WO2013117033A1 - 基于小型低温制冷机的用于气体分离和纯化的低温装置 - Google Patents

基于小型低温制冷机的用于气体分离和纯化的低温装置 Download PDF

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WO2013117033A1
WO2013117033A1 PCT/CN2012/072943 CN2012072943W WO2013117033A1 WO 2013117033 A1 WO2013117033 A1 WO 2013117033A1 CN 2012072943 W CN2012072943 W CN 2012072943W WO 2013117033 A1 WO2013117033 A1 WO 2013117033A1
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Prior art keywords
heat exchanger
gas
cold head
primary
outlet
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PCT/CN2012/072943
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English (en)
French (fr)
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董文庆
巢伟
陈杰
李奥
高金林
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南京柯德超低温技术有限公司
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Priority to EP12867912.3A priority Critical patent/EP2829830B1/en
Priority to US14/378,019 priority patent/US9752824B2/en
Priority to JP2014555919A priority patent/JP6051236B2/ja
Publication of WO2013117033A1 publication Critical patent/WO2013117033A1/zh

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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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or 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
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/02—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point using Joule-Thompson effect; using vortex effect
    • 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
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling 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
    • F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/14—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle
    • F25B9/145—Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the cycle used, e.g. Stirling cycle pulse-tube 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0685—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of noble gases
    • 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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0685—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of noble gases
    • F25J3/069—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of noble gases of helium
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • 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
    • F25J2215/30—Helium
    • 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
    • F25J2215/32—Neon
    • 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
    • F25J2270/908—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by regenerative chillers, i.e. oscillating or dynamic systems, e.g. Stirling refrigerator, thermoelectric ("Peltier") or magnetic refrigeration

Definitions

  • the present invention relates to a cryogenic apparatus for gas separation and purification, and more particularly to a cryogenic apparatus for gas separation and purification based on a small cryogenic refrigerator.
  • the separation and purification of the gas of each component in the impurity-containing feed gas is a basic process for obtaining a high purity (99.999% by volume or more) gas. Separation is usually carried out by utilizing the difference between the condensation temperature and the molecular property of each component gas.
  • the conventional methods include rectification, fractionation, adsorption, and catalytic reaction. When the product gas requires high purity, several methods are needed in combination, such as a combination of high pressure low temperature condensation and low temperature adsorption or a combination of pressure swing adsorption and low temperature adsorption at normal temperature.
  • the traditional separation and purification method has a complicated process and high investment cost, and is usually used for large-scale gas separation and purification equipment.
  • rare gases such as helium and neon
  • rare gases such as helium and neon
  • the demand is increasing. What is important is that China is a barren country, and the United States, as the world’s leading exporter, has listed it as a strategic resource. Therefore, the recycling and recycling of hydrazine is particularly important; in addition, the extraction from the air separation unit is one of the ways to obtain bismuth and bismuth in the industry.
  • the purity is about 90%, and the rest is mainly impurity gases such as air.
  • This purity of helium is usually not directly usable and requires special separation and purification procedures.
  • the traditional methods generally include the extraction of crude mixture gas, the preparation of pure helium gas mixture and the preparation of pure helium and pure helium.
  • the three process procedures are complex, high in investment cost, and lack of economy, and are rarely used in actual air separation plants.
  • Small cryogenic refrigerators generally include GM refrigerators, pulse tube refrigerators, Stirling refrigerators, J-T refrigerators, and the like. Small cryogenic refrigerators typically have a cooling temperature range of 0 – 80 K (-273.15 ° C – -193.15 ° C), cooling capacity is about 0.1 – 100 W. Small cryogenic refrigerators are important equipment for obtaining extremely low temperatures. Low temperature devices for gas separation and purification based on small cryogenic refrigerators are suitable for small gas separation and purification.
  • the present invention provides a method for gas separation and purification based on a small cryogenic refrigerator.
  • the traditional separation and purification scheme is improved.
