CN106642996A - Cryogenic rectification device and method in process argon recovery system - Google Patents

Cryogenic rectification device and method in process argon recovery system Download PDF

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Publication number
CN106642996A
CN106642996A CN201611184614.5A CN201611184614A CN106642996A CN 106642996 A CN106642996 A CN 106642996A CN 201611184614 A CN201611184614 A CN 201611184614A CN 106642996 A CN106642996 A CN 106642996A
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China
Prior art keywords
argon
cryogenic
gas
condenser
argon gas
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CN201611184614.5A
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Chinese (zh)
Inventor
文顺清
顾燕新
王军辉
李相承
尤文月
陈霞
孔芬霞
王清清
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Hangzhou Hangyang Co Ltd
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Hangzhou Hangyang Co Ltd
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Priority to CN201611184614.5A priority Critical patent/CN106642996A/en
Publication of CN106642996A publication Critical patent/CN106642996A/en
Pending legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/58—Argon
    • 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
    • F25J2215/58—Argon
    • 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
    • F25J2220/02—Separating impurities in general from 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
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

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

Abstract

Disclosed is a cryogenic rectification device and method in a process argon recovery system. The cryogenic rectification device mainly comprises a cryogenic heat exchanger, a cryogenic rectification column, a rectification column bottom evaporator and a rectification column top condenser; an argon input flow passage, a product argon output flow passage and a rectification exhaust gas output flow passage are arranged in the cryogenic heat exchanger, wherein the argon input flow passage is connected to the rectification column bottom evaporator through a pipeline, the product argon output flow passage is connected to the cryogenic rectification column top through a connecting pipeline and the rectification exhaust gas output flow passage is connected to the rectification column top condenser through a pipeline; the cryogenic rectification method comprises the steps that compressed argon is cooled when entering the cryogenic heat exchanger, the cooled cryogenic argon enters the evaporator, condensed liquid argon enters the cryogenic rectification column top and is used as falling liquid of the rectification column top after mixing with backflow liquid argon from the condenser to conduct rectification in the rectification column with ascending gas generated in the evaporator; pure liquid argon is obtained at the bottom of the rectification column, enters the cryogenic rectification column top condenser after being throttled through a throttle valve, provides a cold source and evaporates after mixing with added liquid argon and therefore pure argon is obtained.

