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CN113390231B - A production device and production process for producing ultrapure oxygen and liquid nitrogen using a precooling system - Google Patents

A production device and production process for producing ultrapure oxygen and liquid nitrogen using a precooling system Download PDF

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Publication number
CN113390231B
CN113390231B CN202110806862.3A CN202110806862A CN113390231B CN 113390231 B CN113390231 B CN 113390231B CN 202110806862 A CN202110806862 A CN 202110806862A CN 113390231 B CN113390231 B CN 113390231B
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China
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raw material
tower
outlet
precooler
inlet
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CN202110806862.3A
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CN113390231A (en
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
    • 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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04278—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using external refrigeration units, e.g. closed mechanical or regenerative refrigeration units
    • 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
    • F25J3/04309—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 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
    • F25J3/04406—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
    • F25J3/04412—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 in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • 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
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • 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
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/40—Air or oxygen enriched air, i.e. generally less than 30mol% of 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/04—Recovery of liquid products
    • 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
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/14—External refrigeration with work-producing gas expansion loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

本发明属于一种采用预冷系统生产超纯氧和液氮的生产装置以及生产工艺；包括超纯氧生产系统、液氮制备系统，所述超纯氧生产系统包括氧气原料储罐，氧气原料储罐通过原料换热单元和热耦合精馏塔与超纯氧储罐相连；液氮制备系统以及冷量供给系统分别为原料换热单元提供冷量；液氮制备系统分别为热耦合精馏塔以及热耦合精馏塔顶的顶部冷凝器提供冷量；具有结构简单、流程设计合理、采用上下塔和循环制冷工艺、装置占地面积小，投资少，产品稳定、在得到超纯氧产品的同时能够副产液氮的优点。

The present invention relates to a production device and a production process for producing ultrapure oxygen and liquid nitrogen by using a precooling system; the device comprises an ultrapure oxygen production system and a liquid nitrogen preparation system, wherein the ultrapure oxygen production system comprises an oxygen raw material storage tank, and the oxygen raw material storage tank is connected to the ultrapure oxygen storage tank through a raw material heat exchange unit and a thermally coupled distillation tower; the liquid nitrogen preparation system and the cold supply system respectively provide cold for the raw material heat exchange unit; the liquid nitrogen preparation system respectively provides cold for the thermally coupled distillation tower and the top condenser at the top of the thermally coupled distillation tower; the device has the advantages of simple structure, reasonable process design, upper and lower towers and a circulating refrigeration process, small device footprint, low investment, stable products, and the ability to produce liquid nitrogen as a by-product while obtaining ultrapure oxygen products.

Description

Production device and production process for producing ultrapure oxygen and liquid nitrogen by adopting precooling system
Technical Field
The invention belongs to the technical field of coupling production of ultrapure-grade liquid oxygen and liquefied nitrogen, and particularly relates to a production device and a production process for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system.
Background
The ultra-pure oxygen has great application prospect in the fields of semiconductor elements, integrated circuits, photovoltaic industry and the like, but has great difficulty in preparing the ultra-pure oxygen industrially, and as is well known, air is an inexhaustible source spring for producing the industrial oxygen, 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 fused salt catalytic absorption method, can be adopted for preparing the oxygen by air separation. Because air mainly consists of nitrogen, oxygen, argon, carbon dioxide, methane, oxygen and the like, the industrial oxygen prepared by an air separation method has complex composition, and particularly contains impurities such as argon, nitrogen and the like which are difficult to remove by a normal temperature separation method, the difficulty of preparing ultra-pure oxygen by using the industrial oxygen as a raw material is very high. Based on the above, the low temperature rectification method is mainly adopted in industry to produce ultrapure oxygen, but oxygen is required to be liquefied and in a low temperature state in the process of producing ultrapure oxygen so as to achieve the aim of rectification and purification, a large amount of cold energy is required to be consumed in an intangible way, the cold energy is wasted, and the defects of oxygen emptying and the like are also caused.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides the production device and the production process which have the advantages of simple structure, reasonable flow design, small occupied area of the device by adopting an upper tower, a lower tower and a circulating refrigeration process, less investment, stable product and capability of producing ultrapure oxygen and liquid nitrogen by adopting a precooling system while obtaining the ultrapure oxygen product.
The purpose of the invention is realized in the following way:
A production device for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system comprises an ultrapure 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 thermally coupled 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 provides cold energy for the top condenser at the top of the thermal coupling rectifying tower respectively.
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 outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet of a lower tower rectifying tower in the lower tower rectifying tower, a gas phase outlet at the top of the lower tower rectifying tower is respectively connected with an upper tower reboiler and a first raw material gas inlet of an upper tower rectifying tower of the upper tower rectifying tower through a second tee joint, and a liquid phase outlet of the upper tower rectifying tower at the bottom of the upper tower rectifying tower is connected with an ultrapure 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 upper tower rectifying tower raw material gas inlet of the upper tower rectifying tower.
Preferably, a liquid phase outlet at the bottom of the lower tower rectifying tower is connected with a liquid oxygen normal pressure storage tank through a ninth regulating valve;
The outlet of the upper tower reboiler is connected with the inlet of the second raw material liquid of the lower tower rectifying tower at the upper part of the lower tower rectifying tower;
The gas phase outlet at the top of the upper tower rectifying tower is connected with the upper tower rectifying tower raw material liquid inlet of the upper tower rectifying tower through the tube pass of the top condenser and a tenth regulating valve;
a seventh regulating valve is arranged between the liquid phase outlet at the bottom of the upper tower rectifying tower and the ultrapure oxygen storage tank, and the 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 second raw material liquid inlet of the lower tower rectifying tower, and a close-up 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 a precooler first raw material gas inlet of the precooler, a precooler first raw material gas outlet, a main heat exchanger first raw material gas inlet of the main heat exchanger, a main heat exchanger first raw material gas outlet and an 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 precooler second raw material gas inlet, a precooler second raw material gas outlet, a main heat exchanger second raw material gas inlet of a main heat exchanger, a main heat exchanger second raw material gas outlet, a second regulating valve and a liquid nitrogen normal pressure storage tank through four-way.
Preferably, the third end of the four-way valve is connected with the inlet of the nitrogen compressor through a first regulating valve, a lower tower reboiler, a fourth regulating valve, a shell pass of a top condenser, a precooler third raw material gas inlet of the precooler, a precooler third raw material gas outlet and a first tee, and an air inlet pipeline with a nitrogen raw material storage tank is arranged between the first tee and the inlet of the nitrogen compressor.
Preferably, the fourth end of the four-way valve is connected with the third end of the first three-way valve through the nitrogen expansion compressor, the main heat exchanger raw material inlet and the main heat exchanger raw material outlet of the main heat exchanger in sequence.
Preferably, the cold energy supply system comprises an R23 refrigerant tank, and an outlet of the R23 refrigerant tank is connected with an 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.