  • the first stage and the second stage cold head of the small-sized cryogenic refrigerator are used as a cold source, and gases of different condensation temperatures are respectively liquefied and solidified, thereby obtaining a high-purity gas with a lower condensation temperature (such as: helium), other high purity gases that have been liquefied and have higher condensation temperatures are also available. This allows separation and purification of two or more gases at a lower cost.
  • a cryogenic device for gas separation and purification based on a small cryogenic refrigerator comprising: a primary heat exchanger, a secondary heat exchanger, a four-stage heat exchanger, at least one small cryogenic refrigerator, and at least one a small-scale cryogenic refrigerator comprising a first cold head and a second cold head, wherein the secondary heat exchanger is disposed on the first cold head to form a first-stage cold head heat exchanger, The fourth-stage heat exchanger is disposed on the second cold head to form a secondary cold head heat exchanger, and the first-stage heat exchanger is provided with a mixed gas inlet, a mixed gas outlet, a purified gas inlet, and a purified a gas outlet, the mixed gas outlet is connected to the inlet of the primary cold head heat exchanger, an outlet of the primary cold head heat exchanger is connected to the inlet of the liquid collection tank, and the gas outlet of the liquid collection tank is connected to the secondary The head of the cold head heat exchanger is connected to the outlet of the secondary cold head heat exchanger and is
  • a three-stage heat exchanger is further disposed between the liquid collection tank gas outlet and the secondary cold head heat exchanger inlet, and the secondary cold head heat exchanger outlet also passes through the third-stage heat exchange.
  • the gas is connected to the primary end of the primary heat exchanger for purification.
  • another chiller including a primary heat exchange tank located at the first cold head and a secondary heat exchange tank located at the second cold head, the liquid outlet of the liquid collection tank being cooled by the first stage
  • the head heat exchanger enters the cold end of the primary heat exchanger to purify the gas, and the gas outlet of the liquid collecting tank is connected to the secondary cold head heat exchanger inlet through the first heat exchange tank.
  • the outlet of the secondary cold head heat exchanger is connected to another liquid collecting tank, and the gas outlet of the other liquid collecting tank is connected to the cold end of the primary heat exchanger through the secondary heat exchange tank to be purified
  • the liquid outlet of the other liquid collecting tank is purified by the first-stage cold head heat exchanger and the first-stage heat exchange tank into the cold end of the first-stage heat exchanger, and the hot end of the first-stage heat exchanger is purified.
  • the first stage heat exchanger, the second stage heat exchanger, the third stage heat exchanger and the fourth stage heat exchanger type are a coil heat exchanger, a coil heat exchanger, a plate heat exchanger or a fin type change Heater.
  • the small cryogenic refrigerator is a GM refrigerator, a pulse tube refrigerator, a Stirling refrigerator or a J-T refrigerator.
  • the invention introduces a small-sized cryogenic refrigerator into a conventional gas separation and purification system, and uses a first-stage and a second-stage cold head of a small-sized cryogenic refrigerator as a cold source to separately liquefy and solidify other gases of different condensation temperatures, and a condensation temperature.
  • a first-stage and a second-stage cold head of a small-sized cryogenic refrigerator as a cold source to separately liquefy and solidify other gases of different condensation temperatures, and a condensation temperature.
  • FIG. 1 is a schematic diagram of a cryogenic apparatus system for gas separation and purification based on a GM refrigerator for obtaining high purity helium and nitrogen according to the present invention.
  • FIG. 2 is a schematic diagram of a cryogenic apparatus system for gas separation and purification based on a GM refrigerator for obtaining high purity helium, neon and nitrogen gas.
  • Embodiment 1 is a cryogenic apparatus for gas separation and purification based on a GM refrigerator that obtains high purity helium and nitrogen.
  • Low-temperature device for gas separation and purification based on GM refrigerator including mixed gas inlet 1, primary heat exchanger 2, secondary heat exchanger 3, liquid collecting tank 4, tertiary heat exchanger 5, four-stage exchange Heater 6, helium gas outlet 7, nitrogen outlet 8, GM refrigerator 9, and vacuum hood 10, the mixed gas inlet 1 is connected to the hot end inlet of the primary heat exchanger 2, and the cold end outlet of the primary heat exchanger 2 is connected.
