninth conduit; 110. a tenth pipe; 111. an eleventh pipe; 112. a twelfth duct; 113. a thirteenth pipe; 114. a fourteenth pipe; 115. a fifteenth conduit; 116. a sixteenth pipe; 117. a seventeenth pipeline; 118. an eighteenth pipe; 119. a nineteenth pipe; 120. a twentieth pipe; 121. a twenty-first pipe.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to the accompanying drawings and examples.
The purification system is a very versatile technology and many, such as TSA or PSA, are possible and not required.
Example 1
A device for producing high-purity nitrogen and ultrapure oxygen by flash evaporation waste gas low-temperature pressurization circulation comprises an air compressor 1, a purification system 2 and a cold box 16, wherein the cold box comprises a main heat exchanger 3, turbo expanders 4 and 5, a rectifying tower 6, a flash tower 7, a pressure reducing valve 8, an oxygen tower 9, an ultrapure oxygen tower 10 and a jet evaporator 11, evaporators are arranged at the inner lower parts of the flash tower 7, the oxygen tower 9 and the ultrapure oxygen tower 10, and a condenser 15 is arranged at the inner upper part of the ultrapure oxygen tower 10; the air compressor 1 is connected with the purification system 2 through a first pipeline 101, and a gas outlet of the purification system 2 is connected with the rectifying tower 6 after passing through the main heat exchanger 3 through a second pipeline 102; the liquid outlet at the bottom of the rectifying tower 6 is connected with the flash tower 7 through a third pipeline 103; a gas outlet at the top of the rectifying tower 6 is communicated with a fourth pipeline 104, a fifth pipeline 105, a seventh pipeline 107 and a sixteenth pipeline 116, the fourth pipeline 104 extends out of the cold box 16 after passing through the main heat exchanger 3, the fifth pipeline 105 is connected with an evaporator 13 at the lower part of the oxygen tower 9, a liquid outlet of the evaporator 13 in the oxygen tower 9 is connected with a sixth pipeline 106, the sixth pipeline 106 is connected with the top of the rectifying tower 6, the seventh pipeline 107 is connected with an evaporator 12 at the lower part of the flash tower 7, a liquid outlet of the evaporator 12 in the flash tower 7 is communicated with an eighth pipeline 108, and the eighth pipeline 108 is connected with the top of the rectifying tower 6; a liquid outlet at the bottom of the flash tower 7 is communicated with a ninth pipeline 109, the ninth pipeline 109 is connected with the oxygen tower 9 after passing through the pressure reducing valve 8, a gas outlet at the top of the oxygen tower 9 is communicated with a tenth pipeline 110, the tenth pipeline 110 is connected with the expansion end 4 of the turboexpander after passing through the main heat exchanger 3, and the jet evaporator 11 is arranged on the tenth pipeline 110; an outlet of the expansion end 4 of the turboexpander is communicated with an eleventh pipeline 111, and the eleventh pipeline 111 is connected with the purification system 2 after passing through the main heat exchanger 3; the gas phase outlet of the flash tower 7 is connected with the boosting end 5 of the turboexpander through a twelfth pipeline 112; the outlet of the supercharging end 5 of the turboexpander is communicated with a thirteenth pipeline 113, and the thirteenth pipeline 113 is connected with the lower part of the rectifying tower 6 after passing through the main heat exchanger 3; the gas outlet at the middle lower part of the oxygen tower 9 is connected with the middle part of the ultrapure oxygen tower 10 through a fourteenth pipeline 114; the liquid outlet at the bottom of the oxygen tower 9 is connected with the jet evaporator 11 through a fifteenth pipeline 115, and the jet liquid is sent to the tenth pipeline 110 to be connected with the expansion end 4 of the turboexpander after passing through the main heat exchanger 3; a sixteenth pipeline 116 is connected with the evaporator 14 at the lower part of the ultrapure oxygen tower 10, and the liquefied ultrapure oxygen is sent to the condenser 15 at the upper part of the ultrapure oxygen tower 10 through a seventeenth pipeline 117; the liquid extracted by the evaporator 13 at the lower part of the oxygen tower 9 is sent to the condenser 15 at the upper part of the ultrapure oxygen tower 10 through an eighteenth pipeline 118; a gas outlet of the condenser 15 at the top of the ultrapure oxygen tower 10 is connected with an outlet of the expansion end 4 of the turboexpander through a twentieth pipeline 120, a nineteenth pipeline 119 is connected with the top of the ultrapure oxygen tower 10 in a gas manner, and the nineteenth pipeline 119 is communicated with the twentieth pipeline 120, so that the condensed gas at the top of the ultrapure oxygen tower 10 enters the purification system 2 after being reheated by the main heat exchanger 3 through an eleventh pipeline 111; a twenty-first pipeline 121 is communicated with a gas outlet at the lower part of the ultra-pure oxygen tower 10, and the twenty-first pipeline 121 extends out of the cold box 16 after passing through the main heat exchanger 3 so as to send out an ultra-pure oxygen product.