A production process of a production device for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system, which comprises the following steps:
the method comprises the steps that raw material oxygen in an oxygen raw material storage tank is precooled by a precooler, enters a main heat exchanger for continuous cooling, enters a lower tower rectifying tower from a first raw material liquid inlet in the lower tower rectifying tower, wherein the temperature of the raw material oxygen is 20-30 ℃, the pressure is 0.5Mpa, the flow is 5000Nm/h, the gas phase fraction is 1, and the oxygen mole fraction is 99.5-99.6%;
Step two, the raw material liquid entering the lower tower rectifying tower in the step one is subjected to primary rectifying purification, and gas phases after rectifying purification enter an upper tower reboiler and an upper tower rectifying tower respectively through a second tee joint, wherein the gas phase outlet temperature of the top of the lower tower rectifying tower 4 is-175 to-177 ℃, and the oxygen mole fraction is 99.9-99.95%;
step three, performing secondary rectification after the gas phase enters an upper tower rectifying tower, and enabling a liquid phase after the secondary rectification to enter an ultrapure oxygen storage tank through a liquid phase outlet of the upper tower rectifying tower and then enter a filling row through a filling pump, wherein the temperature of the liquid phase after the secondary rectification purification is-181-183 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999%;
Step four, the liquid phase after primary rectification in the step two in the lower tower rectifying tower enters a liquid oxygen normal pressure storage tank through a liquid phase outlet at the bottom of the lower tower rectifying tower and a ninth regulating valve to recycle industrial oxygen;
The gas phase after the secondary rectification in the step three is subjected to heat exchange liquefaction through a tube pass of a top condenser and then enters a third tee joint, one part of the gas phase enters an upper column rectifying tower through a tenth regulating valve and an upper column rectifying tower raw material liquid inlet to be refluxed, the temperature of the upper column rectifying tower raw material liquid inlet is-181.5 to-183.5 ℃, the other part of the gas phase enters a fourth tee joint through a short-circuit pipeline, the material passing through an upper column reboiler in the step two enters the fourth tee joint, and the gas phase and the material are converged in the fourth tee joint and then reflux into a lower column rectifying tower through a lower column rectifying tower second raw material liquid inlet;
Step six, throttling the refrigerant R23 in the R23 refrigerant tank through a third regulating valve, re-heating through a precooler raw material inlet and a precooler raw material outlet of the precooler after throttling, and entering the R23 refrigerant tank through an R23 compressor and an inlet of the R23 refrigerant tank after re-heating, wherein the temperature at the inlet of the R23 compressor is-48 to-50 ℃, and the mole fraction of the R23 is 100%;
The compressed nitrogen in the outlet of the nitrogen compressor sequentially enters a liquid nitrogen normal-pressure storage tank through a four-way joint with a precooler second raw material gas inlet of the precooler, a precooler second raw material gas outlet, a main heat exchanger second raw material gas inlet of a main heat exchanger, a main heat exchanger second raw material gas outlet and a second regulating valve, wherein the temperature of the main heat exchanger second raw material gas outlet is-182 to-184 ℃, and the pressure is 0.01-0.03mPaG;
The third end of the four-way pipe is filled with compressed nitrogen into a reboiler of a lower tower through a first regulating valve to exchange heat with the interior of a rectifying tower of the lower tower, the heat exchange is performed again with gas phase from the rectifying tower of the upper tower through a fourth regulating valve, the heat exchange is performed again, the heat exchange is performed sequentially, and the heat exchange is performed again, and the heat exchange is performed sequentially through a shell pass of the top condenser, a precooler third raw material gas inlet of the precooler, a precooler third raw material gas outlet and a first tee joint, and the heat exchange is filled into a nitrogen compressor to form circulation, wherein the temperature of the precooler third raw material gas inlet of the precooler is-184 to-187 ℃, the flow is 4000-4200 Nm 3/h, the gas phase fraction is 1, the temperature of the precooler third raw material gas outlet of the precooler is 30-35 ℃, and the pressure is 1.3-1.5 mPAG;
Step nine, enabling compressed nitrogen in the fourth end of the four-way valve to enter a main heat exchanger through a nitrogen expander to provide cold energy for the main heat exchanger, and enabling the compressed nitrogen to enter a nitrogen compressor through a main heat exchanger raw material outlet of the main heat exchanger and a third end of a first tee joint to circularly compress the nitrogen, wherein the temperature of an outlet pipeline of the expander is minus 183 to minus 185 ℃, and the pressure is 0.02-0.03 mPaG;
and step ten, supplementing raw material gas into a liquid nitrogen preparation system through an air inlet pipeline by using raw material nitrogen in a nitrogen raw material storage tank, wherein the specification of the raw material nitrogen is 0.4MPaG/25 ℃,3500Nm 3/h.
According to the production device and the production process for producing the ultrapure oxygen and the liquid nitrogen by adopting the precooling system, the raw material of the ultrapure oxygen is provided by adopting the industrial-grade low-pressure oxygen, and the working principles of R23 working medium refrigeration and expander refrigeration are utilized, and the ultrapure oxygen purification process with the product purity of not less than 99.9999% and the device for producing the liquid nitrogen are stably produced by utilizing the coupling rectification of the upper tower and the lower tower. The invention has the advantages that 1, the raw materials of oxygen and nitrogen are cooled for the first time by adopting R23 working medium refrigeration, after heat exchange is carried out by the cold energy of an expander, the liquefaction of the oxygen and the nitrogen is realized, the energy consumption is saved, and the environment is protected, 2, an ultrapure oxygen device adopts an upper tower and lower tower coupling rectification technology, an ultrapure oxygen product is obtained, is stored by an ultrapure oxygen storage tank and then is used for filling a bottle for gas through a liquid pump, the sales requirements of an outsourcing liquid ultrapure oxygen product and a gas ultrapure oxygen product can be simultaneously realized, the purity of the product can reach more than 99.9999%, the dependence of the semiconductor industry on imported ultrapure oxygen is solved, the full raw materials are provided for the research of the semiconductor industry and the electronic special gas industry, the economic and social benefits are promoted, 4, the energy is highly integrated, specifically, the lower tower top gas is a heat source provided for the upper tower, the load of a nitrogen compressor is reduced, the energy consumption of the device is reduced, 5, the design of a precooling system is also included, the liquid nitrogen compressor can be greatly reduced, the sales requirements of the liquid ultrapure oxygen product and the gas can be met, the sales requirements of the tank car and the bottle for the gas can be simultaneously realized, the maximum consumption of the semiconductor device can be realized, the invention, the maximum consumption of the high-grade semiconductor device can be used for the production and the refrigeration device can be used for the production of the refrigeration device, the full-cycle has the advantages of the invention, the full consumption and the full consumption of the refrigeration device and the production technology can be realized, and the full consumption can reach the use, and the advantages of the production and the high quality, and the advantages of the production and the can realize and the full use, and the economy and can realize and the economy.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Fig. 2 is a schematic structural diagram of the thermally coupled rectifying column of the present invention.
In the upper graph:
1. An oxygen raw material storage tank; 2, precooler; 3, a main heat exchanger; 4, a lower column rectifying tower, an upper column rectifying tower, 6, a top condenser, 7, a lower column reboiler, 8, an upper column reboiler, 9, an ultrapure oxygen storage tank, 10, a filling pump, 11, a filling discharge, 12, an R23 compressor, 13, an 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 lower column rectifying tower first raw material liquid inlet, 28, a precooler first raw material gas inlet, 29, an upper column rectifying tower raw material liquid inlet, 30, a precooler second raw material gas outlet, 31, an upper column liquid outlet, 32, a lower column rectifying tower second raw material liquid inlet, 33, a main heat exchanger second raw material outlet, 34, a main heat exchanger, a third regulating valve, a third heat exchanger, a fourth heat exchanger, a third heat exchanger, a raw material inlet, a third heat exchanger, a main heat exchanger, a third heat exchanger, a raw material liquid, a material inlet, a raw material inlet, a third, a material, a third, a material, a third, a material, a material, a raw, a raw, a, raw, a, raw, raw, raw column raw column raw.
Detailed Description
For a clearer understanding of the technical features, objects and effects of the present invention, embodiments of the present invention will now be described with reference to the drawings, in which like reference numerals refer to like parts throughout the various views. For simplicity of the drawing, only the parts relevant to the invention are schematically shown in each drawing, and they do not represent the actual structure thereof as a product.
As shown in figures 1 and 2, the invention discloses a production device and a production process for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system, wherein the production device comprises an ultrapure oxygen production system, the ultrapure oxygen production system comprises an oxygen raw material storage tank 1, the oxygen raw material storage tank 1 is connected with an ultrapure oxygen storage tank 9 through a raw material heat exchange unit and a thermally coupled rectifying tower, a liquid nitrogen preparation system and a cold energy supply system respectively provide cold energy for the raw material heat exchange unit, and the liquid nitrogen preparation system respectively provides cold energy for the thermally coupled rectifying tower and a top condenser 6 at the top of the thermally coupled rectifying tower.
Further, the thermally coupled rectifying tower comprises a lower rectifying tower 4 and an upper rectifying tower 5 arranged at the top of the lower rectifying tower 4, wherein an outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet 27 of the lower rectifying tower in the lower rectifying tower 4, a gas phase outlet at the top of the lower rectifying tower 4 is respectively connected with an upper reboiler 8 and a first raw material gas inlet 34 of the upper rectifying tower 5 through a second tee joint 47, and a 31 at the bottom of the upper rectifying tower 5 is connected with an ultrapure oxygen storage tank 9.
