CN215295547U - Production device for producing ultra-pure oxygen and liquid nitrogen by adopting pre-cooling system - Google Patents

Production device for producing ultra-pure oxygen and liquid nitrogen by adopting pre-cooling system Download PDF

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Publication number
CN215295547U
CN215295547U CN202121644202.1U CN202121644202U CN215295547U CN 215295547 U CN215295547 U CN 215295547U CN 202121644202 U CN202121644202 U CN 202121644202U CN 215295547 U CN215295547 U CN 215295547U
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raw material
tower
oxygen
rectifying tower
liquid nitrogen
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CN202121644202.1U
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Inventor
郑梦杰
闫红伟
李灏
崔增涛
银延蛟
张亚清
吕书山
郭俊磊
米圣伟
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Henan Xinlianxin Shenleng Energy Co ltd
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Henan Xinlianxin Shenleng Energy Co ltd
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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
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0012—Primary atmospheric gases, e.g. air
    • F25J1/0015—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0012—Primary atmospheric gases, e.g. air
    • F25J1/0017—Oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/0035—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work
    • F25J1/0037—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by gas expansion with extraction of work of a return stream
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    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
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    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
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    • F25J1/0205—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle as a dual level SCR refrigeration cascade
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    • F25J1/0208—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a single-component refrigerant [SCR] fluid in a closed vapor compression cycle in combination with an internal quasi-closed refrigeration loop, e.g. with deep flash recycle loop
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    • F25J1/0228—Coupling of the liquefaction unit to other units or processes, so-called integrated processes
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    • F25J1/0279—Compression of refrigerant or internal recycle fluid, e.g. kind of compressor, accumulator, suction drum etc.
    • F25J1/0292—Refrigerant compression by cold or cryogenic suction of the refrigerant gas
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    • F25J2210/42—Nitrogen
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    • 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
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    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

Abstract

The utility model belongs to a production device which adopts a precooling system to produce hyperpure oxygen and liquid nitrogen; the system comprises an ultra-pure oxygen production system and a liquid nitrogen preparation system, wherein the ultra-pure oxygen production system comprises an oxygen raw material storage tank, and the oxygen raw material storage tank is connected with the ultra-pure oxygen storage tank through a raw material heat exchange unit and a thermal coupling rectifying tower; the liquid nitrogen preparation system and the cold energy supply system respectively provide cold energy for the raw material heat exchange unit; the liquid nitrogen preparation system respectively provides cold energy for the thermal coupling rectifying tower and a top condenser at the top of the thermal coupling rectifying tower; the device has the advantages of simple structure, reasonable flow design, adoption of upper and lower towers and a circulating refrigeration process, small occupied area, less investment, stable product and capability of producing liquid nitrogen as a byproduct while obtaining an ultra-pure oxygen product.

Description

Production device for producing ultra-pure oxygen and liquid nitrogen by adopting pre-cooling system
Technical Field
The utility model belongs to the technical field of the coupling production of super pure liquid oxygen and liquefied nitrogen, concretely relates to adopt precooling system to produce apparatus for producing super pure oxygen and liquid nitrogen.
Background
The application of the ultra-pure oxygen to the fields of semiconductor elements, integrated circuits, photovoltaic industry and the like has great application prospect, but the industrial preparation of the ultra-pure oxygen has great difficulty; as is known, air is an inexhaustible source for industrial oxygen production, and four methods, namely a low-temperature rectification method, a normal-temperature pressure swing adsorption method, a membrane separation method and a high-temperature alkaline molten salt catalytic absorption method, can be adopted for oxygen generation through air separation. Because air mainly comprises nitrogen, oxygen, argon, carbon dioxide, methane, oxygen and the like, industrial oxygen prepared by an air separation method has complex composition, particularly contains impurities such as argon, nitrogen and the like which are difficult to remove by a normal-temperature separation method, and the difficulty of preparing the ultra-pure oxygen by using the industrial oxygen as a raw material is very high. Based on this, the industry mainly adopts the cryogenic rectification method to produce the ultrapure oxygen, but the oxygen is required to be liquefied and in a low-temperature state in the process of producing the ultrapure oxygen so as to achieve the purpose of rectification and purification, a large amount of cold energy is consumed invisibly, and the defects of cold energy waste, oxygen emptying and the like are also caused.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to overcome the defect among the prior art, and provide a simple structure, flow reasonable in design, adopt about tower and circulation refrigeration technology, device area little, the small investment, the product is stable, can by-product liquid nitrogen adopt the apparatus for producing super pure oxygen and liquid nitrogen of precooling system when obtaining super pure oxygen product.