The working process of the device is as follows:
the raw material compressed air exhaust pressure of the air compressor 1 is 0.63MPaA, the oxygen content of the compressed and purified air is 20.95%, the nitrogen content is 78.118%, the argon content is 0.993%, and the rest is trace impurities such as carbon dioxide, hydrocarbon, nitrous oxide, carbon monoxide, hydrogen, other rare gases and the like, the pressure is 0.615MPaA, the temperature is 15 ℃, the air enters the main heat exchanger 3, is cooled to be close to the liquefaction temperature of-172 ℃ by the return flow gas, and then enters the rectifying tower 6. The rectifying tower 6 has operating pressure of 0.6MPaA and theoretical plate number of 50, and adopts a structured packing tower. The nitrogen with the purity of more than 99.99 percent is obtained at the top of the rectifying tower 6, one part of the nitrogen at the top of the rectifying tower 6 is taken as a nitrogen product, reheated by the main heat exchanger 3 to 13 ℃, sent out of the cold box 16, and further compressed for use according to the requirement, wherein the purity of the nitrogen product is more than 99.99 percent, and the pressure of the nitrogen product out of the cold box 16 is more than 0.57 MPaA. The second part of nitrogen enters an evaporator 13 in an oxygen tower 9 to be liquefied, the third part of nitrogen enters an evaporator 12 in a flash tower 7 to be condensed and liquefied, the pressure of the second part of nitrogen and the third part of nitrogen are maintained to be 0.6MPaA and the temperature of saturated liquid to be-176.9 ℃ after being liquefied, and the second part of nitrogen and the third part of nitrogen are merged and used as reflux to be supplemented to enter a rectifying tower 6. The fourth part enters an evaporator 14 in the ultra-pure oxygen tower 10 for condensation and liquefaction. 0.6MPaA of oxygen-enriched liquid air with oxygen content of 36.2 percent and nitrogen content of 62.3 percent is obtained at the bottom of the rectifying tower 6. The oxygen-enriched liquid air enters the flash tower 7 for flash evaporation, the operating pressure of the flash tower 7 is 0.39MPaA, and the pressure energy of flash evaporation waste gas is fully utilized as much as possible. The theoretical plate number of the flash tower 7 is set to 5, and the sieve plate tower is adopted to save the cost. The heavy component oxygen is further enriched at the bottom of the flash tower 7 after flash evaporation, the oxygen content of the bottom liquid is 44.5%, the pressure is 0.392MPaA, and the temperature of the saturated liquid is-177.5 ℃. However, the heavy component is enriched not only with oxygen, but also other impurity heavy components, for example, with an argon content >1.8%, a hydrocarbon content >50ppm, a carbon dioxide content >0.5ppm, and a nitrous oxide content >0.2ppm. The oxygen-enriched liquid at the bottom of the flash tower 7 is decompressed and throttled to 0.245MPaA by a pressure reducing valve 8, enters the top of an oxygen tower 9 at the temperature of-183.3 ℃ and is used as a raw material liquid. The nitrogen content of the top gas phase flash waste gas of the flash tower 7 is as high as 81.5%, the oxygen content is 17.5%, the rest is impurities such as argon, and the higher pressure is maintained at 0.39MPaA, the flash waste gas with the saturated gas temperature of-178.4 ℃ is extracted from the condenser 15 at the upper part of the flash tower 7, the flash waste gas is reheated to-174 ℃ by the main heat exchanger 3 and then enters the pressurization end of the turboexpander to be pressurized to 5-0.605 MPaA which is higher than the operation pressure of the rectifying tower 6, and the temperature after pressurization is-155.3 ℃. After being pressurized, the waste gas is cooled to the temperature close to the saturation temperature of-173 ℃ by the main heat exchanger 3 