Further, 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 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 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 rectifying tower at the upper part of the lower rectifying tower 4, a gas phase outlet at the top of the upper rectifying tower 5 is connected with a 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 the liquid phase outlet at the bottom of the upper rectifying tower 5 and the ultrapure oxygen storage tank 9, an outlet of the ultrapure oxygen storage tank 9 is connected with a filling row 11 through a filling 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 rectifying tower, and a near pipeline 52 is arranged between a third end of the third tee joint 50 and a third end of the fourth tee joint 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 lower tower rectifying tower first raw material liquid inlet 27 through a precooler first raw material gas inlet 28, a precooler first raw material gas outlet 42, a main heat exchanger first raw material gas inlet 43, a main heat exchanger first raw material gas outlet 44 and an eighth regulating valve 46 of the precooler 2.
Further, the liquid nitrogen preparation system comprises a nitrogen compressor 14, wherein an outlet of the nitrogen compressor 14 is sequentially connected with a precooler second raw material gas inlet 40, a precooler second raw material gas outlet 30, a main heat exchanger second raw material gas inlet 41 of the main heat exchanger 3, a main heat exchanger second raw material gas outlet 33, a second regulating valve 25 and a liquid nitrogen normal pressure storage tank 17 of the precooler 2 through a four-way valve 38.
Further, a third end of the four-way valve 38 is connected with an inlet of the nitrogen compressor 14 through a first regulating valve 22, a lower tower reboiler 7, a fourth regulating valve 23, a shell side of the top condenser 6, a precooler third raw material gas inlet 36 of the precooler 2, a precooler third raw material gas outlet 42 and a first tee 37 in sequence, and an air inlet pipeline with a nitrogen raw material storage tank 45 is arranged between the first tee 37 and the inlet of the nitrogen compressor 14.
Further, the fourth end of the four-way valve 38 is connected to the third end of the first tee 37 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 in sequence.
Further, the cold energy supply system includes 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 ultrapure oxygen and liquid nitrogen by adopting a precooling system, which comprises the following steps:
The method comprises the steps that firstly, raw material oxygen in an oxygen raw material storage tank 1 is precooled by a precooler 2, enters a main heat exchanger 3 for continuous cooling, enters a lower tower rectifying tower 4 from a first raw material liquid inlet 27 in the lower tower rectifying tower 4, wherein the temperature of the raw material oxygen is 20-30 ℃, the pressure is 0.5Mpa, the flow is 5000Nm/h, the gas phase fraction is 1, and the oxygen mole fraction is 99.5-99.6%;
Step two, carrying out primary rectification purification on the raw material liquid entering the lower tower rectifying tower 4 in the step one, and respectively entering gas phases after rectification purification into an upper tower reboiler 8 and an upper tower rectifying tower 5 through a second tee joint 47, wherein the gas phase outlet temperature of the top of the lower tower rectifying tower 4 is-175 to-177 ℃, and the oxygen mole fraction is 99.9-99.95%;
Step three, the gas phase in the step two enters an upper tower rectifying tower 5 and is subjected to secondary rectification, 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 filling row 11 through a filling pump 10, wherein the temperature of the liquid phase after the secondary rectification purification is-181 to-183 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999%;
step four, the liquid phase after primary rectification in the step two by the lower tower rectifying tower 4 enters a liquid oxygen normal pressure storage tank 16 through a liquid phase outlet at the bottom of the lower tower rectifying tower 4 and a ninth regulating valve 26 for industrial oxygen recovery;
The gas phase after secondary rectification in the step three is subjected to heat exchange liquefaction through a tube pass of a top condenser 6 and then enters a third tee joint 50, one part of the gas phase enters an upper tower rectifying tower 5 through a tenth regulating valve 20 and an upper tower rectifying tower raw material liquid inlet 29 to be refluxed, the temperature at the position of the upper tower rectifying tower raw material liquid inlet 29 is-181.5 to-183.5 ℃, the other part of the gas phase enters a fourth tee joint 51 through a close-up pipeline 52, the material passing through an upper tower reboiler 8 in the step two enters the fourth tee joint 51, and the gas phase and the material are converged in the fourth tee joint 51 and then reflux into a lower tower rectifying tower 4 through a lower tower rectifying tower second raw material liquid inlet 32;
Step six, throttling the refrigerant R23 in the R23 refrigerant tank 13 through a third regulating valve 24, reheating through a precooler raw material inlet 35 and a precooler raw material outlet 48 of the precooler 2 after throttling, and entering the R23 refrigerant tank 13 through an inlet of the R23 compressor 12 and an inlet of the R23 refrigerant tank 13 after reheating, wherein the temperature at the inlet of the R23 compressor 12 is-48 to-50 ℃ and the mole fraction of the R23 is 100%;
The compressed nitrogen in the outlet of the nitrogen compressor 14 sequentially enters a liquid nitrogen normal pressure storage tank 17 through a four-way valve 38, and the temperature of the outlet 33 of the second raw material gas of the main heat exchanger is-182 to-184 ℃ and the pressure of the outlet 33 of the second raw material gas of the main heat exchanger is 0.01-0.03mPaG, wherein the inlet 40 of the second raw material gas of the precooler 2, the outlet 30 of the second raw material gas of the precooler, the inlet 41 of the second raw material gas of the main heat exchanger 3, the outlet 33 of the second raw material gas of the main heat exchanger and the second regulating valve 25 are all arranged in the liquid nitrogen normal pressure storage tank 17;
The compressed nitrogen in the third end of the four-way valve enters a lower tower reboiler 7 through a first regulating valve 22 to exchange heat with the interior of a lower tower rectifying tower 4, the heat exchange is performed again through a fourth regulating valve 23, the heat exchange is performed on the heat exchange gas in the top condenser 6, the heat exchange is performed again, the heat exchange gas sequentially enters a nitrogen compressor 14 through a shell pass of the top condenser 6, a precooler third raw material gas inlet 36 of a precooler 2, a precooler third raw material gas outlet 42 and a first tee joint 37 to form circulation, the temperature of the precooler third raw material gas inlet 36 of the precooler 2 is-184 to-187 ℃, the flow is 4000-4200 Nm 3/h, the gas phase fraction is 1, the temperature of the precooler third raw material gas outlet 42 of the precooler 2 is 30-35 ℃, and the pressure is 1.3-1.5 PaG;
Step nine, the compressed nitrogen in the fourth end of the four-way valve in step seven enters the main heat exchanger 3 through the nitrogen expander 15 to provide cold energy for the main heat exchanger, and enters the nitrogen compressor 14 through the main heat exchanger raw material outlet 49 of the main heat exchanger 3 and the third end of the first tee 37 to circularly compress, wherein the temperature of an outlet pipeline of the expander is minus 183 to minus 185 ℃, and the pressure is 0.02 to 0.03mPaG;
step ten, raw material nitrogen in a nitrogen raw material storage tank 45 is supplemented into a liquid nitrogen preparation system through an air inlet pipeline, wherein the specification of the raw material nitrogen is 0.4MPaG/25 ℃,3500Nm 3/h.
The invention relates to an ultra-pure oxygen device which uses industrial low-pressure oxygen as a raw material, adopts working medium refrigeration to cool the raw material oxygen and nitrogen for the first time, realizes the liquefaction of the oxygen and the nitrogen after heat exchange by the cold energy of an expander, and obtains an ultra-pure oxygen product after the liquefied oxygen is used in the ultra-pure oxygen device and is subjected to coupling rectification by an upper tower and a lower tower. The method has the advantages that 1, raw material oxygen and nitrogen are cooled for the first time by adopting R23 working medium refrigeration, liquefaction of the oxygen and the nitrogen is realized after heat exchange of cold energy of an expander, energy consumption is saved, 2, an ultrapure oxygen device adopts an upper tower and lower tower coupling rectification technology to obtain an ultrapure oxygen product, the occupied area of the device is small, investment is saved, the recovery period is short, 3, R23 working medium refrigeration and nitrogen circulation systems are heat pump rectification technology, no waste gas is discharged, the method is beneficial to atmosphere environmental protection, the system stability is beneficial, the product purity is guaranteed, 4, the method has high integration, specifically, lower tower top gas provides a heat source for an upper tower reboiler, the load of a nitrogen compressor is reduced, and the energy consumption of the device is reduced.