The purpose of the utility model is realized like this:
a production device for producing ultra-pure oxygen and liquid nitrogen by adopting a precooling system comprises an ultra-pure oxygen production system,
the ultra-pure oxygen production system comprises an oxygen raw material storage tank, wherein the oxygen raw material storage tank is connected with the ultra-pure oxygen storage tank through a raw material heat exchange unit and a thermal coupling rectifying tower;
the liquid nitrogen preparation system and the cold energy supply system respectively provide cold energy for the raw material heat exchange unit;
the liquid nitrogen preparation system respectively provides cold energy for the thermal coupling rectifying tower and the top condenser at the top of the thermal coupling rectifying tower.
Preferably, the thermally coupled rectifying tower comprises a lower rectifying tower and an upper rectifying tower arranged at the top of the lower rectifying tower;
the export of raw materials heat transfer unit links to each other with the first feed liquid import of lower column rectifying column in the lower column rectifying column, and the gas phase export at the lower column rectifying column top links to each other with the last tower reboiler and the last rectifying column feed gas import of last rectifying column respectively through the second tee bend, and the last rectifying column liquid phase export of last rectifying column bottom links to each other with super pure oxygen storage tank.
Preferably, a fifth regulating valve is arranged between the second tee joint and the upper tower reboiler, and a sixth regulating valve is arranged between the second tee joint and the feed gas inlet of the upper tower rectifying tower.
Preferably, a liquid phase outlet at the bottom of the rectifying tower of the lower tower is connected with the liquid oxygen normal pressure storage tank through a ninth regulating valve;
an outlet of the upper tower reboiler is connected with a second raw material liquid inlet of the lower tower rectifying tower at the upper part of the lower tower rectifying tower;
a gas phase outlet at the top of the upper rectifying tower is connected with a raw material liquid inlet of the upper rectifying tower through a tube side of a top condenser and a tenth regulating valve;
a seventh regulating valve is arranged between a liquid phase outlet at the bottom of the upper tower rectifying tower and the ultrapure oxygen storage tank, and an outlet of the ultrapure oxygen storage tank is connected with a filling row through a filling pump;
a third tee joint is arranged between the tube pass of the top condenser and the tenth regulating valve, a fourth tee joint is arranged between the outlet of the upper tower reboiler and the inlet of the second raw material liquid of the lower tower rectifying tower, and a near pipeline is arranged between the third end of the third tee joint and the third end of the fourth tee joint.
Preferably, the raw material heat exchange unit comprises a precooler and a main heat exchanger, and the oxygen raw material storage tank is connected with the first raw material liquid inlet of the lower tower rectifying tower through the first raw material gas inlet of the precooler, the first raw material gas outlet of the precooler, the first raw material gas inlet of the main heat exchanger, the first raw material gas outlet of the main heat exchanger and the eighth regulating valve.
Preferably, the liquid nitrogen preparation system comprises a nitrogen compressor, and an outlet of the nitrogen compressor is sequentially connected with a second raw material gas inlet of the precooler, a second raw material gas outlet of the precooler, a second raw material gas inlet of the main heat exchanger, a second raw material gas outlet of the main heat exchanger, a second regulating valve and a liquid nitrogen normal-pressure storage tank through a four-way joint.
