WO2021016779A1 - Système de préparation de co2 alimentaire - Google Patents

Système de préparation de co2 alimentaire Download PDF

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Publication number
WO2021016779A1
WO2021016779A1 PCT/CN2019/098066 CN2019098066W WO2021016779A1 WO 2021016779 A1 WO2021016779 A1 WO 2021016779A1 CN 2019098066 W CN2019098066 W CN 2019098066W WO 2021016779 A1 WO2021016779 A1 WO 2021016779A1
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WO
WIPO (PCT)
Prior art keywords
gas
rectification tower
tower
outlet
liquid
Prior art date
Application number
PCT/CN2019/098066
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English (en)
Chinese (zh)
Inventor
万和昌
万里鹏
万舒妤
Original Assignee
江西江氨科技有限公司
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Filing date
Publication date
Application filed by 江西江氨科技有限公司 filed Critical 江西江氨科技有限公司
Priority to PCT/CN2019/098066 priority Critical patent/WO2021016779A1/fr
Publication of WO2021016779A1 publication Critical patent/WO2021016779A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/50—Carbon dioxide
    • 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
    • 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
    • F25J2200/74—Refluxing the column with at least a part of the partially 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/78—Refluxing the column with a liquid stream originating from an upstream or downstream fractionator 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
    • 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
    • F25J2215/80—Carbon dioxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/80—Separating impurities from carbon dioxide, e.g. H2O or water-soluble contaminants
    • F25J2220/82—Separating low boiling, i.e. more volatile components, e.g. He, H2, CO, Air gases, CH4
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/80—Separating impurities from carbon dioxide, e.g. H2O or water-soluble contaminants
    • F25J2220/84—Separating high boiling, i.e. less volatile components, e.g. NOx, SOx, H2S
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/30—Compression of the feed stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration

Definitions

  • the invention relates to the technical field of food-grade carbon dioxide production, in particular to a food-grade CO 2 preparation system.
  • the production of traditional food-grade carbon dioxide generally adopts molecular sieve dehydration and de-alcoholization and catalytic combustion de-hydrocarbon devices and processes, which require a large amount of heat for heating the regeneration gas in implementation, high energy consumption and complex operation processes.
  • the raw gas contains impurity gas and moisture.
  • the temperature before entering the rectification tower should be maintained at about 10-15 degrees. If the temperature is too low, the carbon dioxide and moisture in the pipeline will easily produce hydrate and block the pipeline, but the temperature is too high It is not conducive to the subsequent rectification in the rectification tower. This production process will undoubtedly increase the burden and production cost of the enterprise.
  • the purpose of the present invention is to overcome the shortcomings of the prior art, adapt to actual needs, and disclose an easy-to-implement food-grade CO2 preparation system.
  • the present invention provides a food-grade CO 2 preparation system, which includes two rectification towers, the two rectification towers are respectively a first rectification tower and a second rectification tower;
  • the bottom of the first distillation tower is enriched with the first high boiler and the top is enriched with the first low boiler;
  • the bottom of the second distillation tower is enriched with the second high boiler, and the top is enriched with the second low boiler;
  • the first low boiler discharged from the top of the first rectifying tower enters the reboiler in the second rectifying tower to reboil the second reboiler entering the second rectifying tower to recover the first high boiler Carrying heat.
  • the bottom of the second rectification tower is provided with a liquid outlet, and the second high-boiler product in the second rectification tower is discharged through the bottom liquid outlet.
  • an antifreeze liquid is added to the raw gas pipeline before the raw gas enters the first rectification tower.
  • the pipe connected with the feed gas inlet of the first rectification tower is provided with an antifreeze inlet.
  • a compressor is provided on the pipeline connected with the feed gas inlet of the first rectification tower, and the feed gas is compressed by the compressor and enters the first rectification tower.
  • the antifreeze liquid inlet is arranged at the front or rear end of the compressor.
  • the feed gas enters the first rectification tower through the middle or lower part of the first rectification tower.
  • the reboiler in the first rectification tower is connected to an external heat source.
  • the bottom outlet of the first rectification tower is the residual liquid discharge outlet and is used for The first high boiler is discharged, and the top of the first distillation tower is provided with a first low boiler exhaust port;
  • the first low-boiler exhaust port at the top of the first rectification tower is in communication with the second reboiler inlet in the second rectification tower.
  • the outlet of the second reboiler is in communication with the inlet of the first gas-liquid separator, and the liquid-phase outlet of the first gas-liquid separator is in communication with the inlet on the top of the first distillation tower;
  • the bottom outlet of the second rectification tower is a finished product discharge outlet, and it also includes a second gas-liquid separator and a heat exchanger.
  • the gas-phase outlet of the first gas-liquid separator and the second low The boiling material exhaust ports are all connected with the inlet of the heat exchanger, the outlet of the heat exchanger is connected with the inlet of the second gas-liquid separator, the gas-phase outlet of the second gas-liquid separator is the exhaust gas outlet, and the second gas-liquid separator
  • the liquid phase outlet is connected with the inlet at the top of the second rectification tower.
  • the gas-phase discharge pipe of the first gas-liquid separator is provided with a pressure reducing valve.
  • the structure design of the present invention is novel, compared with the existing food-grade CO 2 preparation system, the design is more reasonable, the energy supply is simpler (only need to supply energy to the reboiler in the first distillation tower), and it is easier to realize. Energy consumption is low. Secondly, by adding antifreeze before rectification, it can avoid the occurrence of pipeline blockage caused by crystallization of the inner wall of the pipeline after the temperature of the raw gas is lowered, and improve the efficiency of gas production and the stability of the system during gas production.
  • Figure 1 is a schematic diagram of the principle of the food-grade CO 2 preparation system of the present invention.
  • Example 1 A food-grade CO 2 preparation system, see Figure 1.
  • the two rectification towers are the first rectification tower 9 and the second rectification tower 16.
  • the bottom of the first rectification tower is enriched with the first high boiler, and the top is enriched The first low boiler;
  • the bottom of the second distillation tower is enriched with the second high boiler, and the top is enriched with the second low boiler; among them, the middle of the first distillation tower 9 is provided with a feed gas inlet 8 which is
  • the pipe connected to the feed gas inlet 8 of the first rectification tower 9 is provided with an antifreeze liquid inlet 3, and at the same time, the pipe connected to the feed gas inlet 8 of the first rectification tower 9 is provided with a compressor 2.
  • the raw material gas passes through the buffer tank 1 and is compressed by the compressor 2 and then enters the first rectification tower 9.
  • the above-mentioned antifreeze liquid inlet 3 is arranged at the front or rear end of the compressor 2. In specific use, it is antifreeze The liquid inlet 3 can be added according to actual needs.
  • the reboiler 6 in the first rectification tower 9 is connected to an external heat source through a pipeline 5, and the bottom outlet 7 of the first rectification tower is a residual liquid discharge outlet and is used to discharge the first high boilers.
  • the top of the first distillation tower 9 is provided with a first low-boiler exhaust port 11.
  • the first low-boiler exhaust port 11 at the top of the first rectification tower 9 is connected to the inlet 15 of the second reboiler 14 in the second rectification tower 16 through a pipeline.
  • the outlet 13 of the second reboiler 14 in the second rectification tower 16 is in communication with the inlet 26 of the first gas-liquid separator, and the liquid phase outlet 27 of the first gas-liquid separator is connected to the inlet 10 at the top of the first rectification tower. Connected.
  • the bottom outlet of the second rectification tower 9 is the finished product discharge port 12, and also includes a second gas-liquid separator 20, a heat exchanger 19, and a gas-phase outlet 24 and a second gas-liquid separator 25 of the first gas-liquid separator 25
  • the second low-boiler exhaust port 18 at the top of the second rectification tower 16 is connected with the inlet of the heat exchanger 19, and the outlet of the heat exchanger 19 is connected with the inlet 21 of the second gas-liquid separator.
  • the gas phase outlet 23 is an exhaust gas outlet, and the liquid phase outlet 22 of the second gas-liquid separator is in communication with the inlet 17 at the top of the second rectification tower.
  • the present design also has a pressure reducing valve 28 on the gas discharge pipe of the first gas-liquid separator 24.
  • the working principle of the food-grade CO2 preparation system of the present invention is as follows:
  • the raw material gas is compressed by compressor 2 after passing through the buffer tank. After compression, the CO 2 content in the raw material gas is 70%-99.99%, and the pressure is 1.4-4.0Mpa. At this time, add antifreeze to prevent gas through the antifreeze inlet 3 In the subsequent pipeline, the pipeline is blocked by condensation of hydrate in the gas due to low temperature; at this time, the reboiler 6 in the first rectification tower is heated by an external heat source, and the temperature of the heat source entering the reboiler 6 is 5-40 °C.
  • the temperature of the feed gas is reduced after passing through the heat exchanger before entering the first rectification tower (by reducing the temperature before rectification, the rectification efficiency inside the rectification tower can be improved, and the high boiling point substances in the rectification tower can be improved.
  • the separation rate of low-boiling substances is to separate the impurity gas from carbon dioxide as much as possible, which is of great significance for improving the purity of carbon dioxide. After the raw material gas enters the first rectification tower, it is reboiled by the reboiler 6.
  • the temperature of the heat source discharged from the outlet of the device is -9°C; after the feed gas enters the first rectification tower, the first high boilers are mostly impurities and are discharged through the bottom outlet 7 of the first rectification tower.
  • the discharged residual night contains medium CO 2
  • the content is 80%-95%, the pressure is 1.4-4.0Mpa Mpa, and the temperature is -11°C; the first low boiler of the first rectification tower has a higher concentration of CO 2 which can be extracted.
  • the first low After the boiling matter passes through the tray rectification inside the first distillation tower, the first low boiler gas is discharged through the first low boiler exhaust port 11 at the top. At this time, the first low boiler gas is discharged from the first distillation tower.
  • the low boiler gas has a CO 2 content of 70%-98%, a pressure of 1.4-4.0Mpa Mpa, and a temperature of -15°C—-17°C.
  • the first low-boiler gas discharged from the first rectification tower enters the reboiler in the second rectification tower to reboil the second reboiler entering the second rectification tower.
  • the reboiler in the second rectification tower does not need to be supplied with external energy, and the energy of the second reboiler 14 comes from the first low boiler gas discharged from a rectification tower.
  • the first low boiler gas discharged from the first rectification tower passes through the second reboiler and then enters the first gas-liquid separator 25 for gas-liquid separation. Before entering the first gas-liquid separator, its CO 2 content is 70% -98%, air pressure is 1.4-4.0Mpa Mpa, temperature is -17°C—-19°C.
  • the liquid substance After being separated by the first gas-liquid separator, the liquid substance enters the first rectification tower through the middle or lower part of the first rectification tower 9 for rectification again; the gas-phase substance goes up to the second gas-liquid separator Inside.
  • the second reboiler reboils the second reboiler in the second distillation tower (the second reboiler in the second distillation tower is the liquid phase separated by the second gas-liquid separator Substance), the second high boiler after reboiling in the second rectification tower is the finished product, that is, food grade carbon dioxide and is discharged through the liquid outlet at the bottom of the second rectification tower.
  • the discharged finished product has a CO 2 content of 99.997%.
  • the air pressure is 2.2-2.3Mpa and the temperature is -19°C.
  • the second low boiler (its CO 2 content is 70%-80%, the pressure is 2.2-2.3Mpa, and the temperature is -18°C—-20°C) after being re-boiled by the second rectifying tower and the first gas-liquid
  • the gas phase separated by the separator will pass through the heat exchanger together with the latter and then enter the second gas-liquid separator for gas-liquid separation.
  • the gas phase is the residual gas and is discharged from the entire system.
  • the CO 2 content is 40%-60%
  • the air pressure is 2.2-2.3Mpa
  • the temperature is -25°C—- 40°C
  • the liquid phase material enters the second rectification tower again to form a second reboiler and is reboiled and rectified again.
  • the CO 2 content in the liquid phase material is about 85%.
  • the second high boiler after reboiled in the second rectification tower is the finished product, that is, food-grade carbon dioxide and is discharged through the liquid outlet at the bottom of the second rectification tower.
  • the discharged finished product has a CO 2 content of 99.997% and the pressure is 2.2-2.3Mpa, the temperature is -19°C.
  • the first rectification tower and the first gas-liquid separator in this design can constitute a second-cycle rectification purification process.
  • the heat exchanger, the second gas-liquid separator and the second rectification tower can constitute a three-cycle rectification purification process, and the preparation of high-purity food-grade carbon dioxide can be achieved through the three-cycle process mentioned above.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne un système de préparation de CO2 alimentaire facile à mettre en œuvre, le système comprenant deux tours de rectification. Les deux tours de rectification sont respectivement une première tour de rectification et une seconde tour de rectification ; un premier produit à basse ébullition, évacué à partir de la partie supérieure de la première tour de rectification, entre dans un rebouilleur dans la seconde tour de rectification afin de faire rebouillir un second produit de rebouilleur entrant dans la seconde tour de rectification ; une sortie de liquide est formée au niveau de la partie inférieure de la seconde tour de rectification, et un second produit fini à haute ébullition, dans la seconde tour de rectification, est évacué par l'intermédiaire de la sortie de liquide au niveau de la partie inférieure.
PCT/CN2019/098066 2019-07-27 2019-07-27 Système de préparation de co2 alimentaire WO2021016779A1 (fr)