The technical solutions of the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Example 1
The production device for producing the ultrapure oxygen and the liquid nitrogen by adopting the pre-cooling system comprises an ultrapure oxygen production system, wherein the ultrapure oxygen production system comprises an oxygen raw material storage tank 1, the oxygen raw material storage tank 1 is connected with an ultrapure oxygen storage tank 9 through a raw material heat exchange unit and a thermal coupling rectifying tower, a liquid nitrogen preparation system and a cold energy supply system respectively provide cold energy for the raw material heat exchange unit, and 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. The thermally coupled rectifying tower comprises a lower rectifying tower 4 and an upper rectifying tower 5 arranged at the top of the lower rectifying tower 4, wherein an outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet 27 of the lower rectifying tower in the lower rectifying tower 4, a gas phase outlet at the top of the lower rectifying tower 4 is respectively connected with an upper reboiler 8 and a first raw material gas inlet 34 of the upper rectifying tower 5 through a second tee joint 47, and an upper rectifying tower liquid phase outlet 31 at the bottom of the upper rectifying tower 5 is connected with an ultrapure oxygen storage tank 9. 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. The liquid phase outlet at the bottom of the lower tower rectifying tower 4 is connected with a liquid oxygen normal pressure storage tank 16 through a ninth regulating valve 26, the outlet of the upper tower reboiler 8 is connected with a lower tower rectifying tower second raw material liquid inlet 32 at the upper part of the lower tower rectifying tower 4, the gas phase outlet at the top of the upper tower rectifying tower 5 is connected with an upper tower rectifying tower raw material liquid inlet 29 of the upper tower 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 the liquid phase outlet at the bottom of the upper tower rectifying tower 5 and an ultrapure oxygen storage tank 9, the outlet of the ultrapure oxygen storage tank 9 is connected with a filling row 11 through a filling 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 lower tower second raw material liquid inlet 32, and a close pipeline 52 is arranged between the third end of the third tee joint 50 and the third end of the fourth tee joint 51. 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 a lower tower rectifying tower first raw material liquid inlet 27 through a precooler first raw material gas inlet 28, a precooler first raw material gas outlet 42, a main heat exchanger first raw material gas inlet 43, a main heat exchanger first raw material gas outlet 44 and an eighth regulating valve 46 of the main heat exchanger 3 of the precooler 2. The liquid nitrogen preparation system comprises a nitrogen compressor 14, wherein an outlet of the nitrogen compressor 14 is sequentially connected with a precooler second raw material gas inlet 40, a precooler second raw material gas outlet 30, a main heat exchanger second raw material gas inlet 41 of a main heat exchanger 3, a main heat exchanger second raw material gas outlet 33, a second regulating valve 25 and a liquid nitrogen normal pressure storage tank 17 of the precooler 2 through a four-way valve 38. the third end of the four-way valve 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, a 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 42 and a first tee 37 in sequence, and an air inlet pipeline with a nitrogen raw material storage tank 45 is arranged between the first tee 37 and the inlet of the nitrogen compressor 14. The fourth end of the four-way valve 38 is connected with the third end of the first three-way valve 37 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 in sequence. 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.
A production process of a production device for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system, which comprises the following steps:
The method comprises the steps that firstly, raw material oxygen in an oxygen raw material storage tank 1 is precooled by a precooler 2, enters a main heat exchanger 3 for continuous cooling, enters a lower tower rectifying tower 4 from a first raw material liquid inlet 27 in the lower tower rectifying tower 4, wherein the temperature of the raw material oxygen is 20 ℃, the pressure is 0.5Mpa, the flow is 5000Nm/h, the gas phase fraction is 1, and the oxygen mole fraction is 99.5%;
step two, the raw material liquid entering the lower tower rectifying tower 4 in the step one is subjected to primary rectifying purification, and gas phases after rectifying purification enter an upper tower reboiler 8 and an upper tower rectifying tower 5 respectively through a second tee joint 47, wherein the gas phase outlet temperature of the top of the lower tower rectifying tower 4 is-175 ℃, and the oxygen mole fraction is 99.9%;
Step three, the gas phase in the step two enters an upper tower rectifying tower 5 and is subjected to secondary rectification, 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 filling row 11 through a filling pump 10, and the liquid phase temperature after the secondary rectification purification is-183 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999%;
step four, the liquid phase after primary rectification in the step two by the lower tower rectifying tower 4 enters a liquid oxygen normal pressure storage tank 16 through a liquid phase outlet at the bottom of the lower tower rectifying tower 4 and a ninth regulating valve 26 for industrial oxygen recovery;
the gas phase after secondary rectification in the step three is subjected to heat exchange liquefaction through a tube pass of a top condenser 6 and then enters a third tee joint 50, one part of the gas phase enters an upper tower rectifying tower 5 through a tenth regulating valve 20 and an upper tower rectifying tower raw material liquid inlet 29 for backflow, the temperature at the position of the upper tower rectifying tower raw material liquid inlet 29 is-183.5 ℃, the other part of the gas phase enters a fourth tee joint 51 through a short-circuit pipeline 52, the material passing through an upper tower reboiler 8 in the step two enters the fourth tee joint 51, and the gas phase and the material are converged in the fourth tee joint 51 and then flow back into a lower tower rectifying tower 4 through a lower tower rectifying tower second raw material liquid inlet 32;
Step six, throttling the refrigerant R23 in the R23 refrigerant tank 13 through a third regulating valve 24, reheating through a precooler raw material inlet 35 and a precooler raw material outlet 48 of the precooler 2 after throttling, and entering the R23 refrigerant tank 13 through an inlet of the R23 compressor 12 and an inlet of the R23 refrigerant tank 13 after reheating, wherein the temperature at the inlet of the R23 compressor 12 is-50 ℃, and the mole fraction of R23 is 100%;
The compressed nitrogen in the outlet of the nitrogen compressor 14 sequentially enters a liquid nitrogen normal pressure storage tank 17 through a four-way valve 38, and the temperature of the primary heat exchanger second raw material gas outlet 33 is minus 184 ℃, and the pressure is 0.01mPaG;
The compressed nitrogen in the third end of the four-way valve in the step seven enters a lower tower reboiler 7 through a first regulating valve 22 to exchange heat with the interior of a lower tower rectifying tower 4, the heat exchange is throttled through a fourth regulating valve 23 and then supplied to a top condenser 6 to exchange heat with gas phase from an upper tower rectifying tower 5 in the top condenser 6 again, and the heat exchange is sequentially carried out through a shell pass of the top condenser 6, a precooler third raw material gas inlet 36 of a precooler 2, a precooler third raw material gas outlet 42 and a first tee joint 37 to enter a nitrogen compressor 14 to form circulation, wherein the temperature of the precooler third raw material gas inlet 36 of the precooler 2 is-187 ℃, the flow rate is 4000Nm 3/h, the gas phase fraction is 1, the temperature of the precooler third raw material gas outlet 42 of the precooler 2 is 30 ℃, and the pressure is 1.3mPaG;
Step nine, the compressed nitrogen in the fourth end of the four-way valve in step seven enters the main heat exchanger 3 through the nitrogen expander 15 to provide cold energy for the main heat exchanger, and enters the nitrogen compressor 14 through the main heat exchanger raw material outlet 49 of the main heat exchanger 3 and the third end of the first tee 37 to circularly compress, wherein the temperature of an expander outlet pipeline is 185 ℃ below zero, and the pressure is 0.02mPaG;
step ten, raw material nitrogen in a nitrogen raw material storage tank 45 is supplemented into a liquid nitrogen preparation system through an air inlet pipeline, wherein the specification of the raw material nitrogen is 0.4MPaG/25 ℃,3500Nm 3/h.