Preferably, the third end of the four-way joint is connected with the inlet of the nitrogen compressor sequentially through a first regulating valve, a lower tower reboiler, a fourth regulating valve, the shell pass of the top condenser, the third raw material gas inlet of the precooler, the third raw material gas outlet of the precooler and a first tee joint, and an air inlet pipeline with a nitrogen raw material storage tank is arranged between the first tee joint and the inlet of the nitrogen compressor.
Preferably, the fourth end of the four-way joint is connected with the third end of the first three-way joint sequentially through the nitrogen expansion compressor, the raw material inlet of the main heat exchanger and the raw material outlet of the main heat exchanger.
Preferably, the cold energy supply system comprises an R23 refrigerant tank, and the outlet of the R23 refrigerant tank is connected with the inlet of the R23 refrigerant tank through a third regulating valve, a precooler raw material inlet of the precooler, a precooler raw material outlet and an R23 compressor.
The production device for producing the ultra-pure oxygen and the liquid nitrogen by adopting the precooling system is prepared according to the scheme, and the ultra-pure oxygen purification process and the device for producing the liquid nitrogen rich in the ultra-pure oxygen with the product purity not lower than 99.9999 percent are stably produced by adopting a raw material for providing the ultra-pure oxygen by adopting industrial-grade low-pressure oxygen, and utilizing the working principles of R23 working medium refrigeration and expander refrigeration and utilizing upper and lower tower coupling rectification. Compared with the traditional process technology, the utility model has the advantages of as follows: 1. the R23 working medium is adopted for refrigeration, the oxygen and nitrogen raw materials are cooled for the first time, and the liquefaction of the oxygen and the nitrogen is realized after the cold energy of the expander is exchanged, so that the energy consumption is saved, and the environmental protection is facilitated; 2. the ultra-pure oxygen device adopts an upper tower and lower tower coupling rectification technology to obtain an ultra-pure oxygen product, the ultra-pure oxygen product is stored in an ultra-pure oxygen storage tank and then is used for filling bottled gas through a liquid pump, so that the ultra-pure liquid product and the ultra-pure gas product can be sold outside, and the sales requirements of tank cars and bottled gas are met; 3. the purity of the product can reach more than 99.9999 percent, the dependence of the domestic semiconductor industry on imported ultra-pure oxygen is solved, sufficient raw materials are provided for the research of the domestic semiconductor industry and the electronic special gas industry, and the development of economic and social benefits is promoted; 4. The utility model has high energy integration, in particular to a lower tower top gas which provides a heat source for an upper tower reboiler, reduces the load of a nitrogen compressor and reduces the energy consumption of the device; 5. the utility model also comprises the design of a pre-cooling system, which can greatly reduce the circulation volume of the nitrogen compressor, further reduce the energy consumption of unit products, is favorable for the balance of system load and is convenient for operation; 6. simultaneously the utility model discloses can reach the technology that working medium circulation recycled and oxygen nitrogen gas do not have the unloading, the cold volume utilization maximize of device, the super pure oxygen of liquid of production is applied to fields such as semiconductor element and integrated circuit, photovoltaic trade, and the liquid nitrogen is used for other devices to consume or sell outward to and reach the characteristics of sparingly investing in and manufacturing cost.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural diagram of the thermal coupling rectifying tower of the present invention.