Description

Hypothermia distillation device and method in a kind of technique argon recovery systems
Technical field
The present invention relates to the hypothermia distillation device and method in technique argon recovery systems, especially by cryogenic rectification Method is by the light component such as hydrogen, nitrogen in crude argon（With respect to argon gas）Impurity carries out detached method, belongs to cryogenic air separation rectifying Technical field.
Background technology
Argon gas is the larger gas of another kind of content in air in addition to oxygen and nitrogen, obtains advantage of lower cost, together When it has excellent chemical inertness and physical property, inert atmosphere can be provided for various techniques, reach substitutional impurity gas, blow Sweep pressed powder, take away the purposes such as heat unnecessary in technique.
Although in air separation industries, argon gas cost is relatively low with respect to other inert gases, for large gas is needed Ask, it is obtained, and cost is still very big, if recycling for technique argon gas can be realized, reduces cost there will be very big Jing Ji benefit.Therefore there are the businesses and institutions of many research argon gas recovery technologies both at home and abroad, existing procucts put goods on the market and use.
In argon gas recovery technology, hypothermia distillation device is its important unit, and general process organization is using pressure Contracting air and（Or）Liquid nitrogen etc. provides Cooling and Heat Source, and normal pressure output argon gas, subsequent configuration argon gas compressor is compressed to pressure needed for user Power, its flowage structure is complicated, and equipment investment and energy consumption are all relatively large.
The content of the invention
It is an object of the invention to overcome the shortcomings of that prior art is present, there is provided a kind of improved, process organization is better than it His existing procedure, system cost is less than other flow processs with energy consumption, while the technique that recovery utilization rate is not less than other existing procedures Hypothermia distillation device and method in argon recovery systems.
A kind of low temperature essence of the purpose of the present invention by following technical solution completing, in technique argon recovery systems Distillation unit, it mainly includes cryogenic heat exchanger, low-temperature fractionating tower, rectifier bottoms evaporimeter, rectifying column evaporator overhead condenser；It is described Cryogenic heat exchanger in be provided with argon gas input duct, product argon gas delivery channel and rectifying flue gas output stream road, wherein argon Gas input duct is connected to rectifier bottoms evaporimeter by pipeline, and picks out pipeline in the rectifier bottoms evaporimeter, and this connects Go out the top that pipeline is connected to low-temperature fractionating tower, product argon gas delivery channel is connected to low-temperature fractionating tower tower by connecting line Top, and rectifying flue gas output stream road is connected to rectifying column evaporator overhead condenser by pipeline, separately arranges on the top of low-temperature fractionating tower There is input to supplement the external pipeline of liquid argon.
As preferred：Described low-temperature fractionating tower is single column structure, the rectifier bottoms evaporimeter and the rectifying column Cold and heat source is all argon gas itself in evaporator overhead condenser, does not introduce air, liquid nitrogen medium.
A kind of cryogenic rectification method of the hypothermia distillation device using in the technique argon recovery systems, described method It is：
The compressed argon is cooled into cryogenic heat exchanger, and the low temperature argon gas after cooling enters evaporimeter, there is provided thermal source is simultaneously certainly Body is condensed, and condensed liquid argon gas enters cryogenic rectification top of tower, after mixing with the liquid argon of condenser reflux, as rectifying column The lower descending liquid at top, the rising gas produced with evaporimeter carries out rectifying in rectifying column；Rectifier bottoms obtain pure liquid argon, warp knuckle The condenser entered at the top of low-temperature fractionating tower after stream valve throttling, after mixing with supplementary liquid argon, there is provided simultaneously itself evaporation is obtained low-temperature receiver Pure argon, pure argon enters cryogenic heat exchanger, to reclaim and enter user pipe as product gas after cold.
As preferred：Described rectifying column top gas are entered after condenser, mostly as the thermal source of condenser, there is provided Infinite reflux after heat and itself condensation mixes to rectifying column top with liquid argon gas；Small part discharges low temperature essence as rectifying waste gas Evaporate tower and reclaim cold into cryogenic heat exchanger, the rectifying waste gas after rewarming discharges hypothermia distillation device；
The argon gas is compressed argon before into technique, and impurities are the impurity that relative argon gas is light component.
The invention has the advantages that：
1）Process organization of the present invention is simple, only needs a low-temperature fractionating tower to coordinate with sump evaporator and evaporator overhead condenser, then matches somebody with somebody Transmission and recovery that a cryogenic heat exchanger realizes cold are put, just can complete to separate light component impurity, purify the purpose of argon gas；
2）In the present invention, product argon gas can be designed according to user's desirable pressure, with pressure can export, and be not required to configure argon gas compression Machine；
3）In the present invention, cold and heat source is all argon gas itself in evaporimeter and condenser, and other are situated between to be not required to introducing air, liquid nitrogen etc. Matter；
4）In the present invention, system cold is provided by liquid argon is supplemented, and to be supplemented and still can supply user as pure argon after liquid argon offer cold Use, do not consume argon gas amount；
5）In the present invention, argon gas recovery utilization rate is controlled by adjusting the tolerance of rectifying waste gas.
Description of the drawings
Fig. 1 is the hypothermia distillation device structure flow chart in technique argon recovery systems of the present invention.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention will be described in detail：Shown in Fig. 1, a kind of technique argon gas of the present invention is returned Hypothermia distillation device in receipts system, it mainly includes cryogenic heat exchanger 102, low-temperature fractionating tower 106, rectifier bottoms evaporimeter 104, rectifying column evaporator overhead condenser 109；The input duct of argon gas 101, product argon gas are provided with described cryogenic heat exchanger 102 113 delivery channels and the delivery channel of rectifying waste gas 114, the wherein input duct of argon gas 101 are connected to rectifying column by pipeline 103 Sump evaporator 104, and pipeline 105 is picked out in the rectifier bottoms evaporimeter 104, this picks out pipeline 105 and is connected to low temperature essence The top of tower 106 is evaporated, the delivery channel of product argon gas 113 is connected to the tower top of low-temperature fractionating tower 106 by connecting line 110, and smart Evaporate the delivery channel of waste gas 114 and rectifying column evaporator overhead condenser 109 is connected to by pipeline 111, separately on the top of low-temperature fractionating tower 106 It is provided with the external pipeline that input supplements liquid argon 112.
Described low-temperature fractionating tower 106 is single column structure, and cold and heat source is all in the evaporimeter 104 and the condenser 109 For argon gas itself, air, liquid nitrogen medium are not introduced.
A kind of cryogenic rectification method of the hypothermia distillation device using in the technique argon recovery systems, described method It is：
The compressed argon 101 is cooled into cryogenic heat exchanger 102, and the low temperature argon gas 103 after cooling enters evaporimeter 104, Thermal source and itself condensation are provided, condensed liquid argon gas 105 enters cryogenic rectification top of tower, the liquid with the backflow of condenser 109 After argon mixing, used as the lower descending liquid at the top of rectifying column, the rising gas produced with evaporimeter 104 carries out rectifying in rectifying column.Essence Evaporate tower bottom and obtain pure liquid argon 107, warp knuckle stream valve 108 enters the condenser 109 at the top of low-temperature fractionating tower 106 after throttling, with benefit After topping up argon 112 mixes, there is provided simultaneously itself evaporation obtains pure argon 110 to low-temperature receiver, and pure argon 110 enters cryogenic heat exchanger 102, returns Receive and enter user pipe as product gas 113 after cold.
Described rectifying column top gas are entered after condenser 109, mostly as the thermal source of condenser 109, there is provided heat Infinite reflux after amount and itself condensation mixes to rectifying column top with liquid argon gas 105；Small part is discharged low as rectifying waste gas 111 Warm rectifying column enters cryogenic heat exchanger and reclaims cold, and the rectifying waste gas 114 after rewarming discharges hypothermia distillation device；
The argon gas 101 is compressed argon before into technique, and impurities are the impurity that relative argon gas is light component.
During the present invention is according to the scheme practice illustrated by Fig. 1, there is one typical compressed argon stream, it contains 98% argon, 0.5% hydrogen, 1.5% nitrogen finally obtains the purity of product argon gas 113 more than or equal to 99.9995%, and argon gas recovery utilization rate surpasses Cross 90%.