Example 2
The production device for producing the ultrapure oxygen and the liquid nitrogen by adopting the pre-cooling system comprises an ultrapure oxygen production system, wherein the ultrapure oxygen production system comprises an oxygen raw material storage tank 1, the oxygen raw material storage tank 1 is connected with an ultrapure oxygen storage tank 9 through a raw material heat exchange unit and a thermal coupling rectifying tower, a liquid nitrogen preparation system and a cold energy supply system respectively provide cold energy for the raw material heat exchange unit, and 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. The thermally coupled rectifying tower comprises a lower rectifying tower 4 and an upper rectifying tower 5 arranged at the top of the lower rectifying tower 4, wherein an outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet 27 of the lower rectifying tower in the lower rectifying tower 4, a gas phase outlet at the top of the lower rectifying tower 4 is respectively connected with an upper reboiler 8 and a first raw material gas inlet 34 of the upper rectifying tower 5 through a second tee joint 47, and an upper rectifying tower liquid phase outlet 31 at the bottom of the upper rectifying tower 5 is connected with an ultrapure oxygen storage tank 9. 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. The liquid phase outlet at the bottom of the lower tower rectifying tower 4 is connected with a liquid oxygen normal pressure storage tank 16 through a ninth regulating valve 26, the outlet of the upper tower reboiler 8 is connected with a lower tower rectifying tower second raw material liquid inlet 32 at the upper part of the lower tower rectifying tower 4, the gas phase outlet at the top of the upper tower rectifying tower 5 is connected with an upper tower rectifying tower raw material liquid inlet 29 of the upper tower 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 the liquid phase outlet at the bottom of the upper tower rectifying tower 5 and an ultrapure oxygen storage tank 9, the outlet of the ultrapure oxygen storage tank 9 is connected with a filling row 11 through a filling 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 lower tower second raw material liquid inlet 32, and a close pipeline 52 is arranged between the third end of the third tee joint 50 and the third end of the fourth tee joint 51. 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 a lower tower rectifying tower first raw material liquid inlet 27 through a precooler first raw material gas inlet 28, a precooler first raw material gas outlet 42, a main heat exchanger first raw material gas inlet 43, a main heat exchanger first raw material gas outlet 44 and an eighth regulating valve 46 of the main heat exchanger 3 of the precooler 2. The liquid nitrogen preparation system comprises a nitrogen compressor 14, wherein an outlet of the nitrogen compressor 14 is sequentially connected with a precooler second raw material gas inlet 40, a precooler second raw material gas outlet 30, a main heat exchanger second raw material gas inlet 41 of a main heat exchanger 3, a main heat exchanger second raw material gas outlet 33, a second regulating valve 25 and a liquid nitrogen normal pressure storage tank 17 of the precooler 2 through a four-way valve 38. the third end of the four-way valve 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, a 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 42 and a first tee 37 in sequence, and an air inlet pipeline with a nitrogen raw material storage tank 45 is arranged between the first tee 37 and the inlet of the nitrogen compressor 14. The fourth end of the four-way valve 38 is connected with the third end of the first three-way valve 37 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 in sequence. 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.
A production process of a production device for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system, which comprises the following steps:
The method comprises the steps that firstly, raw material oxygen in an oxygen raw material storage tank 1 is precooled by a precooler 2, enters a main heat exchanger 3 for continuous cooling, enters a lower tower rectifying tower 4 from a first raw material liquid inlet 27 in the lower tower rectifying tower 4, wherein the temperature of the raw material oxygen is 30 ℃, the pressure is 0.5Mpa, the flow is 5000Nm/h, the gas phase fraction is 1, and the oxygen mole fraction is 99.6%;
step two, the raw material liquid entering the lower tower rectifying tower 4 in the step one is subjected to primary rectifying purification, and gas phases after rectifying purification enter an upper tower reboiler 8 and an upper tower rectifying tower 5 respectively through a second tee joint 47, wherein the gas phase outlet temperature of the top of the lower tower rectifying tower 4 is 177 ℃ below zero, and the oxygen mole fraction is 99.95%;
Step three, the gas phase in the step two enters an upper tower rectifying tower 5 and is subjected to secondary rectification, 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 filling row 11 through a filling pump 10, and the liquid phase temperature after the secondary rectification purification is-181 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999%;
step four, the liquid phase after primary rectification in the step two by the lower tower rectifying tower 4 enters a liquid oxygen normal pressure storage tank 16 through a liquid phase outlet at the bottom of the lower tower rectifying tower 4 and a ninth regulating valve 26 for industrial oxygen recovery;
The gas phase after secondary rectification in the step three is subjected to heat exchange liquefaction through a tube pass of a top condenser 6 and then enters a third tee joint 50, one part of the gas phase enters an upper tower rectifying tower 5 through a tenth regulating valve 20 and an upper tower rectifying tower raw material liquid inlet 29 for backflow, the temperature at the position of the upper tower rectifying tower raw material liquid inlet 29 is-181.5 ℃, the other part of the gas phase enters a fourth tee joint 51 through a short-circuit pipeline 52, the material passing through an upper tower reboiler 8 in the step two enters the fourth tee joint 51, and the gas phase and the material are converged in the fourth tee joint 51 and then flow back into a lower tower rectifying tower 4 through a lower tower rectifying tower second raw material liquid inlet 32;
Step six, throttling the refrigerant R23 in the R23 refrigerant tank 13 through a third regulating valve 24, reheating through a precooler raw material inlet 35 and a precooler raw material outlet 48 of the precooler 2 after throttling, and entering the R23 refrigerant tank 13 through an inlet of the R23 compressor 12 and an inlet of the R23 refrigerant tank 13 after reheating, wherein the temperature at the inlet of the R23 compressor 12 is-48 ℃, and the mole fraction of R23 is 100%;
the compressed nitrogen in the outlet of the nitrogen compressor 14 sequentially enters a liquid nitrogen normal pressure storage tank 17 through a four-way valve 38, and the temperature of the primary heat exchanger second raw material gas outlet 33 is-182 ℃ and the pressure is 0.03mPaG;
The compressed nitrogen in the third end of the four-way valve enters a lower tower reboiler 7 through a first regulating valve 22 to exchange heat with the interior of a lower tower rectifying tower 4, the heat exchange is performed again through a fourth regulating valve 23, the heat exchange is performed on the heat exchange gas in the top condenser 6, the heat exchange is performed again, the heat exchange gas sequentially enters a nitrogen compressor 14 through a 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 42 and a first tee joint 37 to form circulation, the temperature of the precooler third raw material gas inlet 36 of the precooler 2 is-184 to-187 ℃, the flow rate is 4200Nm 3/h, the gas phase fraction is 1, the temperature of the precooler third raw material gas outlet 42 of the precooler 2 is 35 ℃, and the pressure is 1.5mPaG;
Step nine, the compressed nitrogen in the fourth end of the four-way valve in step seven enters the main heat exchanger 3 through the nitrogen expander 15 to provide cold energy for the main heat exchanger, and enters the nitrogen compressor 14 through the main heat exchanger raw material outlet 49 of the main heat exchanger 3 and the third end of the first tee 37 to circularly compress, wherein the temperature of an outlet pipeline of the expander is minus 183 ℃, and the pressure is 0.03mPaG;
step ten, raw material nitrogen in a nitrogen raw material storage tank 45 is supplemented into a liquid nitrogen preparation system through an air inlet pipeline, wherein the specification of the raw material nitrogen is 0.4MPaG/25 ℃,3500Nm 3/h.