In the upper diagram:
1. an oxygen raw material storage tank; 2. A precooler; 3. A primary heat exchanger; 4. a lower rectifying tower; 5. Feeding the obtained product to a rectifying tower; 6. A top condenser; 7. a lower column reboiler; 8. A reboiler at the upper tower; 9. An ultra-pure oxygen storage tank; 10. A filling pump; 11. filling rows; 12. a R23 compressor; 13. r23 refrigerant tank; 14. a nitrogen compressor; 15. a nitrogen expander; 16. a liquid oxygen normal pressure storage tank; 17. a liquid nitrogen normal pressure storage tank; 18. a fifth regulating valve; 19. a sixth regulating valve; 20. a tenth regulating valve; 21. a seventh regulating valve; 22. a first regulating valve; 23. a fourth regulating valve; 24. a third regulating valve; 25. a second regulating valve; 26. a ninth regulating valve; 27. A first raw material liquid inlet of the lower rectifying tower; 28. A precooler first feed gas inlet; 29. A raw material liquid inlet of the upper rectifying tower; 30. a precooler second feed gas outlet; 31. a liquid phase outlet of the upper rectifying tower; 32. a second raw material liquid inlet of the lower rectifying tower; 33. A second raw material gas outlet of the main heat exchanger; 34. A feed gas inlet of the upper rectifying tower; 35. A precooler raw material inlet; 36. A precooler third raw gas inlet 36; 37. A first tee joint; 38. Four-way connection; 39. a main heat exchanger raw material inlet; 40. A precooler second feed gas inlet; 41. A second feed gas inlet of the main heat exchanger; 42. a precooler first feed gas outlet; 43. A primary heat exchanger first feed gas inlet; 44. A first feed gas outlet of the main heat exchanger; 45. A nitrogen raw material storage tank; 46. an eighth regulating valve; 47. a second tee joint; 48. A precooler raw material outlet; 49. a main heat exchanger raw material outlet; 50. a third tee joint; 51. a fourth tee joint; 52. a near-road pipeline; 53. and a third raw material gas outlet of the precooler.
Detailed Description
In order to clearly understand the technical features, objects, and effects of the present invention, embodiments of the present invention will be described with reference to the accompanying drawings, in which like reference numerals refer to like parts in the drawings. For the sake of simplicity, only the parts related to the utility model are schematically shown in the drawings, and they do not represent the actual structure as a product.
As shown in fig. 1 and 2, the utility model relates to a production device for producing ultra-pure oxygen and liquid nitrogen by using a precooling system, which comprises an ultra-pure oxygen production system, wherein the ultra-pure oxygen production system comprises an oxygen raw material storage tank 1, and the oxygen raw material storage tank 1 is connected with an ultra-pure oxygen storage tank 9 through a raw material heat exchange unit and a thermal coupling rectifying tower; the liquid nitrogen preparation system and the cold energy supply system respectively provide cold energy for the raw material heat exchange unit; the liquid nitrogen preparation system respectively provides cold energy for the thermal coupling rectifying tower and the top condenser 6 at the top of the thermal coupling rectifying tower.
Further, the thermally coupled rectifying tower comprises a lower tower rectifying tower 4 and an upper tower rectifying tower 5 arranged at the top of the lower tower rectifying tower 4; the outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet 27 of a lower tower rectifying tower in the lower tower rectifying tower 4, a gas phase outlet at the top of the lower tower rectifying tower 4 is respectively connected with a raw material gas inlet 34 of an upper tower rectifying tower of an upper tower reboiler 8 and an upper tower rectifying tower 5 through a second tee 47, and a raw material 31 at the bottom of the upper tower rectifying tower 5 is connected with an ultra-pure oxygen storage tank 9.
Further, a fifth regulating valve 18 is arranged between the second tee 47 and the upper tower reboiler 8, and a sixth regulating valve 19 is arranged between the second tee 47 and the upper tower rectifying tower raw material gas inlet 34 of the upper tower rectifying tower 5.
