WO2021016779A1 - Food-grade co2 preparation system - Google Patents

Food-grade co2 preparation system 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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Prior art keywords
gas
rectification tower
tower
outlet
liquid
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PCT/CN2019/098066
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French (fr)
Chinese (zh)
Inventor
万和昌
万里鹏
万舒妤
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江西江氨科技有限公司
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Priority to PCT/CN2019/098066 priority Critical patent/WO2021016779A1/en
Publication of WO2021016779A1 publication Critical patent/WO2021016779A1/en

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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)
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Abstract

Disclosed in the present invention is an easy-to-implement food-grade CO2 preparation system, which comprises two rectifying towers. The two rectifying towers are correspondingly a first rectifying tower and a second rectifying tower; a first low boiler discharged from the top of the first rectifying tower enters a reboiler in the second rectifying tower so as to reboil a second reboiler entering the second rectifying tower; a liquid outlet is formed at the bottom of the second rectifying tower, and a second high boiler finished product in the second rectifying tower is discharged via the liquid outlet at the bottom.

Description

食品级CO 2的制备系统 Food grade CO 2 preparation system 技术领域Technical field
本发明涉及食品级二氧化碳生产技术领域，尤其涉及一种食品级CO 2的制备系统。 The invention relates to the technical field of food-grade carbon dioxide production, in particular to a food-grade CO 2 preparation system.
背景技术Background technique
传统食品级二氧化碳的生产一般采用分子筛脱水脱醇和催化燃烧法脱烃装置及其工艺，其在实施中需要大量的热量用于加热再生气体，能耗高、操作工艺复杂，其次，由于精馏前原料气中含有杂质气体及水分，其进入精馏塔前的温度需保持10-15度左右，若温度过低管路内的二氧化碳及水分极易产生水合物堵塞管路，但，温度过高又不利于后续精馏塔内精馏的进行，此生产工艺无疑于增加了企业的负担和生产成本。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. Secondly, due to the pre-rectification 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.
发明内容Summary of the invention
本发明的目的在于克服现有技术的不足，适应现实需要，公开一种易于实现的食品级CO2的制备系统。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.
为了实现本发明的目的，本发明所采用的技术方案为：In order to achieve the purpose of the present invention, the technical solutions adopted by the present invention are:
本发明提供一种食品级CO 2制备系统，它包括两个精馏塔，两个精馏塔分别为第一精馏塔、第二精馏塔； 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;
第一精馏塔底部富集第一高沸物，顶部富集第一低沸物；第二精馏塔底部富集第二高沸物，顶部富集第二低沸物；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;
第一精馏塔顶部排出的第一低沸物进入第二精馏塔内的再沸器中用于对进入第二精馏塔内的第二再沸物再沸以回收第一高沸物携带的热能。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.
第二精馏塔底部设有液体出口,第二精馏塔内的第二高沸物成品通过所述底部液体出口排出。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.
所述第二精馏塔内的再沸器出口排出的第一低沸物通过气液分离后，其液相进入第一精馏塔内，其气相经过热量回收后排空。After the first low boiler discharged from the outlet of the reboiler in the second rectification tower is separated from the gas and liquid, its liquid phase enters the first rectification tower, and the gas phase is evacuated after heat recovery.