and then enters the lower part of the rectifying tower 6 to directly recycle the nitrogen component. The oxygen column 9 was operated at a pressure of 0.245MPaA and was a structured packed column having 30 theoretical plates. The gas phase at the top of the oxygen tower 9 is saturated gas with the main components of oxygen content of 42.4%, nitrogen content of 55.5%, argon content of 2% and pressure of 0.245MPaA, and the gas enters the main heat exchanger 3 to be reheated to-169 ℃ and enters the expansion end 4 of the turboexpander as expansion waste gas to provide cold energy for the whole device. The pressure of the expanded waste gas is 0.125MPaA, the temperature is-183.6 ℃, and the expanded waste gas is reheated to 13 ℃ by a main heat exchanger 3 and then enters a purification system 2 to be used as the regeneration gas of the adsorbent. The components of the regeneration waste gas are all from air, the carbon dioxide content of the main desorption medium is 500ppm, and the regeneration waste gas is directly discharged into the atmosphere at a high-point safe position. In the liquid oxygen at the bottom of the oxygen tower 9, heavy components such as hydrocarbon are further concentrated, and are led out in time for safe operation, vaporized by waste gas through a jet evaporator 11 and heated to-180 ℃, and enter the main heat exchange 3 to recover the cold energy. Pure oxygen gas is extracted from the middle lower part of the oxygen tower 9 and enters the middle part of the ultra-pure oxygen tower 10 as the raw material gas thereof. At the moment, heavy components in the oxygen are removed, but light component impurities such as argon, nitrogen, hydrogen and the like still do not meet the requirement of ultra-pure oxygen. The ultra pure oxygen column 10 was operated at a pressure of 0.24MPaA and was a structured packed column with 20 theoretical plates. The heat source of the lower evaporator 14 of the ultra-pure oxygen column 10 is pressure nitrogen at the top of the rectification column 6, namely, the fourth part, the pressure after liquefaction is 0.6MPaA, and the temperature is-176.9 ℃. The part of the liquid nitrogen is throttled and decompressed and then sent into a condenser 15 at the upper part of an ultrapure oxygen tower 10 to be used as a cold source, part of the supplementary cold source of the condenser 15 is from liquefied liquid nitrogen of an evaporator 13 at the lower part of an oxygen tower 9, and the two liquid nitrogen streams are converged and then controlled at the pressure of 0.15MPaA and the temperature of-192 ℃. A small amount of light component waste gas is led out from the top of the ultra-pure oxygen tower 10, and the main components of the waste gas are controlled to contain 60 percent of oxygen and 40 percent of argon. The light component waste gas is converged into nitrogen gas which is evaporated by a condenser of an ultra-pure oxygen tower 10, the pressure is 0.15MPaA, the temperature is-192 ℃, then the converged expanded waste gas is reheated to 12 ℃ by a main heat exchanger 3, and the reheated waste gas is used as regeneration gas of a purification system 2. The ultrapure oxygen is led out from the lower part of the ultrapure oxygen tower 10, the purity is more than or equal to 99.9999 percent, the pressure is 0.24MPaA, the ultrapure oxygen is reheated to 12 ℃ by a main heat exchanger 3 and is sent out of a cold box 16 as a product, the pressure is 0.23MPaA, and the ultrapure oxygen can be bottled or compressed for use according to requirements. The production of ultrapure oxygen is mainly based on demand, with extraction rates <10%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that modifications can be made by those skilled in the art without departing from the principle of the present invention, and these modifications should also be construed as the protection scope of the present invention.