Further, a liquid phase outlet at the bottom of the lower rectifying tower 4 is connected with the liquid oxygen normal pressure storage tank 16 through a ninth regulating valve 26; the outlet of the upper tower reboiler 8 is connected with the second raw material liquid inlet 32 of the lower tower rectifying tower at the upper part of the lower tower rectifying tower 4; a gas phase outlet at the top of the upper rectifying tower 5 is connected with an upper rectifying tower raw material liquid inlet 29 of the upper rectifying tower 5 through a tube pass of the top condenser 6 and a tenth regulating valve 20; a seventh regulating valve 21 is arranged between a liquid phase outlet at the bottom of the upper tower rectifying tower 5 and the ultrapure oxygen storage tank 9, and an outlet of the ultrapure oxygen storage tank 9 is connected with a charging row 11 through a charging pump 10; a third tee 50 is arranged between the tube pass of the top condenser 6 and the tenth regulating valve 20, a fourth tee 51 is arranged between the outlet of the upper tower reboiler 8 and the second raw material liquid inlet 32 of the lower tower rectifying tower, and a near pipeline 52 is arranged between the third end of the third tee 50 and the third end of the fourth tee 51.
Further, the raw material heat exchange unit comprises a precooler 2 and a main heat exchanger 3, and the oxygen raw material storage tank 1 is connected with the first raw material liquid inlet 27 of the lower rectifying tower through a first raw material gas inlet 28 of the precooler 2, a first raw material gas outlet 42 of the precooler, a first raw material gas inlet 43 of the main heat exchanger 3, a first raw material gas outlet 44 of the main heat exchanger and an eighth regulating valve 46.
Further, the liquid nitrogen preparation system comprises a nitrogen compressor 14, and an outlet of the nitrogen compressor 14 is connected with a second raw material gas inlet 40 of the precooler 2, a second raw material gas outlet 30 of the precooler, a second raw material gas inlet 41 of the main heat exchanger 3, a second raw material gas outlet 33 of the main heat exchanger, a second regulating valve 25 and the liquid nitrogen normal-pressure storage tank 17 through a four-way connection 38 in sequence.
Further, the third end of the four-way joint 38 is connected with the inlet of the nitrogen compressor 14 sequentially through a first regulating valve 22, a lower tower reboiler 7, a fourth regulating valve 23, the shell pass of the top condenser 6, a precooler third raw material gas inlet 36 of the precooler 2, a precooler third raw material gas outlet 53 and a first three-way joint 37, and an air inlet pipeline with a nitrogen raw material storage tank 45 is arranged between the first three-way joint 37 and the inlet of the nitrogen compressor 14.
Further, the fourth end of the four-way joint 38 is connected with the third end of the first three-way joint 37 sequentially through the nitrogen expansion compressor 15, the main heat exchanger raw material inlet 39 and the main heat exchanger raw material outlet 49 of the main heat exchanger 3.
Further, the refrigeration capacity supply system comprises an R23 refrigerant tank 13, and an outlet of the R23 refrigerant tank 13 is connected to an inlet of the R23 refrigerant tank 13 through a third regulating valve 24, a precooler raw material inlet 35 of the precooler 2, a precooler raw material outlet 48 and an R23 compressor 12.
A production process of a production device for producing ultra-pure oxygen and liquid nitrogen by adopting a precooling system comprises the following steps:
the method comprises the following steps: the raw material oxygen in the oxygen raw material storage tank 1 is precooled by a precooler 2, enters a main heat exchanger 3 for continuous cooling, and enters a lower tower rectifying tower 4 from a first raw material liquid inlet 27 in the lower tower rectifying tower 4; the temperature of the raw material oxygen is as follows: 20-30 ℃, and the pressure is as follows: 0.5Mpa, flow: 5000Nm/h, gas phase fraction: 1, oxygen mole fraction: 99.5-99.6%;
step two: performing primary rectification purification on the raw material liquid entering the lower rectifying tower 4 in the step one, and respectively entering the gas phase after rectification purification into an upper tower reboiler 8 and an upper tower rectifying tower 5 through a second tee 47; the temperature of a gas phase outlet at the top of the lower tower rectifying tower 4 is as follows: -175 to-177 ℃, and the oxygen molar fraction is as follows: 99.9-99.95%;