经所述第二精馏塔顶部排出的第二低沸物经热量回收和气液分离后，其液相进入第二精馏塔内，其气相经过热量回收后排空。After heat recovery and gas-liquid separation of the second low boiler discharged from the top of the second rectification tower, its liquid phase enters the second rectification tower, and its gas phase is emptied after heat recovery.
根据原料气的组成，必要时在所述原料气进入第一精馏塔前的原料气管道内加入防冻液。According to the composition of the raw gas, if necessary, an antifreeze liquid is added to the raw gas pipeline before the raw gas enters the first rectification tower.
与所述第一精馏塔的原料气进口连接的管道上设有防冻液加入口。The pipe connected with the feed gas inlet of the first rectification tower is provided with an antifreeze inlet.
与所述第一精馏塔的原料气进口连接的管道上设有压缩机，原料气通过压缩机压缩后进入第一精馏塔内。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.
所述防冻液加入口设置于压缩机的前端或后端。The antifreeze liquid inlet is arranged at the front or rear end of the compressor.
原料气通过第一精馏塔的中部或下部进入第一精馏塔内，第一精馏塔内的再沸器与外部热源连接，第一精馏塔的底部出口为残液排出口并用于排出第一高沸物，第一精馏塔的顶部设有第一低沸物排气口；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;
还包括第一气液分离器，所述第一精馏塔顶部的第一低沸物排气口与第二精馏塔内的第二再沸器进口连通，第二精馏塔内的第二再沸器出口与第一气液分离器的进口连通，第一气液分离器的液相出口与第一精馏塔顶部的进口连通；It also includes a first gas-liquid separator. 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;
所述第二精馏塔的底部出口为成品排出口，还包括第二气液分离器、换热器，所述第一气液分离器的气相出口、第二精馏塔顶部的第二低沸物排气口均与换热器的进口连通，换热器的出口与第二气液分离器的进口连通，第二气液分离器的气相出口为废气出口，第二气液分离器的液相出口与第二精馏塔顶部的进口连通。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.
所述第一气液分离器的气相排出管上设有减压阀。The gas-phase discharge pipe of the first gas-liquid separator is provided with a pressure reducing valve.
本发明的有益效果在于：The beneficial effects of the present invention are:
本发明其结构设计新颖，相对于现有的食品级CO 2制备系统本设计更加合理，能源供给更加简单(仅需对第一精馏塔内的再沸器供能即可)，更易实现，能耗低，其次，通过在精馏前加入防冻液可避免原料气温度降低后出现管路内壁结晶堵塞管路现象的发生，提高制气效率和制气时系统的稳定性。 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.
附图说明Description of the drawings
图1为本发明的食品级CO 2制备系统原理示意图。 Figure 1 is a schematic diagram of the principle of the food-grade CO 2 preparation system of the present invention.
具体实施方式Detailed ways
下面结合附图和实施例对本发明进一步说明：The present invention will be further described below in conjunction with the drawings and embodiments:
实施例1：一种食品级CO 2制备系统，参见图1。 Example 1: A food-grade CO 2 preparation system, see Figure 1.
它包括两个精馏塔，两个精馏塔分别为第一精馏塔9、第二精馏塔16，本发明中，第一精馏塔底部富集第一高沸物，顶部富集第一低沸物；第二精馏塔底部富集第二高沸物，顶部富集第二低沸物；其中，第一精馏塔9的中部位置处设有原料气进口8，与所述第一精馏塔9的原料气进口8连接的管道上设有防冻液加入口3，同时，与所述第一精馏塔9的原料气进口8连接的管道上设有压缩机2，原料气经过缓冲罐1后经压缩机2压缩后进入第一精馏塔9内，而上述所述防冻液加入口3设置于压缩机2的前端或后端，在具体的使用中，其防冻液加入口3可根据实际需要进行增设。It includes two rectification towers. The two rectification towers are the first rectification tower 9 and the second rectification tower 16. In the present invention, 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.
进一步的，本设计中，第一精馏塔9内的再沸器6通过管路5与外部热源连接，第一精馏塔的底部出口7为残液排出口并用于排出第一高沸物，第一精馏塔9的顶部设有第一低沸物排气口11。Further, in this design, 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.
还包括第一气液分离器25，所述第一精馏塔9顶部的第一低沸物排气口11通过管路与第二精馏塔16内的第二再沸器14进口15连通，第二精馏塔16内的第二再沸器14出口13与第一气液分离器的进口26连通，第一气液分离器的液相出口27与第一精馏塔顶部的进口10连通。It also includes a first gas-liquid separator 25. 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.
进一步的，所述第二精馏塔9的底部出口为成品排出口12，还包括第二气液分离器20、换热器19，所述第一气液分离器25的气相出口24、第二精馏塔16顶部的第二低沸物排气口18均与换热器19的进口连通，换热器19的出口与第二气液分离器的进口21连通，第二气液分离器的气相出口23为废气出口，第二气液分离器的液相出口22与第二精馏塔顶部的进口17连通。Further, 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.
进一步的，本设计还在所述第一气液分离器24的气相排出管上设有减压阀28。Furthermore, the present design also has a pressure reducing valve 28 on the gas discharge pipe of the first gas-liquid separator 24.