Example 3
The production device for producing the ultrapure oxygen and the liquid nitrogen by adopting the pre-cooling system comprises an ultrapure oxygen production system, wherein the ultrapure oxygen production system comprises an oxygen raw material storage tank 1, the oxygen raw material storage tank 1 is connected with an ultrapure oxygen storage tank 9 through a raw material heat exchange unit and a thermal coupling rectifying tower, a liquid nitrogen preparation system and a cold energy supply system respectively provide cold energy for the raw material heat exchange unit, and 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. The thermally coupled rectifying tower comprises a lower rectifying tower 4 and an upper rectifying tower 5 arranged at the top of the lower rectifying tower 4, wherein an outlet of the raw material heat exchange unit is connected with a first raw material liquid inlet 27 of the lower rectifying tower in the lower rectifying tower 4, a gas phase outlet at the top of the lower rectifying tower 4 is respectively connected with an upper reboiler 8 and a first raw material gas inlet 34 of the upper rectifying tower 5 through a second tee joint 47, and an upper rectifying tower liquid phase outlet 31 at the bottom of the upper rectifying tower 5 is connected with an ultrapure oxygen storage tank 9. 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. The liquid phase outlet at the bottom of the lower tower rectifying tower 4 is connected with a liquid oxygen normal pressure storage tank 16 through a ninth regulating valve 26, the outlet of the upper tower reboiler 8 is connected with a lower tower rectifying tower second raw material liquid inlet 32 at the upper part of the lower tower rectifying tower 4, the gas phase outlet at the top of the upper tower rectifying tower 5 is connected with an upper tower rectifying tower raw material liquid inlet 29 of the upper tower 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 the liquid phase outlet at the bottom of the upper tower rectifying tower 5 and an ultrapure oxygen storage tank 9, the outlet of the ultrapure oxygen storage tank 9 is connected with a filling row 11 through a filling 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 lower tower second raw material liquid inlet 32, and a close pipeline 52 is arranged between the third end of the third tee joint 50 and the third end of the fourth tee joint 51. 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 a lower tower rectifying tower first raw material liquid inlet 27 through a precooler first raw material gas inlet 28, a precooler first raw material gas outlet 42, a main heat exchanger first raw material gas inlet 43, a main heat exchanger first raw material gas outlet 44 and an eighth regulating valve 46 of the main heat exchanger 3 of the precooler 2. The liquid nitrogen preparation system comprises a nitrogen compressor 14, wherein an outlet of the nitrogen compressor 14 is sequentially connected with a precooler second raw material gas inlet 40, a precooler second raw material gas outlet 30, a main heat exchanger second raw material gas inlet 41 of a main heat exchanger 3, a main heat exchanger second raw material gas outlet 33, a second regulating valve 25 and a liquid nitrogen normal pressure storage tank 17 of the precooler 2 through a four-way valve 38. the third end of the four-way valve 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, a 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 42 and a first tee 37 in sequence, and an air inlet pipeline with a nitrogen raw material storage tank 45 is arranged between the first tee 37 and the inlet of the nitrogen compressor 14. The fourth end of the four-way valve 38 is connected with the third end of the first three-way valve 37 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 in sequence. 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.
A production process of a production device for producing ultrapure oxygen and liquid nitrogen by adopting a precooling system, which comprises the following steps:
The method comprises the steps that firstly, raw material oxygen in an oxygen raw material storage tank 1 is precooled by a precooler 2, enters a main heat exchanger 3 for continuous cooling, enters a lower tower rectifying tower 4 from a first raw material liquid inlet 27 in the lower tower rectifying tower 4, wherein the temperature of the raw material oxygen is 25 ℃, the pressure is 0.5Mpa, the flow is 5000Nm/h, the gas phase fraction is 1, and the oxygen mole fraction is 99.55%;
Step two, the raw material liquid entering the lower tower rectifying tower 4 in the step one is subjected to primary rectifying purification, and gas phases after rectifying purification enter an upper tower reboiler 8 and an upper tower rectifying tower 5 respectively through a second tee joint 47, wherein the gas phase outlet temperature of the top of the lower tower rectifying tower 4 is minus 176 ℃, and the oxygen mole fraction is 99.93%;
step three, the gas phase in the step two enters an upper tower rectifying tower 5 and is subjected to secondary rectification, 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 filling row 11 through a filling pump 10, and the liquid phase temperature after the secondary rectification purification is-182 ℃, and the molar purity of the ultrapure oxygen is not lower than 99.9999%;
step four, the liquid phase after primary rectification in the step two by the lower tower rectifying tower 4 enters a liquid oxygen normal pressure storage tank 16 through a liquid phase outlet at the bottom of the lower tower rectifying tower 4 and a ninth regulating valve 26 for industrial oxygen recovery;
The gas phase after secondary rectification in the step three is subjected to heat exchange liquefaction through a tube pass of a top condenser 6 and then enters a third tee joint 50, one part of the gas phase enters an upper tower rectifying tower 5 through a tenth regulating valve 20 and an upper tower rectifying tower raw material liquid inlet 29 for backflow, the temperature at the position of the upper tower rectifying tower raw material liquid inlet 29 is-182.5 ℃, the other part of the gas phase enters a fourth tee joint 51 through a short-circuit pipeline 52, the material passing through an upper tower reboiler 8 in the step two enters the fourth tee joint 51, and the gas phase and the material are converged in the fourth tee joint 51 and then flow back into a lower tower rectifying tower 4 through a lower tower rectifying tower second raw material liquid inlet 32;
Step six, throttling the refrigerant R23 in the R23 refrigerant tank 13 through a third regulating valve 24, reheating through a precooler raw material inlet 35 and a precooler raw material outlet 48 of the precooler 2 after throttling, and entering the R23 refrigerant tank 13 through an inlet of the R23 compressor 12 and an inlet of the R23 refrigerant tank 13 after reheating, wherein the temperature at the inlet of the R23 compressor 12 is-49 ℃, and the mole fraction of R23 is 100%;
The compressed nitrogen in the outlet of the nitrogen compressor 14 sequentially enters a liquid nitrogen normal pressure storage tank 17 through a four-way valve 38, and the temperature of the primary heat exchanger second raw material gas outlet 33 is minus 183 ℃ and the pressure is 0.02mPaG;
The compressed nitrogen in the third end of the four-way valve in the step seven enters a lower tower reboiler 7 through a first regulating valve 22 to exchange heat with the interior of a lower tower rectifying tower 4, the heat exchange is throttled through a fourth regulating valve 23 and then supplied to a top condenser 6 to exchange heat with gas phase from an upper tower rectifying tower 5 in the top condenser 6 again, the heat exchange is carried out again and then enters a nitrogen compressor 14 through a shell side of the top condenser 6, a precooler third raw material gas inlet 36 of a precooler 2, a precooler third raw material gas outlet 42 and a first tee joint 37 in sequence to form circulation, wherein the temperature of the precooler third raw material gas inlet 36 of the precooler 2 is 185.5 ℃, the flow rate is 4100Nm 3/h, the gas phase fraction is 1, the temperature of the precooler third raw material gas outlet 42 of the precooler 2 is 32.5 ℃, and the pressure is 1.4mPaG;
Step nine, the compressed nitrogen in the fourth end of the four-way valve in step seven enters the main heat exchanger 3 through the nitrogen expander 15 to provide cold energy for the main heat exchanger, and enters the nitrogen compressor 14 through the main heat exchanger raw material outlet 49 of the main heat exchanger 3 and the third end of the first tee 37 to circularly compress, wherein the temperature of an outlet pipeline of the expander is-184 ℃, and the pressure is 0.025mPaG;
step ten, raw material nitrogen in a nitrogen raw material storage tank 45 is supplemented into a liquid nitrogen preparation system through an air inlet pipeline, wherein the specification of the raw material nitrogen is 0.4MPaG/25 ℃,3500Nm 3/h.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "connected," "connected," and the like are to be construed broadly, and may be, for example, fixedly connected, integrally connected, detachably connected, or communicating between two elements, directly connected, or indirectly connected through an intermediate medium, and the specific meaning of the terms in the present invention may be understood by those skilled in the art according to the specific circumstances. The above examples are only specific to practical embodiments of the present invention, and they are not intended to limit the scope of the present invention, but all equivalent embodiments, modifications and adaptations without departing from the technical spirit of the present invention are intended to be included in the scope of the present invention.