Claims (10)

1. The utility model provides a device of high-purity nitrogen gas of flash distillation waste gas low temperature pressure boost circulation production and ultrapure oxygen which characterized in that: the system comprises an air compressor, a purification system and a cold box, wherein the cold box comprises a main heat exchanger, an expansion machine, a rectifying tower, a flash tower, an oxygen tower, an ultra-pure oxygen tower, a pressure reducing valve and a jet evaporator, the evaporators are arranged at the lower parts in the flash tower, the oxygen tower and the ultra-pure oxygen tower, and a condenser is arranged at the upper part in the ultra-pure oxygen tower; the air compressor is connected with the purification system through a first pipeline, a gas outlet of the purification system is communicated with a second pipeline, and the second pipeline is connected with the rectifying tower after passing through the main heat exchanger; the liquid outlet at the bottom of the rectifying tower is connected with the flash tower through a third pipeline; a gas outlet at the top of the rectifying tower is communicated with a fourth pipeline, a fifth pipeline, a seventh pipeline and a sixteenth pipeline, the fourth pipeline extends out of the cold box after passing through the main heat exchanger, the fifth pipeline is connected with an evaporator at the lower part of the oxygen tower, a liquid outlet of the evaporator in the oxygen tower is connected with a sixth pipeline, the sixth pipeline is connected with the top of the rectifying tower, the seventh pipeline is connected with the evaporator at the lower part of the flash tower, a liquid outlet of the evaporator in the flash tower is communicated with an eighth pipeline, and the eighth pipeline is connected with the top of the rectifying tower; a liquid outlet at the bottom of the flash tower is communicated with a ninth pipeline, the ninth pipeline is connected with the upper part of the oxygen tower after passing through the pressure reducing valve, a gas outlet at the top of the oxygen tower is communicated with a tenth pipeline, the tenth pipeline is connected with the expansion end of the expansion machine after passing through the main heat exchanger, and the injection evaporator is arranged on the tenth pipeline; an outlet of an expansion end of the expansion machine is communicated with an eleventh pipeline, and the eleventh pipeline is connected with the purification system after passing through the main heat exchanger; the gas phase outlet of the flash tower is connected with the pressurization end of the expansion machine through a twelfth pipeline; an outlet of the pressurization end of the expansion machine is communicated with a thirteenth pipeline, and the thirteenth pipeline is connected with the lower part of the rectifying tower after passing through the main heat exchanger; a gas outlet at the middle lower part of the oxygen tower is connected with the middle part of the ultrapure oxygen tower through a fourteenth pipeline; the liquid outlet at the bottom of the oxygen tower is connected with the jet evaporator through a fifteenth pipeline, a sixteenth pipeline is connected with the evaporator at the lower part of the ultrapure oxygen tower, the outlet of the evaporator at the lower part of the ultrapure oxygen tower is communicated with a seventeenth pipeline, and the seventeenth pipeline is connected with the condenser at the upper part of the ultrapure oxygen tower; a liquid outlet of the evaporator at the lower part of the oxygen tower is connected with a condenser at the upper part of the ultrapure oxygen tower through an eighteenth pipeline; a condenser gas outlet at the upper part of the ultrapure oxygen tower is connected with an outlet at the expansion end of the expansion machine through a twentieth pipeline, and a top gas outlet of the ultrapure oxygen tower is communicated with the twentieth pipeline through a nineteenth pipeline; and a gas outlet at the lower part of the ultra-pure oxygen tower is communicated with a twenty-first pipeline, and the twenty-first pipeline extends out of the cold box after passing through the main heat exchanger.
2. The apparatus for producing high purity nitrogen and ultra pure oxygen with flash off gas low temperature pressurization cycle according to claim 1, wherein: the theoretical plate number of the rectifying tower is 35 to 50, or the corresponding actual plate number of the rectifying tower is 45 to 65.
3. The apparatus for producing high purity nitrogen and ultra pure oxygen by cryogenic pressure boost recycle of flash off gas according to claim 1, wherein: the theoretical plate number of the flash tower is 2~8 or the sieve plate tower corresponding to the actual tray number of the flash tower is 4-10 trays.
4. The apparatus for producing high purity nitrogen and ultra pure oxygen with flash off gas low temperature pressurization cycle according to claim 1, wherein: the theoretical plate number of the oxygen tower is 20 to 30 or the corresponding actual tray number of the oxygen tower is 25 to 45 trays.