Claims (4)

1. the hypothermia distillation device in a kind of technique argon recovery systems, it mainly includes cryogenic heat exchanger（102）, cryogenic rectification Tower（106）, rectifier bottoms evaporimeter（104）, rectifying column evaporator overhead condenser（109）；It is characterized in that described low-temperature heat exchange Device（102）In be provided with argon gas（101）Input duct, product argon gas（113）Delivery channel and rectifying waste gas（114）Output stream Road, wherein argon gas（101）Input duct is connected to rectifier bottoms evaporimeter by pipeline（104）, and in the rectifier bottoms Evaporimeter（104）Pipeline is picked out, this picks out pipeline and is connected to low-temperature fractionating tower（106）Top, product argon gas（113）Output stream Road is connected to low-temperature fractionating tower by connecting line（106）Tower top, and rectifying waste gas（114）Delivery channel is connected to by pipeline Rectifying column evaporator overhead condenser（109）, separately in low-temperature fractionating tower（106）Top be provided with input supplement liquid argon（112）It is external Pipeline.
2. the hypothermia distillation device in technique argon recovery systems according to claim 1, it is characterised in that described is low Warm rectifying column（106）For single column structure, the evaporimeter（104）With the condenser（109）Middle cold and heat source is all argon gas sheet Body, does not introduce air, liquid nitrogen medium.
3. the cryogenic rectification method of the hypothermia distillation device in technique argon recovery systems described in a kind of utilization claim 1 or 2, It is characterized in that described method is：
The compressed argon（101）Into cryogenic heat exchanger（102）It is cooled, the low temperature argon gas after cooling（103）Into evaporation Device（104）, there is provided thermal source and itself condensation, condensed liquid argon gas（105）Into cryogenic rectification top of tower, with condenser （109）After the liquid argon mixing of backflow, as the lower descending liquid at the top of rectifying column, with evaporimeter（104）The rising gas of generation is in rectifying Rectifying is carried out in tower, rectifier bottoms obtain pure liquid argon（107）, warp knuckle stream valve（108）Low-temperature fractionating tower is entered after throttling（106） The condenser at top（109）, with supplementary liquid argon（112）After mixing, there is provided simultaneously itself evaporation obtains pure argon to low-temperature receiver（110）, it is pure Argon gas（110）Into cryogenic heat exchanger（102）, reclaim after cold as product gas（113）Into user pipe.
4. the cryogenic rectification method in technique argon recovery systems according to claim 3, it is characterised in that described essence Evaporate top of tower gas and enter condenser（109）Afterwards, mostly as condenser（109）Thermal source, there is provided heat and itself condensation Afterwards infinite reflux is to rectifying column top and liquid argon gas（105）Mixing；Small part is used as rectifying waste gas（111）Discharge low-temperature fractionating tower Cold, the rectifying waste gas after rewarming are reclaimed into cryogenic heat exchanger（114）Discharge hypothermia distillation device；
The argon gas（101）It is compressed argon before into technique, impurities are the impurity that relative argon gas is light component.
CN201611184614.5A 2016-12-20 2016-12-20 Cryogenic rectification device and method in process argon recovery system Pending CN106642996A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110368709A (en) * 2019-07-05 2019-10-25 苏州市兴鲁空分设备科技发展有限公司 Argon device for recovering tail gas
WO2020025214A1 (en) * 2018-07-28 2020-02-06 Messer Group Gmbh Method for recycling argon