  • the secondary heat exchanger 3 is imported, the secondary heat exchanger 3 is wound on the first cold head of the GM refrigerator, the outlet of the secondary heat exchanger 3 is connected to the gas inlet of the liquid collecting tank 4, and the gas outlet of the liquid collecting tank 4 is connected to the third
  • the heat exchanger inlet of the stage heat exchanger 5, the cold end outlet of the third stage heat exchanger 5 is connected to the inlet of the fourth stage heat exchanger 6, the fourth stage heat exchanger 6 is coiled on the secondary cold head of the GM refrigerator, and the fourth stage heat exchanger 6 outlet is connected to the cold end inlet of the third stage heat exchanger 5, the hot end outlet of the third stage heat exchanger 5 is connected to the cold end inlet of the first stage heat exchanger 2, and the hot end outlet of the first stage heat exchanger 2 is connected to the helium outlet 7
  • the liquid outlet of the header tank 4 is connected to the nitrogen outlet 8.
  • the low-temperature device for gas separation and purification based on a GM refrigerator obtained by obtaining high-purity helium gas and nitrogen gas has the following work flow:
  • the raw material gas (including helium and nitrogen) enters the system from the mixed gas inlet 1 and then enters the primary heat exchanger 2 for pre-cooling. After pre-cooling to a lower temperature, it enters the secondary heat exchanger 3 for further cooling.
  • the heat exchanger 3 is wound around the primary cold head of the GM refrigerator 9.
  • the raw material gas leaves the outlet of the secondary heat exchanger 3, it is a gas-liquid mixture, and most of the nitrogen in the raw material gas has been liquefied, and the gas-liquid mixture enters the liquid collecting tank 4 to perform gas-liquid separation, and the liquid is at the bottom of the liquid collecting tank 4. At this time, the gas leaving the liquid collection tank 4 still contains a small amount of nitrogen which is not liquefied.
  • the helium gas and a small amount of unliquefied nitrogen leave the liquid collection tank 4 and enter the tertiary heat exchanger 5 to be cooled again.
  • a small amount of unliquefied nitrogen gas is solidified in the tertiary heat exchanger 5, and is changed from the third stage.
  • the purity of helium from the cold end of the heat exchanger 5 is above 99.999%, which is high purity gas.
  • the high-purity gas enters the fourth-stage heat exchanger 6, and the fourth-stage heat exchanger 6 is wound around the secondary cold head of the GM refrigerator 9, and the temperature of the helium gas leaving the fourth-stage heat exchanger 6 reaches a minimum value.
  • the gas first passes through the third-stage heat exchanger 5 and then passes through the first-stage heat exchanger 2 and then returns to the normal temperature to reach the helium gas outlet 7, and the liquefied nitrogen gas in the liquid collection tank 4 automatically controls the discharge at intervals.
  • the second embodiment is a cryogenic device for gas separation and purification based on a GM refrigerator for obtaining high purity helium, neon and nitrogen gas.
  • Low-temperature device for gas separation and purification based on GM refrigerator including raw material gas inlet 11, primary heat exchanger 12, primary cold head heat exchanger 13, liquid collecting tank-14, secondary cold head heat exchanger 15, liquid tank II 16, first stage heat exchange tank 17, secondary heat exchange tank 18, GM refrigerator 19, GM refrigerator 2, nitrogen outlet 21, helium gas outlet 22, helium gas outlet 23 and vacuum hood twenty four.
  • the invention relates to a cryogenic device for gas separation and purification based on a GM refrigerator which obtains high purity helium, neon and nitrogen gas, and the working process is as follows:
  • the feed gas (containing helium, neon, and nitrogen) is first introduced into the primary heat exchanger 12 from the feed gas inlet 11 for pre-cooling.
  • the raw material gas precooled by the primary heat exchanger 12 enters the primary cold head heat exchanger 13 to further cool down, liquefies the nitrogen in the raw material gas, and the raw material gas is converted into the outlet at the outlet of the primary cold head heat exchanger 13 A gas-liquid mixture of liquid nitrogen, gaseous nitrogen, helium and neon.