本发明的食品级CO2制备系统其工作原理如下：The working principle of the food-grade CO2 preparation system of the present invention is as follows:
1、原料气通过缓冲罐后经压缩机2压缩，压缩后原料气中CO 2含量为70％-99.99％，气压为1.4-4.0Mpa，此时，通过防冻液加入口3加入防冻液防止气体在后续管路中因低温导致气中水合物凝结堵塞管路；此时，第一精馏塔内的再沸器6通过外部热源进行加热，进入再沸器6内的热源温度为5-40℃。 1. 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 ℃.
2、原料气进入第一精馏塔前经过换热器后将其温度降低(通过在精馏前将温度降低可提高精馏塔内部的精馏效率，可提高精馏塔内高沸点物质与低沸点物质的分离率，使其杂质气体尽可能的与二氧化碳分离，对于提高二氧化碳的纯度具有重要的意义)，而后原料气进入第一精馏塔内后被再沸器6再沸，再沸器出口排出热源温度为-9℃；原料气进入第一精馏塔内后，第一高沸物多为杂质并经第一精馏塔的底部出口7排出，排出的残夜中含有中CO 2含量为80％-95％，气压为1.4-4.0Mpa Mpa，温度为-11℃；第一精馏塔的第一低沸物中其CO 2浓度较高可被提取，此时，第一低沸物经过第一精馏塔内部的塔板精馏后，其第一低沸物气体通过顶部的第一低沸物排气口11排出，此时，将第一精馏塔排出的第一低沸物气体其CO 2含量为70％-98％，气压为1.4-4.0Mpa Mpa，温度为-15℃—-17℃。 2. 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. At this time, 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℃—-17℃.
3、经第一精馏塔排出的第一低沸物气体进入第二精馏塔内的再沸器中用于对进入第二精馏塔内的第二再沸物再沸，此步骤中，第二精馏塔内的再沸器无需通过外部能源供给，其第二再沸器14的能源均来自一精馏塔排出的第一低沸物气体。经第一精馏塔排出的第一低沸物气体经过第二再沸器后进入第一气液分离器25中进行气液分离，进入第一气液分离器前其CO 2含量为70％-98％，气压为1.4-4.0Mpa Mpa，温度为-17℃—-19℃。 3. 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. In this step 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℃—-19℃.
4、经第一气液分离器分离后，其液态物质通过第一精馏塔9的中部或下部进入第一精馏塔内再次进行精馏操作；其气相物质向上进入第二气液分离器内。4. 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.
5、第二再沸器对第二精馏塔内的第二再沸物进行再沸处理(第二精馏塔内的第二再沸物为经第二气液分离器分离后的液相物质)，经第二精馏塔再沸后的第二高沸物为成品，即食品级二氧化碳并经第二精馏塔底部的液体出口排出，排出后的成品其CO 2含量为99.997％，气压为2.2-2.3Mpa，温度为-19℃。 5. 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.
经第二精馏塔再沸后的第二低沸物(其CO 2含量为70％—80％，气压为2.2-2.3Mpa，温度为-18℃—-20℃)与经第一气液分离器分离后的气相物会同后一并经过换热器后进入第二气液分离器内进行气液分离。 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.
6、经第二气液分离器后，其气相物为残气并排出整个系统，此时，其CO 2含量为40％—60％，气压为2.2-2.3Mpa，温度为-25℃—-40℃；其液相物质再次进入第二精馏塔内形成第二再沸物再次进行再沸及精馏处理，此时其液相物质中CO 2含量为85％左右。而经第二精馏塔再沸后的第二高沸物为成品，即食品级二氧化碳并经第二精馏塔底部的液 体出口排出，排出后的成品其CO 2含量为99.997％，气压为2.2-2.3Mpa，温度为-19℃。 6. After passing through the second gas-liquid separator, the gas phase is the residual gas and is discharged from the entire system. At this time, the CO 2 content is 40%-60%, the air pressure is 2.2-2.3Mpa, and the temperature is -25℃—- 40°C; the liquid phase material enters the second rectification tower again to form a second reboiler and is reboiled and rectified again. At this time, 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℃.
如此通过上述步骤可制备出高纯度(99.997％)的食品级二氧化碳，通过上述可发现，本设计中其第一精馏塔、第一气液分离器可构成二次循环的精馏提纯过程，而换热器、第二气液分离器及第二精馏塔可构成三次循环精馏提纯过程，通过上述三次的循环过程可实现高纯度的食品级二氧化碳制备。In this way, high-purity (99.997%) food-grade carbon dioxide can be prepared through the above steps. From the above, it can be found that 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.
本发明的实施例公布的是较佳的实施例，但并不局限于此，本领域的普通技术人员，极易根据上述实施例，领会本发明的精神，并做出不同的引申和变化，但只要不脱离本发明的精神，都在本发明的保护范围内。The embodiment of the present invention discloses a preferred embodiment, but it is not limited to this. Those of ordinary skill in the art can easily understand the spirit of the present invention and make different extensions and changes based on the above embodiments. However, as long as they do not depart from the spirit of the present invention, they are all within the protection scope of the present invention.

