CN107434243A - A kind of superelevation pure hydrogen, argon gas, helium purification process - Google Patents

A kind of superelevation pure hydrogen, argon gas, helium purification process Download PDF

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Publication number
CN107434243A
CN107434243A CN201710609233.5A CN201710609233A CN107434243A CN 107434243 A CN107434243 A CN 107434243A CN 201710609233 A CN201710609233 A CN 201710609233A CN 107434243 A CN107434243 A CN 107434243A
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gas
adsorption dehumifier
regeneration
breathing
air
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高嵩
计国栋
赵霖
刘皖南
谭丽燕
乐昀
邱长春
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Dalian Zhong Ding Chemical Co Ltd
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Dalian Zhong Ding Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/56Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00Noble gases; Compounds thereof
    • C01B23/001Purification or separation processes of noble gases
    • C01B23/0036Physical processing only
    • C01B23/0052Physical processing only by adsorption in solids
    • C01B23/0057Physical processing only by adsorption in solids characterised by the adsorbent
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00Noble gases; Compounds thereof
    • C01B23/001Purification or separation processes of noble gases
    • C01B23/0036Physical processing only
    • C01B23/0052Physical processing only by adsorption in solids
    • C01B23/0084Physical processing only by adsorption in solids in getters
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/042Purification by adsorption on solids
    • C01B2203/043Regenerative adsorption process in two or more beds, one for adsorption, the other for regeneration
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0009Physical processing
    • C01B2210/0014Physical processing by adsorption in solids
    • C01B2210/0015Physical processing by adsorption in solids characterised by the adsorbent
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0009Physical processing
    • C01B2210/0014Physical processing by adsorption in solids
    • C01B2210/0023Physical processing by adsorption in solids in getters
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/133Renewable energy sources, e.g. sunlight

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Drying Of Gases (AREA)
  • Separation Of Gases By Adsorption (AREA)

Abstract

The present invention relates to fields such as semiconductor, LED, photovoltaic solar productions, a kind of superelevation pure hydrogen, argon gas, helium purification process are specifically related to.Main technical schemes are as follows:Including drying deoxidation step, air-breathing process, step for regeneration;Three processes realize that described control system includes central control unit and the respectively flowmeter with central control unit, program-controlled valve group, A.C. contactor, pressure sensor, heating element by control system.The present invention to O in unstripped gas2、H2O、CO、CO2、N2、CH4, the abjection of the impurity depth such as TCH, solving gaseous impurity influences electronics industry production device, the problem of causing electronic component Quality Down.And then regenerated using two towers purifying flow, one of adsorption dehumifier work, another adsorption dehumifier, the alternation of two such adsorption dehumifier and regeneration, so as to which the continuous purification to unstripped gas can be realized.