  • the gas-liquid mixture flows out of the primary cold head heat exchanger 13, it flows into the liquid collecting tank 14, and the gas and the liquid are separated in the liquid collecting tank 14, and the separated liquid nitrogen is returned to the primary heat exchanger 12.
  • the raw material gas is pre-cooled, and the separated helium gas, helium gas, and nitrogen gas that has not been liquefied enter the primary heat exchange tank 17 to continue cooling.
  • the unliquefied nitrogen gas is solidified in the primary heat exchange tank 17, and the gas flowing out of the primary heat exchange tank 17 is a mixed gas of helium and neon.
  • the mixed gas of helium and neon enters the secondary cold head heat exchanger 15 to further cool, and the helium gas therein is liquefied, and the mixed gas of helium and neon is converted into the outlet of the secondary cold head heat exchanger 15 to include A gas-liquid mixture of liquid helium, gaseous helium and helium.
  • the gas-liquid mixture of the liquid helium gas, the gaseous helium gas and the helium gas flows out of the secondary cold head heat exchanger 15, and then flows into the liquid collecting tank 2, and the gas and the liquid are separated in the liquid collecting tank 26, and the separated Helium and helium gas that is not liquefied enter the secondary heat exchange tank 18.
  • the helium gas that is not liquefied is solidified in the secondary heat exchange tank 18, the gas flowing out of the secondary heat exchange tank 18 is low-temperature high-purity helium gas, and the low-temperature high-purity helium gas is returned to the first-stage heat exchanger 12, Cold and normal temperature raw material gas, helium gas is rewarmed to normal temperature, you can get high temperature pure helium at room temperature.
  • the separated liquid helium gas is returned to the first-stage cold head heat exchanger 13, and the raw material gas precooled by the first-stage heat exchanger 12 is pre-cooled, and the liquid helium gas is converted into a gaseous state by the heat absorption and is rewarmed.