Claims (9)

  1. 一种食品级CO 2制备系统，它包括两个精馏塔，两个精馏塔分别为第一精馏塔、第二精馏塔；第一精馏塔底部富集第一高沸物，顶部富集第一低沸物；第二精馏塔底部富集第二高沸物，顶部富集第二低沸物；其特征在于： A food-grade CO 2 production system, which includes two rectification towers, the two rectification towers are respectively the first rectification tower and the second rectification tower; the bottom of the first rectification tower is enriched with the first high boiler, 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; it is characterized by:
    第一精馏塔排出的第一低沸物进入第二精馏塔内的再沸器中用于对进入第二精馏塔内的第二再沸物再沸；The first low boiler discharged from the first rectifying tower enters the reboiler in the second rectifying tower to reboil the second reboiler entering the second rectifying tower;
    第二精馏塔底部设有液体出口,第二精馏塔内的第二高沸物成品通过底部的液体出口排出。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 liquid outlet at the bottom.
  2. 如权利要求1所述的食品级CO 2制备系统，其特征在于：所述第二精馏塔内的再沸器出口排出的第一低沸物通过气液分离后、其液相进入第一精馏塔内，其气相经过热量回收后排空。 The food-grade CO 2 production system according to claim 1, characterized in that: the first low boiler discharged from the outlet of the reboiler in the second rectification column passes through gas-liquid separation, and its liquid phase enters the first In the distillation tower, the gas phase is emptied after heat recovery.
  3. 如权利要求2所述的食品级CO 2制备系统，其特征在于：经所述第二精馏塔排出的低沸物经气液分离后，其液相进入第二精馏塔内，其气相经过热量回收后排空。 The food-grade CO 2 production system according to claim 2, characterized in that: after the low boilers discharged from the second rectification tower are separated from gas and liquid, the liquid phase enters the second rectification tower, and the gas phase Evacuate after heat recovery.
  4. 如权利要求1所述的食品级CO 2制备系统，其特征在于：在所述原料气进入第一精馏塔前的原料气管道内加入防冻液。 The food-grade CO 2 preparation system according to claim 1, wherein an antifreeze liquid is added into the raw gas pipeline before the raw gas enters the first distillation tower.
  5. 如权利要求4所述的食品级CO 2制备系统，其特征在于：与所述第一精馏塔的原料气进口连接的管道上设有防冻液加入口。 The food-grade CO 2 preparation system according to claim 4, characterized in that the pipe connected with the feed gas inlet of the first rectification tower is provided with an antifreeze inlet.
  6. 如权利要求5所述的食品级CO 2制备系统，其特征在于：与所述第一精馏塔的原料气进口连接的管道上设有压缩机，原料气通过压缩机压缩后进入第一精馏塔内。 The food-grade CO 2 preparation system according to claim 5, characterized in that: a compressor is provided on the pipe connected to the feed gas inlet of the first rectification tower, and the feed gas enters the first refinery after being compressed by the compressor Inside the distillation tower.
  7. 如权利要求6所述的食品级CO 2制备系统，其特征在于：所述防冻液加入口设置于压缩机的前端或后端。 The food-grade CO 2 preparation system according to claim 6, wherein the antifreeze adding port is arranged at the front or rear end of the compressor.
  8. 如权利要求1所述的食品级CO 2制备系统，其特征在于：原料气通过第一精馏塔的进气口进入第一精馏塔内，第一精馏塔内的再沸器与外部热源连接，第一精馏塔的底部出口为残液排出口并用于排出第一高沸物，第一精馏塔的设有第一低沸物排气口； The food-grade CO 2 production system according to claim 1, wherein the raw material gas enters the first rectification tower through the air inlet of the first rectification tower, and the reboiler in the first rectification tower and the outside The heat source is connected, the bottom outlet of the first rectification tower is a residual liquid discharge outlet and is used to discharge the first high boiler, and the first rectification tower is provided with a first low boiler exhaust port;
    还包括第一气液分离器，所述第一精馏塔的第一低沸物排气口与第二精馏塔内的第二再沸器进口连通，第二精馏塔内的第二再沸器出口与第一气液分离器的进口连通，第一气液分离器的液相出口与第一精馏塔的进口连通；It also includes a first gas-liquid separator, the first low-boiler exhaust port of the first rectification tower is in communication with the second reboiler inlet in the second rectification tower, and the second The outlet of the 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 of the first distillation tower;
    所述第二精馏塔的底部出口为成品排出口，还包括第二气液分离器、换热器，所述第一气液分离器的气相出口、第二精馏塔的第二低沸物排气口均与换热器的进口连通，换热器的出口与第二气液分离器的进口连通，第二气液分离器的气相出口为废气出口，第二气液分离器的液相出口与第二精馏塔顶部的进口连通。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 boiling point of the second rectification tower The gas 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 liquid of the second gas-liquid separator The phase outlet is connected with the inlet at the top of the second rectification tower.
  9. 如权利要求8所述的食品级CO 2制备系统，其特征在于：所述第一气液分离器的气相排出管上设有减压阀。 The food-grade CO 2 preparation system according to claim 8, wherein the gas-phase discharge pipe of the first gas-liquid separator is provided with a pressure reducing valve.
PCT/CN2019/098066 2019-07-27 2019-07-27 Food-grade co2 preparation system WO2021016779A1 (en)