Description

A kind of superelevation pure hydrogen, argon gas, helium purification process
Technical field
The invention belongs to the fields such as semiconductor, LED, photovoltaic solar production, and in particular to opto-electronic industry production is protected Gas is protected, is more specifically a kind of superelevation pure hydrogen, argon gas, helium purification process.
Background technology
At present, China's purifying hydrogen, argon helium are head-cat deoxidations using a kind of most common technology, and rear end is dried de- Water.Substantial amounts of reaction water can be produced in technique deoxidation process;And oxygen, water in hydrogen can only be removed, and for CO, CH4、 TCH、N2It can not then be removed Deng impurity, and these impurity have a major impact to the quality of production of electronic device, therefore existing purifying side Method can not meet domestic large scale integrated circuit production requirement.
The content of the invention
To make up the deficiencies in the prior art, the present invention provides a kind of superelevation pure hydrogen, argon gas, helium purification process, to original Expect O in gas2、H2O、CO、CO2、N2、CH4, the abjection of the impurity depth such as TCH, solving gaseous impurity influences electronics industry production device Part, the problem of causing electronic component Quality Down.
Technical scheme is as follows:A kind of superelevation pure hydrogen, argon gas, helium purification process, including dry deoxidation work Sequence, air-breathing process, step for regeneration;
Described drying deoxidation step is:Unstripped gas enters adsorption dehumifier by unstripped gas entrance, the O in unstripped gas2 Reacted with the reduction-state deoxidier in adsorption dehumifier, reduction-state deoxidier absorbs the H in unstripped gas simultaneously2O、CO2;Described Adsorption dehumifier includes adsorption dehumifier A, adsorption dehumifier B, and described adsorption dehumifier A, adsorption dehumifier B are circulated into promoting the circulation of qi Body adsorbs and regeneration, and is equipped with temperature sensor, electric heater, heat accumulation mechanism in adsorption dehumifier A, adsorption dehumifier B;
Described air-breathing process is:Heat exchanger is delivered to through outlet valve by the unstripped gas for drying deoxidation step, is exchanged heat Gas afterwards enters air-breathing reactor, getter effect under, will in gas comprising oxygen, carbon monoxide, methane, water, nitrogen, The impurity of carbon dioxide is removed, and the water cooled but device cooling of gas after purification is discharged through product gas outlet again;Described air-breathing is anti- Answer in device and be provided with heating tube;
Described step for regeneration is:Deoxidier in adsorption dehumifier A, adsorption dehumifier B in a heated condition, to be passed through The mode of regeneration gas is regenerated;
Described drying deoxidation step, air-breathing process, step for regeneration realized by control system, described control system bag Include central control unit and the respectively flowmeter with central control unit, program-controlled valve group, A.C. contactor, pressure sensing Device, heating element.
Further, described air-breathing reactor includes air-breathing reactor A, air-breathing reactor B, air-breathing reactor A and suction Solid/liquid/gas reactions device B carries out air-breathing reaction simultaneously.
Further, in described air-breathing process, under getter effect, oxygen, carbon monoxide, methane will be included in gas Impurity be converted into H2O and CO2And remove, the water, carbon dioxide, nitrogen in gas are absorbed by getter to be removed.
Further, in described drying deoxidation step:O in unstripped gas2At 25 DEG C -28 DEG C with adsorption dehumifier Reduction-state deoxidier reaction.
Further, described regeneration gas is nitrogen, hydrogen.
Further, described deoxidier can be commercially available any one, preferably Application No. 201410407743.0 Disclosed in deoxidier, described getter is metal getter, and described metal getter is made up of zirconium, vanadium and iron, wherein zirconium Account for 60%-75%, vanadium accounts for about 20%-25%, iron accounts for 3%-10%.
Beneficial effects of the present invention are as follows:The present invention to O in hydrogen, argon gas, helium2、H2O、CO、CO2、N2、CH4、TCH Deviate from Deng impurity depth, solving gaseous impurity influences electronics industry production device, the problem of causing electronic component Quality Down. Purification system is dried deoxidation step and worked (absorption impurity) using two towers purifying flow, one of adsorption dehumifier, another Adsorption dehumifier is then regenerated (or pressurize is stand-by), the alternation of two such adsorption dehumifier and regeneration, so as to realize To the continuous purification of unstripped gas.
Brief description of the drawings
Fig. 1 is the structural representation of the present invention;
Wherein:1st, adsorption dehumifier A, 2, adsorption dehumifier B, 3, air-breathing reactor A, 4, heat exchanger, 5, air-breathing reactor B, 6, unstripped gas entrance, 7, water cooler, 8, regeneration gas entrance, 9, cooling water inlet, 10, coolant outlet, 11, product gas goes out Mouth, 12, waste gas exhaust outlet, 13, flowmeter.