  • the temperature is again lowered, and then flows into the first-stage heat exchanger 12 to pre-cool the normal-temperature raw material gas, and the low-temperature helium gas is rewarmed to the normal temperature in the first-stage heat exchanger 12 to obtain the normal temperature.
  • High purity helium is also lowered, and then flows into the first-stage heat exchanger 12 to pre-cool the normal-temperature raw material gas, and the low-temperature helium gas is rewarmed to the normal temperature in the first-stage heat exchanger 12 to obtain the normal temperature.
  • the first embodiment and the second embodiment only cite the principles and methods for obtaining two product gases and three product gases. If more product gas is required, it needs to be improved on the basis of obtaining three product gases.

Abstract

一种基于小型低温制冷机的用于气体分离和纯化的低温装置，包括一级换热器、二级换热器、四级换热器、至少一个小型低温制冷机以及至少一个集液罐，小型低温制冷机包括第一冷头和第二冷头，二级换热器设置在第一冷头上形成一级冷头换热器，四级换热器设置在第二冷头上形成二级冷头换热器，混合气体出口连接至一级冷头换热器入口，一级冷头换热器的出口连接集液罐的入口，集液罐气体出口连接到二级冷头换热器进口。通过用小型低温制冷机的第一级和第二级冷头作为冷源，将不同冷凝温度的气体分别液化和固化，从而得到冷凝温度更低的高纯气体，这样就可以用较低的成本来实现两种或多种气体的分离和纯化。

Description

基于小型低温制冷机的用于气体分离和纯化的低温装置 技术领域
本发明涉及一种气体分离和纯化的低温装置，尤其是一种基于小型低温制冷机的用于气体分离和纯化的低温装置。
 背景技术
含杂质原料气中各组分气体的分离和纯化是获得高纯度（体积百分含量99.999%或以上）气体的基本过程。通常利用各组分气体冷凝温度和分子性质之间的差异来进行分离，传统的方法有：精馏法、分凝法、吸附法、催化反应法等。当产品气要求纯度较高时，需要几种方法联合使用，如高压低温冷凝和低温吸附相结合的方法或常温下的变压吸附和低温吸附相结合的方法等。传统的分离纯化方法流程复杂，投资成本高，通常用于大型的气体分离纯化设备。
一般来说，氦、氖等稀有气体的分离和纯化也是基于以上几种常用方法。稀有气体中，氦气、氖气等稀有气体在航空、航天、军事和科研等领域有着非常重要的应用，且需求量日益增大。重要的是我国属于贫氦国家，美国作为世界上主要的氦出口国已经将氦列为战略资源。因此，氦的回收再利用就显得尤为重要；此外，从空分装置中提取是工业上获得氦、氖的途径之一。
对于回收的氦气，其纯度在90%左右，其余主要是空气等杂质气体。这个纯度的氦气通常无法直接使用，需要经过特别的分离和纯化流程。对于空分装置中氦气、氖气的分离和纯化，传统方法一般包括粗氦氖混合气的提取、纯氦氖混合气的制备和纯氦、纯氖的制备三个工序。三道工序流程都比较复杂，投资成本高，缺乏经济性，一般很少应用于实际的空分装置中。
小型低温制冷机一般包括GM制冷机，脉管制冷机，斯特林制冷机，J-T制冷机等。小型低温制冷机的制冷温度范围一般在0 – 80 K（-273.15℃– -193.15℃），制冷量大约在0.1 – 100 W。小型低温制冷机是获得极低温的重要设备。基于小型低温制冷机的用于气体分离和纯化的低温装置则适合用于小型的气体分离和纯化。
 技术问题
本发明提供了一种基于小型低温制冷机的用于气体分离和纯化的方法。改进了传统的分离和纯化方案，用小型低温制冷机的第一级和第二级冷头作为冷源，将不同冷凝温度的气体分别液化和固化，从而得到冷凝温度更低的高纯气体（如：氦气），已经液化的其它冷凝温度较高的高纯气体同样可以获得。这样就可以用较低的成本来实现两种或多种气体的分离和纯化。