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CN101691320A (en) * 2009-10-14 2010-04-07 清华大学 Method for purifying and recycling methane and carbon dioxide from landfill gas and device thereof
CN104654739A (en) * 2015-02-02 2015-05-27 河南心连心深冷能源股份有限公司 Device and method for preparing food-grade liquid carbon dioxide by rectification and purification with double towers
CN104748506A (en) * 2015-03-13 2015-07-01 河南心连心深冷能源股份有限公司 Device for recycling CO2 from oil field mining assisting tail gas and process thereof

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CN101691320A (en) * 2009-10-14 2010-04-07 清华大学 Method for purifying and recycling methane and carbon dioxide from landfill gas and device thereof
CN104654739A (en) * 2015-02-02 2015-05-27 河南心连心深冷能源股份有限公司 Device and method for preparing food-grade liquid carbon dioxide by rectification and purification with double towers
CN104748506A (en) * 2015-03-13 2015-07-01 河南心连心深冷能源股份有限公司 Device for recycling CO2 from oil field mining assisting tail gas and process thereof

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CN114963691A (en) * 2022-05-31 2022-08-30 山东石油化工学院 Low pressure CO 2 Low-temperature gas separation method and device
CN114963691B (en) * 2022-05-31 2023-12-26 山东石油化工学院 Low pressure CO 2 Gas low-temperature separation method and device

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