Embodiment
The present invention will be further described below in conjunction with the accompanying drawings:
As shown in figure 1, a kind of superelevation pure hydrogen, argon gas, helium purification process, including dry deoxidation step, air-breathing process, Step for regeneration;Described drying deoxidation step is:Unstripped gas enters adsorption dehumifier by unstripped gas entrance 6, in unstripped gas O2Reacted with the reduction-state deoxidier in adsorption dehumifier, reduction-state deoxidier absorbs the H in unstripped gas simultaneously2O、CO2;It is described Adsorption dehumifier include adsorption dehumifier A1, adsorption dehumifier B2, described adsorption dehumifier A1, adsorption dehumifier B2 circulation Gas absorption and regeneration are carried out, and temperature sensor, electric heater, storage are equipped with adsorption dehumifier A1, adsorption dehumifier B2 Heat engine structure;Described air-breathing process is:Heat exchanger 4 is delivered to through outlet valve by the unstripped gas for drying deoxidation step, is exchanged heat Gas afterwards enters air-breathing reactor, getter effect under, will in gas comprising oxygen, carbon monoxide, methane, water, nitrogen, The impurity of carbon dioxide removes, and the water cooled but device 7 of gas after purification cools down discharges through product gas outlet 11 again;Described air-breathing Heating tube is provided with reactor;Described step for regeneration is:Deoxidier in adsorption dehumifier A1, adsorption dehumifier B2 is heating Under the conditions of, regenerated in a manner of being passed through regeneration gas;Described drying deoxidation step, air-breathing process, step for regeneration pass through control System processed realizes that described control system includes central control unit and the respectively flowmeter 13 with central control unit, journey Control valve group, A.C. contactor, pressure sensor, heating element.Described air-breathing reactor includes air-breathing reactor A 3, air-breathing Reactor B 5, air-breathing reactor A 3 and air-breathing reactor B 5 carry out air-breathing reaction simultaneously.In described air-breathing process, in getter Under effect, the impurity comprising oxygen, carbon monoxide, methane in gas is converted into H2O and CO2And remove, water, dioxy in gas Change carbon, nitrogen is absorbed by getter and removed.In described drying deoxidation step:O in unstripped gas2At 25 DEG C -28 DEG C with suction Reduction-state deoxidier reaction in attached drier.Described regeneration gas is nitrogen, hydrogen.Described deoxidier is Application No. Deoxidier disclosed in 201410407743.0.Described getter is publication product, and described getter is inhaled for metal Gas agent, described metal getter are made up of zirconium, vanadium and iron, and wherein zirconium accounts for 60%-75%, vanadium accounts for about 20%-25%, iron accounts for 3%-10%.
The operation principle and procedure declaration of the purification system of the present invention are as follows:
Purifying process dries deoxidation step (W) by two towers and two processes of air-breathing process (X) form.Unstripped gas initially enters Deoxidation step is dried, in the presence of deoxidier, by the O in gas2、H2O、CO2Deng impurity;Subsequently into air-breathing process depth Remove the N in gas2、CH4, the impurity such as TCH (total hydrocarbon), and absorb O2、H2O、CO2.Deoxidation step is dried using de- Oxygen agent imurity-removal has certain capacity, after deoxidier, which absorbs impurity, reaches saturation, can be passed through nitrogen and hydrogen mixture and it is carried out again It is raw.Dry deoxidation step to work (absorption impurity) using two towers purifying flow, one of adsorption dehumifier, another absorption is dry Dry device is then regenerated (or pressurize is stand-by), the alternation of two such adsorption dehumifier and regeneration, so as to realize to raw material The continuous purification of gas.It is specifically divided into following steps:
1) unstripped gas, which enters, dries deoxidation step.Using de- disclosed in Application No. 201410407743.0 in this process Oxygen agent, impurity removal depth is high, and anti-fluctuation ability is strong;Adsorption dehumifier integrates internal heater, and programming rate is fast, built-in heat accumulation machine Structure, short time power-off, does not influence aerogenesis index.Process by adsorption dehumifier, valve group (automatic equipment drives diaphragm valve using gas), Regenerate the compositions such as the flowmeter instrument of Gas Cooler and correlation.
The built-in deoxidier of adsorption dehumifier, the oxygen in gas react and obtained with the deoxidier of reduction-state at normal temperatures Removing:Deoxidation:O2+AO—AO2
Deoxidier adsorbing contaminant has certain capacity, after deoxidier adsorption saturation, can heat logical nitrogen and hydrogen mixture and it is entered Row regeneration.
Regeneration:
This process uses deoxidier to be provided simultaneously with deep removal water and CO for the special product by modification2's Function, after adsorption saturation when deoxidier regenerates can synchronizing regeneration, recover adsorption activity.
Two adsorption dehumifiers alternately work and regenerated to realize the continuous purification to unstripped gas.So as to ensure to use Continuous, the uninterrupted production of enterprise.
2) the dried gas of deoxidation is passed through, into subsequent inspiration process.Deep removal CO, CO therein2、N2、CH4、 The impurity such as TCH are purified to ppb levels.Hydrogen, argon gas, helium after purification is delivered to point of use.
3) whole system uses the S7 series of PLC of Siemens companies as centralized control unit, using touch control screen pair Whole production process is implemented to be monitored and controlled.Possess automatic regeneration SECO (valve switch, temperature control), it is automatic, The functions such as manually operated, running state monitoring.Remote monitoring can be achieved or access the central control system (MODBUS) of client, and Dual control platform can be achieved.
4) the system temperature control is made up of PLC, solid-state relay, thermocouple, electric heater etc..Each reactor temperature of system Degree is detected by thermocouple and signal is transmitted into PLC, and PLC then according to the program and condition of setting prepared in advance, controls solid-state The break-make of relay current, to control the opening of electric heater, stop, so as to be controlled to the temperature of each reactor.With heating The reactor of function has 3 temperature controls, and usual any of which, which a little reaches the alarm of setting or interlocking temperature, can all send alarm Or interlocking.Control system can also be in the abnormal conditions such as temperature of reactor, pressure, flow, condensate water cutoff alarm and according to feelings Condition carries out automatic interlock etc..
Alarm explanation:The feedback signal obtained as PLC is abnormal, and the time for being continued above set alarming value exceedes Anti- ripple is delayed (avoiding fluctuation from causing false alarm), and device will send alarm signal.Alarm indication interface can be manually entered, according to carrying Show failure judgement point.All warning messages can be all recorded in alarm list.Device still keeps purifying aerogenesis state during alarm.
Interlock explanation:Interlocked operation is after alarm, or is simultaneously emitted by alarming.Part alarm signal is within the time of setting Do not handled, or signal is exceeded reaches set interlocking value, device will according to circumstances take corresponding interlocking side automatically Case, to avoid the generation of peril.Non- cross-line interlocking, aerogenesis will not be interrupted, but regeneration step etc. will stop.
Above automatic control schemes reliably ensure that the safety of filler regeneration effect and whole system.Below using purifying hydrogen as Example illustrates to the purifying detailed process of the present invention:
Raw hydrogen enters adsorption dehumifier A1 after inlet valve, flowmeter 13 by program-controlled valve, and depth abjection is former After the impurity such as oxygen, water, carbon dioxide in material gas, heat exchanger 4 is delivered to through outlet valve, it is anti-that the gas after heat exchange enters air-breathing Device 3 and air-breathing reactor 5 are answered, in the presence of temperature is 450-550 DEG C and getter, by the N in gas2、CO、CH4, TCH etc. Impurity, it is converted into H2O and CO2And remove, while absorb H2O、CO2、O2, it is sent to after the water cooled cooling of but device 7 of hydrogen after purification Point of use.When an adsorption dehumifier is in absorption aerogenesis step, then another adsorption dehumifier is then in the difference regenerated Step, every adsorption dehumifier undergo identical step procedure.
Illustrating the course of work of every adsorption dehumifier by taking adsorption dehumifier A1 as an example below, following (following steps exist Fully automatic operation under PLC control, the temperature of all heating, the time of each sequential can be set):
1) (A) is adsorbed
Unstripped gas is from bottom to top by adsorption dehumifier A1, the adsorbed separation of oxygen, carbon dioxide, water in unstripped gas.Inhale The time of attached work is the work period, and the work period can be set according to device parameter, and needs the basis in real work Actual conditions are adjusted.
Pressure process:Operating pressure.
Process temperature:Normal temperature.
Step performs the time:Half period
2) switch
After the adsorption dehumifier A1 absorption aerogenesis times switching time is reached, cut tower and work to standby adsorption dehumifier B2, The absorber of power cut-off is regenerated.Handover operation procedure declaration is as follows:
Cut tower (operation):2 minutes
When confirming that standby 3 temperature (TIC1/2/3) of adsorption dehumifier B2 are respectively less than switching permissive temperature (60 DEG C), PLC Send and open standby adsorption dehumifier B2 entrances and its outlet valve signal, confirm outlet valve opening-closing knot according to writing in reply The adsorption dehumifier A entrances and its outlet valve of beam work.