本发明的技术方案是：
一种基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是：包括一级换热器、二级换热器、四级换热器、至少一个小型低温制冷机以及至少一个集液罐，所述的小型低温制冷机包括第一冷头和第二冷头，所述的二级换热器设置在所述的第一冷头上形成一级冷头换热器，所述的四级换热器设置在第二冷头上形成二级冷头换热器，在所述的一级换热器上设置有混合气体进口、混合气体出口、纯化后气体进口以及纯化后气体出口，所述的混合气体出口连接至所述的一级冷头换热器入口，一级冷头换热器的出口连接所述集液罐的入口，集液罐气体出口连接到二级冷头换热器进口，二级冷头换热器出口连接到一级换热器冷端纯化后气体一进口，一级换热器热端为纯化后气体一出口。
在所述的集液罐气体出口与二级冷头换热器进口之间还设置有一三级换热器，所述的二级冷头换热器出口也经过所述的三级换热器连接至一级换热器冷端纯化后气体一进口。
还包括另一制冷机，该另一制冷机包括位于第一冷头的一级换热罐和位于第二冷头的二级换热罐，所述的集液罐的液体出口经一级冷头换热器进入一级换热器的冷端纯化后气体一进口，所述的集液罐的气体出口经过所述的一级换热罐连接至所述的二级冷头换热器进口，二级冷头换热器的出口连接另一集液罐，该另一集液罐的气体出口经过所述的二级换热罐连接至一级换热器的冷端纯化后气体二进口，所述另一集液罐的液体出口经一级冷头换热器和一级换热罐进入一级换热器的冷端纯化后气体三进口，一级换热器热端为纯化后气体一出口、气体二出口和气体三出口。
所述的一级换热器、二级换热器、三级换热器和四级换热器类型为绕管换热器、盘管式换热器、板式换热器或翅片式换热器。
所述的小型低温制冷机为GM制冷机、脉管制冷机、斯特林制冷机或J-T制冷机。
 有益效果
本发明将小型低温制冷机引入到传统的气体分离和纯化系统中，用小型低温制冷机第一级和第二级冷头作为冷源，将不同冷凝温度的其它气体分别液化和固化，冷凝温度较高的气体在制冷机第一级冷头液化后，冷凝温度较低的气体纯度将达到99%以上，依然存在1%左右的杂质气体未被液化，这就需要温度更低的冷源（制冷机第二级冷头提供）将杂质气体固化，冷源温度越低，气体纯度越高，经过固化后的气体纯度通常达到99.999%以上。这样就可以用较低的成本来实现两种或多种气体的分离和纯化。
附图说明
图1是本发明获得高纯氦气和氮气的基于GM制冷机的用于气体分离和纯化的低温装置系统原理图
图2是获得高纯氦气、氖气和氮气三种产品气的基于GM制冷机的用于气体分离和纯化的低温装置系统原理图
 本发明的实施方式
下面结合附图和实施例对本发明作进一步的说明。
实施例一为获得高纯氦气和氮气的基于GM制冷机的用于气体分离和纯化的低温装置。
如图1所示。基于GM制冷机的用于气体分离和纯化的低温装置，包括混合气进口1、一级换热器2、二级换热器3、集液罐4、三级换热器5、四级换热器6、氦气出口7、氮气出口8、GM制冷机9、和真空罩10，所述混合气进口1连接一级换热器2热端进口，一级换热器2冷端出口连接二级换热器3进口，二级换热器3盘绕在GM制冷机一级冷头上，二级换热器3出口连接到集液罐4气体进口，集液罐4气体出口连接到三级换热器5热端进口，三级换热器5冷端出口连接到四级换热器6进口，四级换热器6盘绕在GM制冷机二级冷头上，四级换热器6出口连接到三级换热器5冷端进口，三级换热器5热端出口连接到一级换热器2冷端进口，一级换热器2热端出口连接到氦气出口7，集液罐4液体出口连接到氮气出口8。GM制冷机9的一级、二级冷头部分，一级换热器2，二级换热器3，三级换热器4，四级换热器5和集液罐4均置于真空罩10中。
所述的获得高纯氦气和氮气的一种基于GM制冷机的用于气体分离和纯化的低温装置，其工作流程如下：
原料气（含氦气和氮气）从混合气进口1进入系统后首先进入一级换热器2预冷，预冷到较低温度后再进入到二级换热器3中进一步冷却，二级换热器3盘绕在GM制冷机9的一级冷头上。
所述原料气离开二级换热器3出口时是气液混合物，原料气中的绝大部分氮气已经液化，气液混合物进入集液罐4后进行气液分离，液体在集液罐4底部聚集，此时，离开集液罐4的气体里面依然含有少量未被液化的氮气。
所述氦气及少量未被液化的氮气离开集液罐4进入到三级换热器5中再次冷却，之前少量的未被液化的氮气在三级换热器5中固化，从三级换热器5冷端出来的氦气纯度达到了99.999%以上，为高纯气。
所述高纯气进入到四级换热器6中，四级换热器6盘绕在GM制冷机9的二级冷头上，离开四级换热器6的氦气温度达到最低值，氦气首先经过三级换热器5再经过一级换热器2后恢复到常温到达氦气出口7，集液罐4中液化的氮气每隔一段时间自动控制排放。
实施例二为获得高纯氦气、氖气和氮气三种产品气的基于GM制冷机的用于气体分离和纯化的低温装置。