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Publication number Priority date Publication date Assignee Title
CA2034578A1 (en) * 1990-01-25 1991-07-26 Gerry Norman Gottier Dephlegmator process for the recovery of helium
RU2117887C1 (en) * 1996-07-30 1998-08-20 Будневич Семен Самойлович Method of obtaining ultra-pure oxygen
CN101231131A (en) * 2007-01-23 2008-07-30 气体产品与化学公司 Purification of carbon dioxide
CN102425917A (en) * 2011-08-30 2012-04-25 杭州杭氧股份有限公司 Multifunctional rectifying tower
CN103759501A (en) * 2014-01-16 2014-04-30 上海交通大学 Low-temperature rectification device for production of ultra-pure xenon
US20140165649A1 (en) * 2012-12-18 2014-06-19 Air Liquide Process & Construction, Inc. Purification of inert gases to remove trace impurities
US20140165648A1 (en) * 2012-12-18 2014-06-19 Air Liquide Process & Construction, Inc. Purification of inert gases to remove trace impurities
CN106123487A (en) * 2016-07-04 2016-11-16 李琦 A kind of devices and methods therefor being produced pure neon by ne-He mixture
CN206862008U (en) * 2016-12-20 2018-01-09 杭州杭氧股份有限公司 A kind of hypothermia distillation device in technique argon recovery systems

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2034578A1 (en) * 1990-01-25 1991-07-26 Gerry Norman Gottier Dephlegmator process for the recovery of helium
RU2117887C1 (en) * 1996-07-30 1998-08-20 Будневич Семен Самойлович Method of obtaining ultra-pure oxygen
CN101231131A (en) * 2007-01-23 2008-07-30 气体产品与化学公司 Purification of carbon dioxide
CN102425917A (en) * 2011-08-30 2012-04-25 杭州杭氧股份有限公司 Multifunctional rectifying tower
US20140165649A1 (en) * 2012-12-18 2014-06-19 Air Liquide Process & Construction, Inc. Purification of inert gases to remove trace impurities
US20140165648A1 (en) * 2012-12-18 2014-06-19 Air Liquide Process & Construction, Inc. Purification of inert gases to remove trace impurities
CN103759501A (en) * 2014-01-16 2014-04-30 上海交通大学 Low-temperature rectification device for production of ultra-pure xenon
CN106123487A (en) * 2016-07-04 2016-11-16 李琦 A kind of devices and methods therefor being produced pure neon by ne-He mixture
CN206862008U (en) * 2016-12-20 2018-01-09 杭州杭氧股份有限公司 A kind of hypothermia distillation device in technique argon recovery systems

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020025214A1 (en) * 2018-07-28 2020-02-06 Messer Group Gmbh Method for recycling argon
US20210310733A1 (en) * 2018-07-28 2021-10-07 Messer Group Gmbh Method for recycling argon
CN110368709A (en) * 2019-07-05 2019-10-25 苏州市兴鲁空分设备科技发展有限公司 Argon device for recovering tail gas

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Application publication date: 20170510