Switch permissive temperature (60 DEG C) as 3 temperature (TIC1/2/3) of adsorption dehumifier B2 have any point to be more than, then do not cut Change, and alarm.
Such as it is set as 30 seconds in defined valve alarm decision time internal standard, writes in reply and judge through valve, valve is not beaten Open, then (adsorption dehumifier A continues to keep heated condition, and sends alarm signal for switching sequence pause.After failture evacuation, manually Pause return continues to run with, and still first determines whether valve letter in reply position is correct, and correct sequential continues executing with).
The adsorption dehumifier of power cut-off then enters regeneration stage.Regeneration step typically by release, regenerate, blow cold, pressurising Formed etc. several steps, total time is about 24~36 hours (each time of regeneration can set).Adsorption dehumifier regeneration finishes Afterwards, pressurize is stand-by, when another absorber power cut-off, switches to carry out Feedstock treating.Below using adsorption dehumifier A1 as Example explanation regeneration step:
3) release (A)
Confirm that regenerative adsorption drier A1 inlet valves, outlet valve are write in reply and be shown as closing, open regenerative adsorption and dry Device A1 regeneration vent valves, are slowly unloaded by the bypass pipe of release flow-limiting valve and are depressed into normal pressure, to avoid adsorption dehumifier A1 pressure violent In the influence of fluctuations filler life-span, after the execution time reaches the step execution time, confirm that adsorption dehumifier A1 pressure is less than regeneration license Pressure (standard setting 0.1Mpa) performs next step (regeneration step) afterwards.Such as it is not less than regeneration pressure, then continues release, push away Next step is performed late, until regenerative adsorption drier A1 pressure is less than regeneration pressure.
Pressure process:Normal pressure (external atmosphere pressure at that time) is down to by operating pressure.
Process temperature:Normal temperature.
Step performs the time:About 30min.
4) regenerate
The electric heater opened in regenerative adsorption drier A1 heats to adsorption dehumifier A1, while opens regeneration air valve True basis weight products hydrogen is extracted, opens the nitrogen of regeneration air valve supplying determination amount, this time the amount of hydrogen and nitrogen is according to container Size determine, open regenerative adsorption device regeneration gas inlet valve, open release flow-limiting valve regenerative adsorption drier A1 regeneration gases and go out Valve is passed through regeneration nitrogen to mouth, hydrogen regenerates to adsorption dehumifier A1.With manual valve regulation regeneration nitrogen, hydrogen flowing quantity to volume Constant flow.
The water of deoxidier generation and the water and CO that desorb during regeneration2It is reproduced gas and carries out adsorption dehumifier A1, then be vented after protecting cooler cooling by valve.
Pressure process:Normal pressure.
Regeneration temperature:Control as 260 DEG C.
Step performs the time:About 16hr.
5) purging cooling
After deoxidier regenerates, stop heating.Regeneration hydrogen inlet valve is closed, stops adding regeneration hydrogen, continues Adsorption dehumifier A1 is purged with regeneration gas, after Step Time terminates, confirms adsorption dehumifier A1 3 temperature (TICA1/ 2/3) temperature is below switching permissive temperature (60 DEG C), next step is performed, as the verification step time terminates adsorption dehumifier A1 The temperature that 3 temperature (TICA1/2/3) have any point is more than 60 DEG C, then continues to purge, and postpones and performing in next step until confirming to inhale Attached drier A1 3 temperature (TICA1/2/3) temperature start to perform next step after being below 60 DEG C.
Pressure process:Normal pressure.
Process temperature:From 260 DEG C to normal temperature.
Step performs the time:About 12hr.
6) pressurising:
Boost to operating pressure to adsorption dehumifier A1 with product gas after regeneration ending, with avoid switching when pressure oscillation It is big to influence sorbent life.
Adsorption dehumifier A1 regeneration vents valve, release flow-limiting valve are closed, is boosted with product gas to adsorption dehumifier A1,
Pressure process:Normal pressure is to operating pressure.
Process temperature:Normal temperature;
Step performs the time:About 25min.
7) it is standby:
Pressure rising time closes regenerating valve, regenerative adsorption device regeneration gas inlet valve after terminating.Into pressurize standby step.Extremely This adsorption dehumifier A1 completes a working cycles, is then in pressurize dormant state, waits the half period to terminate.Start accurate It is standby to carry out next circulation.
Pressure process:Normal pressure is to operating pressure.
Process temperature:Normal temperature;
Step performs the time:Terminate to the work absorber work period.
To sum up, high throughput superelevation purification system realizes the purifying to unstripped gas by robot control system(RCS) Automatic Control.