Claims (2)

1.一种采用预冷系统生产超纯氧和液氮的生产装置，其特征在于：该生产装置包括超纯氧生产系统，1. A production device for producing ultrapure oxygen and liquid nitrogen using a precooling system, characterized in that: the production device comprises an ultrapure oxygen production system, 所述超纯氧生产系统包括氧气原料储罐（1），氧气原料储罐（1）通过原料换热单元和热耦合精馏塔与超纯氧储罐（9）相连；The ultrapure oxygen production system comprises an oxygen raw material storage tank (1), wherein the oxygen raw material storage tank (1) is connected to an ultrapure oxygen storage tank (9) via a raw material heat exchange unit and a thermally coupled distillation tower; 液氮制备系统以及冷量供给系统分别为原料换热单元提供冷量；The liquid nitrogen preparation system and the cold supply system provide cold capacity for the raw material heat exchange unit respectively; 液氮制备系统分别为热耦合精馏塔以及热耦合精馏塔顶的顶部冷凝器（6）提供冷量；The liquid nitrogen preparation system provides cooling capacity for the thermally coupled distillation tower and the top condenser (6) at the top of the thermally coupled distillation tower; 热耦合精馏塔包括下塔精馏塔（4）以及设置在下塔精馏塔（4）顶部的上塔精馏塔（5）；The thermally coupled distillation tower comprises a lower distillation tower (4) and an upper distillation tower (5) arranged on the top of the lower distillation tower (4); 原料换热单元的出口与下塔精馏塔（4）中的下塔精馏塔第一原料液进口（27）相连，下塔精馏塔（4）塔顶的气相出口通过第二三通（47）分别与上塔再沸器（8）和上塔精馏塔（5）的上塔精馏塔原料气进口（34）相连，上塔精馏塔（5）底部的上塔精馏塔液相出口（31）与超纯氧储罐（9）相连；The outlet of the raw material heat exchange unit is connected to the first raw material liquid inlet (27) of the lower distillation tower in the lower distillation tower (4); the gas phase outlet at the top of the lower distillation tower (4) is connected to the upper tower reboiler (8) and the upper tower distillation tower raw material gas inlet (34) of the upper distillation tower (5) through the second tee (47); the upper tower distillation tower liquid phase outlet (31) at the bottom of the upper distillation tower (5) is connected to the ultrapure oxygen storage tank (9); 所述第二三通（47）和上塔再沸器（8）之间设有第五调节阀（18），第二三通（47）和上塔精馏塔（5）的上塔精馏塔原料气进口（34）之间设有第六调节阀（19）；A fifth regulating valve (18) is provided between the second three-way valve (47) and the upper tower reboiler (8), and a sixth regulating valve (19) is provided between the second three-way valve (47) and the upper tower distillation tower feed gas inlet (34) of the upper tower distillation tower (5); 下塔精馏塔（4）底部的液相出口通过第九调节阀（26）与液氧常压储槽（16）相连；The liquid phase outlet at the bottom of the lower distillation tower (4) is connected to the liquid oxygen atmospheric pressure storage tank (16) via a ninth regulating valve (26); 上塔再沸器（8）出口与下塔精馏塔（4）上部的下塔精馏塔第二原料液进口（32）相连；The outlet of the upper tower reboiler (8) is connected to the second raw liquid inlet (32) of the lower tower distillation tower at the upper part of the lower tower distillation tower (4); 上塔精馏塔（5）顶部的气相出口通过顶部冷凝器（6）的管程以及第十调节阀（20）与上塔精馏塔（5）的上塔精馏塔原料液进口（29）相连；The gas phase outlet at the top of the upper distillation tower (5) is connected to the upper distillation tower raw liquid inlet (29) of the upper distillation tower (5) through the pipe path of the top condenser (6) and the tenth regulating valve (20); 上塔精馏塔（5）底部的液相出口和超纯氧储罐（9）之间设有第七调节阀（21），超纯氧储罐（9）的出口通过充装泵（10）与充装排（11）相连；A seventh regulating valve (21) is provided between the liquid phase outlet at the bottom of the upper distillation tower (5) and the ultrapure oxygen storage tank (9), and the outlet of the ultrapure oxygen storage tank (9) is connected to the filling row (11) via a filling pump (10); 顶部冷凝器（6）的管程和第十调节阀（20）之间设有第三三通（50），上塔再沸器（8）出口和下塔精馏塔第二原料液进口（32）之间设有第四三通（51），第三三通（50）的第三端和第四三通（51）的第三端之间设有近路管道（52）；A third three-way valve (50) is provided between the pipe side of the top condenser (6) and the tenth regulating valve (20), a fourth three-way valve (51) is provided between the outlet of the upper tower reboiler (8) and the inlet (32) of the second raw liquid of the lower tower rectification tower, and a shortcut pipeline (52) is provided between the third end of the third three-way valve (50) and the third end of the fourth three-way valve (51); 原料换热单元包括预冷器（2）以及主换热器（3），氧气原料储罐（1）通过预冷器（2）的预冷器第一原料气进口（28）、预冷器第一原料气出口、主换热器（3）的主换热器第一原料气进口（43）、主换热器第一原料气出口（44）和第八调节阀（46）与下塔精馏塔第一原料液进口（27）相连；The raw material heat exchange unit comprises a precooler (2) and a main heat exchanger (3); the oxygen raw material storage tank (1) is connected to the first raw material liquid inlet (27) of the lower distillation tower via a first raw material gas inlet (28) of the precooler (2), a first raw material gas outlet 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); 液氮制备系统包括氮气压缩机（14），氮气压缩机（14）的出口通过四通（38）依次与预冷器（2）的预冷器第二原料气进口（40）、预冷器第二原料气出口（30）、主换热器（3）的主换热器第二原料气进口（41）、主换热器第二原料气出口（33）及第二调节阀（25）和液氮常压储槽（17）相连；The liquid nitrogen preparation system comprises a nitrogen compressor (14), wherein the outlet of the nitrogen compressor (14) is connected in sequence to a precooler second raw gas inlet (40) of a precooler (2), a precooler second raw gas outlet (30), a main heat exchanger second raw gas inlet (41) of a main heat exchanger (3), a main heat exchanger second raw gas outlet (33), a second regulating valve (25), and a liquid nitrogen atmospheric pressure storage tank (17) through a four-way valve (38); 所述四通（38）的第三端依次通过第一调节阀（22）、下塔再沸器（7）、第四调节阀（23）、顶部冷凝器（6）的壳程、预冷器（2）的预冷器第三原料气进口（36）、预冷器第三原料气出口和第一三通（37）与氮气压缩机（14）的进口相连，第一三通（37）与氮气压缩机（14）的进口之间设有带氮气原料储罐（45）的进气管道；The third end of the four-way valve (38) is connected to the inlet of the nitrogen compressor (14) through the first regulating valve (22), the lower tower reboiler (7), the fourth regulating valve (23), the shell side of the top condenser (6), the third raw gas inlet (36) of the precooler (2), the third raw gas outlet of the precooler and the first three-way valve (37) in sequence, and an air intake pipeline with a nitrogen raw material storage tank (45) is provided between the first three-way valve (37) and the inlet of the nitrogen compressor (14); 所述四通（38）的第四端依次通过氮气膨胀机（15）、主换热器（3）的主换热器原料进口（39）和主换热器原料出口（49）与第一三通（37）的第三端相连；The fourth end of the four-way (38) is connected to the third end of the first three-way (37) via the nitrogen expander (15), the main heat exchanger raw material inlet (39) and the main heat exchanger raw material outlet (49) of the main heat exchanger (3); 所述冷量供给系统包括R23冷剂罐（13），R23冷剂罐（13）的出口通过第三调节阀（24）、预冷器（2）的预冷器原料进口（35）、预冷器原料出口（48）和R23压缩机（12）与R23冷剂罐（13）的进口相连。The cold supply system comprises an R23 refrigerant tank (13), wherein the outlet of the R23 refrigerant tank (13) is connected to the inlet of the R23 refrigerant tank (13) via 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). 2.