step three: in the second step, the gas phase enters an upper tower rectifying tower 5 and then is subjected to secondary rectification, and the liquid phase after the secondary rectification enters an ultrapure oxygen storage tank 9 through a liquid phase outlet 31 of the upper tower rectifying tower and then enters a charging row 11 through a charging pump 10; the liquid phase temperature after the secondary rectification and purification is as follows: the temperature is-181 to-183 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999 percent;
step four: in the second step, the liquid phase which is subjected to the primary rectification in the lower rectifying tower 4 enters the liquid oxygen normal pressure storage tank 16 through a liquid phase outlet at the bottom of the lower rectifying tower 4 and a ninth regulating valve 26 to be subjected to industrial oxygen recovery;
step five: the gas phase after the secondary rectification in the third step is liquefied through the tube pass heat exchange of the top condenser 6 and then enters a third tee joint 50, and a part of the gas phase enters the upper rectifying tower 5 through a tenth regulating valve 20 and a raw material liquid inlet 29 of the upper rectifying tower to flow back; the temperature of the raw material liquid inlet 29 of the upper rectifying tower is-181.5 to-183.5 ℃; another part enters a fourth tee 51 through a near pipeline 52; in the second step, the material passing through the upper tower reboiler 8 enters a fourth tee 51; the two are converged in a fourth tee 51 and then flow back to the lower rectifying tower 4 through a second raw material liquid inlet 32 of the lower rectifying tower;
step six: the refrigerant R23 in the R23 refrigerant tank 13 is throttled by the third regulating valve 24, and then reheated by the precooler raw material inlet 35 and the precooler raw material outlet 48 of the precooler 2, and then enters the R23 refrigerant tank 13 through the R23 compressor 12 and the inlet of the R23 refrigerant tank 13; the temperature at the inlet of the R23 compressor 12 is: -48 to-50 ℃, and R23 mole fraction is: 100 percent;
step seven: the compressed nitrogen in the outlet of the nitrogen compressor 14 sequentially enters the liquid nitrogen normal pressure storage tank 17 together with the precooler second raw material gas inlet 40, the precooler second raw material gas outlet 30, the main heat exchanger second raw material gas inlet 41, the main heat exchanger second raw material gas outlet 33 and the second regulating valve 25 of the precooler 2 through the four-way joint 38; the temperature of the second raw material gas outlet 33 of the main heat exchanger is as follows: -182 to-184 ℃, pressure: 0.01 to 0.03 mPAG;
step eight: the compressed nitrogen in the third end of the cross in the seventh step enters through the first regulating valve 22The lower tower reboiler 7 exchanges heat with the lower tower rectifying tower 4, the heat exchanged heat is throttled by the fourth regulating valve 23 and then is supplied to the top condenser 6 to provide cold energy, the heat exchanged heat is exchanged again with the gas phase from the upper tower rectifying tower 5 in the top condenser 6, and the heat exchanged heat again enters the nitrogen compressor 14 through the shell pass of the top condenser 6, the third raw material gas inlet 36 of the precooler 2, the third raw material gas outlet 53 of the precooler and the first tee joint 37 in sequence to form circulation; the temperature of precooler third raw material gas inlet 36 of precooler 2 is: -184 to-187 ℃, flow rate: 4000 to 4200Nm3H, gas phase fraction: 1; the temperature of a third raw material gas outlet 53 of the precooler 2 is 30-35 ℃, and the pressure is as follows: 1.3 to 1.5 mPAG;
step nine: the compressed nitrogen in the fourth end of the four-way joint in the seventh step enters the main heat exchanger 3 through the nitrogen expansion machine 15 to provide cold energy for the four-way joint, and enters the nitrogen compressor 14 through the raw material outlet 49 of the main heat exchanger 3 and the third end of the first tee joint 37 to be circularly compressed; the expander outlet line temperature was: -183 to-185 ℃, pressure: 0.02 to 0.03 mPAG;
step ten: raw material nitrogen in the nitrogen raw material storage tank 45 is supplemented with raw material gas into the liquid nitrogen preparation system through an air inlet pipeline; the specification of the raw material nitrogen is as follows: 0.4MPaG/25 ℃, 3500Nm3/h。