如图2所示。基于GM制冷机的用于气体分离和纯化的低温装置，包括原料气进口11，一级换热器12，一级冷头换热器13，集液罐一14，二级冷头换热器15，集液罐二16，一级换热罐17，二级换热罐18，GM制冷机一19，GM制冷机二20，氮气出口21，氦气出口22，氖气出口23和真空罩24。
所述的获得高纯氦气、氖气和氮气三种产品气的一种基于GM制冷机的用于气体分离和纯化的低温装置，其工作流程如下：
原料气（含氦气、氖气和氮气）从原料气进口11首先进入一级换热器12中进行预冷。经所述一级换热器12预冷后的原料气进入一级冷头换热器13进一步降温，将原料气中的氮气液化，原料气在一级冷头换热器13出口转变为包含液态氮气、气态氮气、氦气和氖气的气液混合物。
所述气液混合物流出一级冷头换热器13后，流入集液罐一14，在集液罐一14中将气体和液体分离，分离后的液态氮气回流至一级换热器12中预冷原料气，分离后的氦气、氖气以及未被液化的氮气进入一级换热罐17继续降温。
所述未被液化的氮气在一级换热罐17中被固化，流出一级换热罐17的气体为氦气和氖气的混合气体。
所述氦气和氖气的混合气体进入二级冷头换热器15进一步降温，将其中的氖气液化，氦气和氖气的混合气体在二级冷头换热器15出口转变为包含液态氖气、气态氖气和氦气的气液混合物。
所述液态氖气、气态氖气和氦气的气液混合物流出二级冷头换热器15后，流入集液罐二16，在集液罐二16中将气体和液体分离，分离后的氦气以及未被液化的氖气进入二级换热罐18。
所述未被液化的氖气在二级换热罐18中被固化，流出二级换热罐18的气体为低温高纯氦气，低温高纯氦气回流至一级换热器12，预冷常温原料气，氦气被复温至常温，即可获得常温高纯氦气。
所述的分离后的液态氖气回流至一级冷头换热器13，预冷经一级换热器12预冷后的原料气，液态氖气吸热转变成气态且被复温，被复温后的氖气进入一级换热罐17再次降温后流入一级换热器12预冷常温原料气，低温氖气在一级换热器12中被复温至常温，即可获得常温高纯氖气。
本实施例一和实施例二只是列举了获得两种产品气和三种产品气的原理和方法，如需要获得更多的产品气则需要在获得三种产品气的基础上加以改进得到。
本发明未涉及部分均与现有技术相同或可采用现有技术加以实现。

Claims (5)

  1. 一种基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是：包括一级换热器（2）、二级换热器（3）、四级换热器（6）、至少一个小型低温制冷机（9）以及至少一个集液罐（4），所述的小型低温制冷机（9）包括第一冷头和第二冷头，所述的二级换热器（3）设置在所述的第一冷头上形成一级冷头换热器，所述的四级换热器（6）设置在第二冷头上形成二级冷头换热器，在所述的一级换热器（2）上设置有混合气体进口、混合气体出口、纯化后气体进口以及纯化后气体出口，所述的混合气体出口连接至所述的一级冷头换热器入口，一级冷头换热器的出口连接所述集液罐（4）的入口，集液罐（4）气体出口连接到二级冷头换热器进口，二级冷头换热器出口连接到一级换热器（2）冷端纯化后气体一进口，一级换热器（2）热端为纯化后气体一出口。
  2. 根据权利要求1所述的基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是：在所述的集液罐气体出口与二级冷头换热器进口之间还设置有一三级换热器（5），所述的二级冷头换热器出口也经过所述的三级换热器（5）连接至一级换热器（2）冷端纯化后气体一进口。
  3. 根据权利要求1所述的基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是：还包括另一制冷机，该另一制冷机包括位于第一冷头的一级换热罐和位于第二冷头的二级换热罐，所述的集液罐的液体出口经一级冷头换热器进入一级换热器的冷端纯化后气体一进口，所述的集液罐的气体出口经过所述的一级换热罐连接至所述的二级冷头换热器进口，二级冷头换热器的出口连接另一集液罐，该另一集液罐的气体出口经过所述的二级换热罐连接至一级换热器的冷端纯化后气体二进口，所述另一集液罐的液体出口经一级冷头换热器和一级换热罐进入一级换热器的冷端纯化后气体三进口，一级换热器热端为纯化后气体一出口、气体二出口和气体三出口。
  4. 根据权利要求1、2或3所述的一种基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是所述的一级换热器、二级换热器、三级换热器和四级换热器类型为绕管换热器、盘管式换热器、板式换热器或翅片式换热器。
  5. 根据权利要求4所述的一种基于小型低温制冷机的用于气体分离和纯化的低温装置，其特征是所述的小型低温制冷机为GM制冷机、脉管制冷机、斯特林制冷机或J-T制冷机。
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