一种利用权利要求1所述的采用预冷系统生产超纯氧和液氮的生产装置的生产工艺，其特征在于：该生产工艺包括如下步骤：2. A production process for producing ultrapure oxygen and liquid nitrogen using the precooling system of claim 1, characterized in that the production process comprises the following steps: 步骤一：氧气原料储罐（1）中的原料氧气经预冷器（2）预冷后，进入主换热器（3）继续降温，并由下塔精馏塔（4）中的第一原料液进口（27）进入到下塔精馏塔（4）内；所述原料氧气的温度为：20～30℃，压力为：0.5Mpa，流量为：5000Nm/h，气相分率为：1，氧气摩尔分数：99.5～99.6%；Step 1: The raw oxygen in the oxygen raw material storage tank (1) is precooled by the precooler (2), enters the main heat exchanger (3) to continue cooling, and enters the lower tower distillation tower (4) through the first raw liquid inlet (27) in the lower tower distillation tower (4); the raw oxygen has a temperature of 20 to 30°C, a pressure of 0.5 MPa, a flow rate of 5000 Nm/h, a gas phase fraction of 1, and an oxygen molar fraction of 99.5 to 99.6%; 步骤二：使步骤一中进入下塔精馏塔（4）的原料液进行一次精馏提纯，精馏提纯后的气相通过第二三通（47）分别进入上塔再沸器（8）和上塔精馏塔（5）内；所述下塔精馏塔4塔顶气相出口温度：-175～-177℃，氧气摩尔分数为：99.9～99.95%；Step 2: subjecting the raw material liquid entering the lower distillation tower (4) in step 1 to a distillation purification, and the gas phase after distillation purification enters the upper tower reboiler (8) and the upper distillation tower (5) respectively through the second three-way (47); the gas phase outlet temperature at the top of the lower distillation tower 4 is: -175 to -177°C, and the oxygen molar fraction is: 99.9 to 99.95%; 步骤三：步骤二中气相进入上塔精馏塔（5）后进行二次精馏，二次精馏后的液相通过上塔精馏塔液相出口（31）进入超纯氧储罐（9），后经充装泵（10）进入到充装排（11）内；所述二次精馏提纯后的液相温度为：-181～-183℃，超纯氧摩尔纯度不低于99.9999%；Step 3: The gas phase in step 2 enters the upper distillation tower (5) and then undergoes secondary distillation. The liquid phase after the secondary distillation enters the ultrapure oxygen storage tank (9) through the liquid phase outlet (31) of the upper distillation tower, and then enters the filling row (11) through the filling pump (10); the liquid phase temperature after the secondary distillation is: -181 to -183°C, and the ultrapure oxygen molar purity is not less than 99.9999%; 步骤四：步骤二中经过下塔精馏塔（4）一次精馏后的液相通过下塔精馏塔（4）底部的液相出口和第九调节阀（26）进入液氧常压储槽（16）中，进行工业氧回收；Step 4: the liquid phase after the primary distillation in the lower distillation tower (4) in step 2 enters the liquid oxygen atmospheric pressure storage tank (16) through the liquid phase outlet at the bottom of the lower distillation tower (4) and the ninth regulating valve (26) for industrial oxygen recovery; 步骤五： 步骤三中二次精馏后的气相通过顶部冷凝器（6）的管程换热液化后进入第三三通（50）内，一部分由第十调节阀（20）和上塔精馏塔原料液进口（29）进入上塔精馏塔（5）中进行回流；所述上塔精馏塔原料液进口（29）处温度为-181.5～-183.5℃；另一部分由近路管道（52）进入第四三通（51）中；步骤二中通过上塔再沸器（8）的物料进入第四三通（51）；上述两者在第四三通（51）中汇合后通过下塔精馏塔第二原料液进口（32）回流至下塔精馏塔（4）内；Step 5: The gas phase after the secondary distillation in step 3 is liquefied through the heat exchange of the tube side of the top condenser (6) and enters the third tee (50), and a part of it enters the upper distillation tower (5) through the tenth regulating valve (20) and the raw liquid inlet (29) of the upper distillation tower for reflux; the temperature at the raw liquid inlet (29) of the upper distillation tower is -181.5 to -183.5°C; the other part enters the fourth tee (51) through the shortcut pipeline (52); the material passing through the upper tower reboiler (8) in step 2 enters the fourth tee (51); the above two are merged in the fourth tee (51) and refluxed to the lower distillation tower (4) through the second raw liquid inlet (32) of the lower distillation tower; 步骤六：R23冷剂罐（13）中的冷剂R23通过第三调节阀（24）进行节流，节流后通过预冷器（2）的预冷器原料进口（35）和预冷器原料出口（48）进行复热，复热后通过R23压缩机（12）和R23冷剂罐（13）的进口进入到R23冷剂罐（13）中；所述R23压缩机（12）进口处温度为：-48～-50℃，R23摩尔分数为：100%；Step 6: The refrigerant R23 in the R23 refrigerant tank (13) is throttled through the third regulating valve (24), and after throttling, it is reheated through the precooler raw material inlet (35) and the precooler raw material outlet (48) of the precooler (2), and after reheating, it 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°C, and the mole fraction of R23 is: 100%; 步骤七：氮气压缩机（14）出口中经过压缩的氮气通过四通（38）依次与预冷器（2）的预冷器第二原料气进口（40）、预冷器第二原料气出口（30）、主换热器（3）的主换热器第二原料气进口（41）、主换热器第二原料气出口（33）和第二调节阀（25）进入液氮常压储槽（17）内；所述主换热器第二原料气出口（33）的温度为：-182～-184℃，压力：0.01～0.03mPaG；Step 7: The compressed nitrogen at the outlet of the nitrogen compressor (14) enters the liquid nitrogen atmospheric pressure storage tank (17) through the four-way (38) and the precooler second raw gas inlet (40) of the precooler (2), the precooler second raw gas outlet (30), the main heat exchanger second raw gas inlet (41) of the main heat exchanger (3), the main heat exchanger second raw gas outlet (33) and the second regulating valve (25); the temperature of the main heat exchanger second raw gas outlet (33) is: -182 to -184°C, and the pressure is: 0.01 to 0.03 mPaG; 步骤八：步骤七中所述四通的第三端内经过压缩的氮气通过第一调节阀（22）进入下塔再沸器（7）中与下塔精馏塔（4）内进行换热，换热后通过第四调节阀（23）节流后至顶部冷凝器（6）提供冷量，在顶部冷凝器（6）内与来自上塔精馏塔（5）的气相进行再次换热，再次换热后依次通过顶部冷凝器（6）的壳程、预冷器（2）的预冷器第三原料气进口（36）、预冷器第三原料气出口和第一三通（37）进入氮气压缩机（14）中构成循环；所述预冷器（2）的预冷器第三原料气进口（36）的温度为：-184～-187℃，流量：4000～4200Nm3/h，气相分率：1；预冷器（2）的预冷器第三原料气出口温度为30～35℃，压力为：1.3～1.5mPaG；Step 8: The compressed nitrogen in the third end of the four-way in step 7 enters the lower tower reboiler (7) through the first regulating valve (22) to exchange heat with the lower tower distillation tower (4), and after heat exchange, passes through the fourth regulating valve (23) to throttle and then enters the top condenser (6) to provide cooling capacity, and in the top condenser (6) it exchanges heat again with the gas phase from the upper tower distillation tower (5), and after the heat exchange again, it passes through the shell side of the top condenser (6), the third raw gas inlet (36) of the precooler (2), the third raw gas outlet of the precooler and the first three-way (37) to enter the nitrogen compressor (14) to form a cycle; the temperature of the third raw gas inlet (36) of the precooler (2) is: -184～-187℃, and the flow rate is: 4000～ 4200Nm3 /h, gas phase fraction: 1; the outlet temperature of the third raw gas of the precooler (2) is 30-35°C, and the pressure is: 1.3-1.5mPaG; 步骤九：步骤七中所述四通的第四端内经过压缩的氮气通过氮气膨胀机（15）进入主换热器（3）为其提供冷量，并通过主换热器（3）的主换热器原料出口（49）和第一三通（37）的第三端进入到氮气压缩机（14）中循环压缩；膨胀机出口管线温度为：-183～-185℃，压力：0.02～0.03mPaG；Step 9: The compressed nitrogen in the fourth end of the four-way pipe in step 7 enters the main heat exchanger (3) through the nitrogen expander (15) to provide cooling capacity for the main heat exchanger (3), and enters the nitrogen compressor (14) through the main heat exchanger raw material outlet (49) of the main heat exchanger (3) and the third end of the first three-way pipe (37) for cyclic compression; the expander outlet pipeline temperature is: -183 to -185°C, and the pressure is: 0.02 to 0.03 mPaG; 步骤十：氮气原料储罐（45）中的原料氮气通过进气管道向液氮制备系统中补入原料气；所述原料氮气的规格为：0.4MPaG/25℃，3500Nm3/h。Step 10: The raw nitrogen in the nitrogen raw material storage tank (45) is added to the liquid nitrogen preparation system through the air inlet pipeline; the specification of the raw nitrogen is: 0.4MPaG/25°C, 3500Nm3 /h.
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