Claims (5)

1. a kind of superelevation pure hydrogen, argon gas, helium purification process, it is characterised in that including dry deoxidation step, air-breathing process, Step for regeneration;
Described drying deoxidation step is:Unstripped gas enters adsorption dehumifier by unstripped gas entrance (6), the O in unstripped gas2With Reduction-state deoxidier reaction in adsorption dehumifier, reduction-state deoxidier absorb the H in unstripped gas simultaneously2O、CO2;Described suction Attached drier includes adsorption dehumifier A (1), adsorption dehumifier B (2), described adsorption dehumifier A (1), adsorption dehumifier B (2) Circulation carries out gas absorption and regeneration, and be equipped with adsorption dehumifier A (1), adsorption dehumifier B (2) temperature sensor, electricity plus Hot device, heat accumulation mechanism;
Described air-breathing process is:Heat exchanger (4) is delivered to through outlet valve by the unstripped gas for drying deoxidation step, after heat exchange Gas enter air-breathing reactor, getter effect under, will in gas comprising oxygen, carbon monoxide, methane, water, nitrogen, two The impurity of carbonoxide is removed, and water cooled but device (7) cooling of gas after purification is discharged through product gas outlet (11) again;Described suction Heating tube is provided with solid/liquid/gas reactions device;
Described step for regeneration is:Deoxidier in adsorption dehumifier A (1), adsorption dehumifier B (2) in a heated condition, with logical The mode for entering regeneration gas is regenerated;
Described drying deoxidation step, air-breathing process, step for regeneration are realized by control system, during described control system includes Centre control unit and the flowmeter (13) being connected respectively with central control unit, program-controlled valve group, A.C. contactor, pressure Sensor, heating element.
2. superelevation pure hydrogen as claimed in claim 1, argon gas, helium purification process, it is characterised in that described air-breathing reaction Device includes air-breathing reactor A (3), air-breathing reactor B (5).
3. superelevation pure hydrogen as claimed in claim 1, argon gas, helium purification process, it is characterised in that described air-breathing process In, under getter effect, the impurity comprising oxygen, carbon monoxide, methane in gas is converted into H2O and CO2And remove, gas In water, carbon dioxide, nitrogen by getter absorb remove.
4. superelevation pure hydrogen as claimed in claim 1, argon gas, helium purification process, it is characterised in that described drying deoxidation In process:O in unstripped gas2Reacted at 25 DEG C -28 DEG C with the reduction-state deoxidier in adsorption dehumifier.
5. superelevation pure hydrogen as claimed in claim 1, argon gas, helium purification process, it is characterised in that described regeneration gas is Nitrogen, hydrogen.
CN201710609233.5A 2017-07-25 2017-07-25 A kind of superelevation pure hydrogen, argon gas, helium purification process Pending CN107434243A (en)