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PCT/CN2019/098066 WO2021016779A1 (fr) 2019-07-27 2019-07-27 Système de préparation de co2 alimentaire

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PCT/CN2019/098066 WO2021016779A1 (fr) 2019-07-27 2019-07-27 Système de préparation de co2 alimentaire

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114963691A (zh) * 2022-05-31 2022-08-30 山东石油化工学院 低压co2气体低温分离方法及装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101691320A (zh) * 2009-10-14 2010-04-07 清华大学 从填埋气中提纯回收甲烷和二氧化碳的方法及其装置
CN104654739A (zh) * 2015-02-02 2015-05-27 河南心连心深冷能源股份有限公司 利用双塔精馏提纯制取食品级液体二氧化碳的装置和方法
CN104748506A (zh) * 2015-03-13 2015-07-01 河南心连心深冷能源股份有限公司 油田助采尾气回收co2的装置及其工艺

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101691320A (zh) * 2009-10-14 2010-04-07 清华大学 从填埋气中提纯回收甲烷和二氧化碳的方法及其装置
CN104654739A (zh) * 2015-02-02 2015-05-27 河南心连心深冷能源股份有限公司 利用双塔精馏提纯制取食品级液体二氧化碳的装置和方法
CN104748506A (zh) * 2015-03-13 2015-07-01 河南心连心深冷能源股份有限公司 油田助采尾气回收co2的装置及其工艺

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114963691A (zh) * 2022-05-31 2022-08-30 山东石油化工学院 低压co2气体低温分离方法及装置
CN114963691B (zh) * 2022-05-31 2023-12-26 山东石油化工学院 低压co2气体低温分离方法及装置

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