5. The apparatus for producing high purity nitrogen and ultra pure oxygen with flash off gas low temperature pressurization cycle according to claim 1, wherein: the theoretical plate number of the ultrapure oxygen tower is 20-30 or the sieve plate tower or the structured packed tower corresponding to the actual tower disc number is 25-45.
6. Method for producing high purity nitrogen and ultra pure oxygen using the apparatus according to any one of claims 1 to 5, characterized in that: the process is as follows: the compressed and purified air enters a main heat exchanger, is cooled by the return gas and then enters a rectifying tower; obtaining pure nitrogen at the top of the rectifying tower, reheating one part of the pure nitrogen as a nitrogen product by a main heat exchanger and then sending the nitrogen product out of a cold box, liquefying the second part of nitrogen by an oxygen tower evaporator and then sending the nitrogen product into the rectifying tower as reflux, condensing and liquefying the third part of nitrogen by a flash tower evaporator and then supplementing the liquefied nitrogen into the rectifying tower as reflux, sending the fourth part of nitrogen into a bottom evaporator of the ultra-pure oxygen tower for condensation and liquefaction, throttling and depressurizing the nitrogen and then sending the nitrogen and the liquefied nitrogen into a condenser at the top of the ultra-pure oxygen tower, finally supplementing the nitrogen and the nitrogen into a twentieth pipeline after evaporation as regeneration waste gas, sending oxygen-enriched liquid air at the bottom of the rectifying tower into the flash tower for flash evaporation, reducing the oxygen content of the liquid at the bottom of the flash tower and then sending the liquid into the oxygen tower as reflux after pressure reduction and throttling by a pressure reducing valve; the gas phase at the top of the oxygen tower enters the main heat exchanger for reheating and enters an expansion end of an expansion machine as expansion waste gas to provide cold energy for the whole device, and the expanded waste gas enters a purification system after being reheated by the main heat exchanger to serve as regeneration gas of the adsorbent; the top gas phase of the flash tower has high nitrogen content, enters the pressurizing end of the expansion machine for pressurizing, and enters the lower part of the rectifying tower after being cooled by the main heat exchanger for directly recycling the nitrogen component; the liquid at the bottom of the oxygen tower is vaporized by the waste gas at the top of the oxygen tower through the jet evaporator and enters the main heat exchanger to recover the cold energy of the liquid; leading out pure oxygen from the middle part of the oxygen tower and sending the pure oxygen into the middle part of the ultra-pure oxygen tower, wherein an evaporator heat source of the ultra-pure oxygen tower is from pressure nitrogen at the top of a rectifying tower, decompressing and sending the liquefied pure oxygen into a condenser at the top of the ultra-pure oxygen tower to be used as a cold source, and part of a supplementary cold source of the condenser of the ultra-pure oxygen tower is from liquefied liquid nitrogen of an evaporator at the bottom of the oxygen tower; the lower part of the ultra-pure oxygen tower leads out ultra-pure oxygen which is reheated by the main heat exchanger and then sent out of the cold box as a product.
7. The method of producing high purity nitrogen and ultrapure oxygen of claim 6 wherein: the working pressure of the rectifying tower is 0.4 to 1.5 MPa.
8. The method of producing high purity nitrogen and ultrapure oxygen of claim 6 wherein: the working pressure of the oxygen tower is 0.2 to 0.8 MPa.
9. The method of producing high purity nitrogen and ultrapure oxygen of claim 6 wherein: the working pressure of the ultrapure oxygen tower is 0.2 to 0.8 MPa.
10. The method of producing high purity nitrogen and ultrapure oxygen of claim 6 wherein: the working pressure of the flash tower is 0.3 to 1.2 MPa.
CN202211171362.8A 2022-09-26 2022-09-26 Device and method for producing high-purity nitrogen and ultrapure oxygen by low-temperature pressurization circulation of flash evaporation waste gas Pending CN115540499A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115790077A (en) * 2023-02-03 2023-03-14 杭氧集团股份有限公司 Device for preparing high-purity nitrogen and ultra-pure oxygen and using method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115790077A (en) * 2023-02-03 2023-03-14 杭氧集团股份有限公司 Device for preparing high-purity nitrogen and ultra-pure oxygen and using method thereof

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