The utility model relates to a device which uses industrial low-pressure oxygen as raw material, adopts working medium refrigeration to cool the raw material oxygen and nitrogen for the first time, and realizes the liquefaction of the oxygen and nitrogen after the heat exchange of the cold energy of an expander; liquefied oxygen is used for an ultra-pure oxygen device, and an ultra-pure oxygen product is obtained after the coupling rectification of an upper tower and a lower tower. Wherein the quality of the ultra-pure liquid oxygen product is more than or equal to 99.9999% according to the quality index of pure oxygen, ultra-pure oxygen and ultra-pure oxygen 2008 GB/T14599-: 1. the R23 working medium is adopted for refrigeration, the oxygen and nitrogen raw materials are cooled for the first time, and the liquefaction of the oxygen and nitrogen is realized after the cold energy of the expansion machine is subjected to heat exchange, so that the energy consumption is saved; 2. the ultra-pure oxygen device adopts the upper and lower tower coupling rectification technology to obtain the ultra-pure oxygen product, the device occupies small area, the investment is saved, and the recovery period is short; 3. the R23 working medium refrigeration and nitrogen circulating system are both heat pump rectification technologies, no waste gas is discharged, the environment protection of atmosphere is facilitated, the system stability is facilitated, and the product purity is guaranteed; 4. the utility model has high energy integration, in particular to a lower tower top gas which provides a heat source for an upper tower reboiler, reduces the load of a nitrogen compressor and reduces the energy consumption of the device; 5. the utility model discloses still included the design of precooling system, it can reduce nitrogen compressor's circulation volume by a wide margin, and then reduces the energy consumption of unit product, and is favorable to the balance of system load, convenient operation.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected," "connecting," and the like are to be construed broadly, and may be, for example, fixedly connected, integrally connected, or detachably connected; or communication between the interior of the two elements; they may be directly connected or indirectly connected through an intermediate, and those skilled in the art can understand the specific meaning of the above terms in the present invention according to the specific situation. The above examples are only specific illustrations of feasible embodiments of the present invention, and they are not intended to limit the scope of the present invention, and all equivalent embodiments, modifications and alterations without departing from the technical spirit of the present invention are intended to be included in the scope of the present invention.

Claims (9)

1. The utility model provides an adopt apparatus for producing of precooling system production hyperpure oxygen and liquid nitrogen which characterized in that: the production device comprises an ultra-pure oxygen production system,
the ultra-pure oxygen production system comprises an oxygen raw material storage tank (1), wherein the oxygen raw material storage tank (1) is connected with an ultra-pure oxygen storage tank (9) through a raw material heat exchange unit and a thermal coupling rectifying tower;
the liquid nitrogen preparation system and the cold energy supply system respectively provide cold energy for the raw material heat exchange unit;
the liquid nitrogen preparation system respectively provides cold energy for the thermal coupling rectifying tower and a top condenser (6) at the top of the thermal coupling rectifying tower.
2. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 1, wherein: the thermally coupled rectifying tower comprises a lower tower rectifying tower (4) and an upper tower rectifying tower (5) arranged at the top of the lower tower rectifying tower (4);
the export of raw materials heat transfer unit links to each other with the first raw materials liquid import of lower column rectifying column (27) in lower column rectifying column (4), and the gas phase export at the top of lower column rectifying column (4) passes through second tee bend (47) and links to each other with last tower reboiler (8) and last tower rectifying column feed gas import (34) of last tower rectifying column (5) respectively, and last tower rectifying column liquid phase export (31) of last tower rectifying column (5) bottom links to each other with super pure oxygen storage tank (9).
3. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 2, wherein: and a fifth regulating valve (18) is arranged between the second tee joint (47) and the upper tower reboiler (8), and a sixth regulating valve (19) is arranged between the second tee joint (47) and the upper tower rectifying tower raw material gas inlet (34) of the upper tower rectifying tower (5).
4. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 2, wherein: a liquid phase outlet at the bottom of the lower rectifying tower (4) is connected with a liquid oxygen normal pressure storage tank (16) through a ninth regulating valve (26);
an outlet of the upper tower reboiler (8) is connected with a second raw material liquid inlet (32) of the lower tower rectifying tower at the upper part of the lower tower rectifying tower (4);
a gas phase outlet at the top of the upper rectifying tower (5) is connected with an upper rectifying tower raw material liquid inlet (29) of the upper rectifying tower (5) through a tube pass of a top condenser (6) and a tenth regulating valve (20);
a seventh regulating valve (21) is arranged between a liquid phase outlet at the bottom of the upper rectifying tower (5) and the ultrapure oxygen storage tank (9), and an outlet of the ultrapure oxygen storage tank (9) is connected with a charging row (11) through a charging pump (10);
a third tee joint (50) is arranged between the tube pass of the top condenser (6) and the tenth regulating valve (20), a fourth tee joint (51) is arranged between the outlet of the upper tower reboiler (8) and the second raw material liquid inlet (32) of the lower tower rectifying tower, and a near pipeline (52) is arranged between the third end of the third tee joint (50) and the third end of the fourth tee joint (51).
5. The apparatus for producing ultra-pure oxygen and liquid nitrogen using a pre-cooling system according to claim 1 or 2, wherein: the raw material heat exchange unit comprises a precooler (2) and a main heat exchanger (3), wherein the oxygen raw material storage tank (1) is connected with a first raw material liquid inlet (27) of the lower tower rectifying tower through a first raw material gas inlet (28) of the precooler (2), a first raw material gas outlet (42) of the precooler, a first raw material gas inlet (43) of the main heat exchanger (3), a first raw material gas outlet (44) of the main heat exchanger and an eighth regulating valve (46).
6. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 1, wherein: the liquid nitrogen preparation system comprises a nitrogen compressor (14), wherein an outlet of the nitrogen compressor (14) is sequentially connected with a second raw material gas inlet (40) of a precooler of the precooler (2), a second raw material gas outlet (30) of the precooler, a second raw material gas inlet (41) of a main heat exchanger of the main heat exchanger (3), a second raw material gas outlet (33) of the main heat exchanger, a second regulating valve (25) and a liquid nitrogen normal-pressure storage tank (17) through a four-way valve (38).
7. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 6, wherein: the third end of the four-way joint (38) is connected with the inlet of the nitrogen compressor (14) through a first regulating valve (22), a lower tower reboiler (7), a fourth regulating valve (23), the shell pass of the top condenser (6), a precooler third raw material gas inlet (36) of the precooler (2), a precooler third raw material gas outlet (53) and a first three-way joint (37) in sequence, and an air inlet pipeline with a nitrogen raw material storage tank (45) is arranged between the first three-way joint (37) and the inlet of the nitrogen compressor (14).
8. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 6, wherein: and the fourth end of the four-way joint (38) is connected with the third end of the first three-way joint (37) sequentially through the nitrogen expansion compressor (15), the main heat exchanger raw material inlet (39) of the main heat exchanger (3) and the main heat exchanger raw material outlet (49).
9. The apparatus for producing ultrapure oxygen and liquid nitrogen with the use of a pre-cooling system according to claim 1, wherein: the cold energy supply system comprises an R23 refrigerant tank (13), wherein the outlet of the R23 refrigerant tank (13) is connected with the inlet of the R23 refrigerant tank (13) through a third regulating valve (24), a precooler raw material inlet (35) of the precooler (2), a precooler raw material outlet (48) and an R23 compressor (12).
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113606866A (en) * 2021-08-06 2021-11-05 苏州市兴鲁空分设备科技发展有限公司 Device and method for preparing nitrogen by air separation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113606866A (en) * 2021-08-06 2021-11-05 苏州市兴鲁空分设备科技发展有限公司 Device and method for preparing nitrogen by air separation

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