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CN109911851A (en) * 2017-12-12 2019-06-21 中国科学院大连化学物理研究所 A kind of ultra-pure hydrogen purification process
CN110280206A (en) * 2019-08-05 2019-09-27 大连中鼎化学有限公司 A kind of multi-functional adsorbent and preparation method thereof, application
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CN110302631A (en) * 2019-07-18 2019-10-08 大连中鼎化学有限公司 The purification devices and its technique of a kind of argon gas that can replace adsorption column online, helium and hydrogen
CN110354633A (en) * 2019-07-18 2019-10-22 大连中鼎化学有限公司 A method of it is purified for hydrogen, argon gas and helium
CN110980647A (en) * 2019-12-25 2020-04-10 厦门市乐立润安科技有限公司 Hydrogen purification method suitable for liquefaction process
CN112902555A (en) * 2021-01-28 2021-06-04 武汉钢铁集团气体有限责任公司 Helium low-temperature purification method and device and helium refrigeration cycle system
WO2023071281A1 (en) * 2021-10-30 2023-05-04 无锡隆基氢能科技有限公司 System and method for purifying hydrogen, and system for producing hydrogen by means of water electrolysis

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103463975A (en) * 2013-09-27 2013-12-25 中国计量科学研究院 Reproducible zero air purifier
CN106145037A (en) * 2015-04-01 2016-11-23 大连中鼎化学有限公司 The device of hydrogen and the method for High Purity Hydrogen processed is reclaimed from silicon epitaxial furnace emptying end gas
CN106139890A (en) * 2015-04-01 2016-11-23 大连中鼎化学有限公司 Cold-rolled steel sheet heat treatment nitrogen hydrogen mixed tail gas reclaims the apparatus and method purifying

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103463975A (en) * 2013-09-27 2013-12-25 中国计量科学研究院 Reproducible zero air purifier
CN106145037A (en) * 2015-04-01 2016-11-23 大连中鼎化学有限公司 The device of hydrogen and the method for High Purity Hydrogen processed is reclaimed from silicon epitaxial furnace emptying end gas
CN106139890A (en) * 2015-04-01 2016-11-23 大连中鼎化学有限公司 Cold-rolled steel sheet heat treatment nitrogen hydrogen mixed tail gas reclaims the apparatus and method purifying

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
中国工业气体协会编: "《中国工业气体大全》", 31 May 2008, 大连理工大学出版社 *
刘建国等,: "《可再生能源导论》", 28 February 2017 *
赵殿礼等,: "《船舶电气设备管理与工艺》", 30 September 2004 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109911851A (en) * 2017-12-12 2019-06-21 中国科学院大连化学物理研究所 A kind of ultra-pure hydrogen purification process
CN109136500A (en) * 2018-10-31 2019-01-04 上海颐柏热处理设备有限公司 A kind of vacuum heat treatment furnace with chemical deoxidization system
CN109775671A (en) * 2019-03-18 2019-05-21 大连华邦化学有限公司 A kind of hyperpure gas purification system and technique based on room temperature absorbing process
CN109775671B (en) * 2019-03-18 2023-08-15 大连华邦化学有限公司 Ultra-pure gas purification system and process based on normal temperature adsorption process
CN110282608A (en) * 2019-07-18 2019-09-27 大连中鼎化学有限公司 A kind of purification devices and its technique for nitrogen, oxygen, argon gas and helium
CN110302631A (en) * 2019-07-18 2019-10-08 大连中鼎化学有限公司 The purification devices and its technique of a kind of argon gas that can replace adsorption column online, helium and hydrogen
CN110354633A (en) * 2019-07-18 2019-10-22 大连中鼎化学有限公司 A method of it is purified for hydrogen, argon gas and helium
CN110280206A (en) * 2019-08-05 2019-09-27 大连中鼎化学有限公司 A kind of multi-functional adsorbent and preparation method thereof, application
CN110980647A (en) * 2019-12-25 2020-04-10 厦门市乐立润安科技有限公司 Hydrogen purification method suitable for liquefaction process
CN112902555A (en) * 2021-01-28 2021-06-04 武汉钢铁集团气体有限责任公司 Helium low-temperature purification method and device and helium refrigeration cycle system
WO2023071281A1 (en) * 2021-10-30 2023-05-04 无锡隆基氢能科技有限公司 System and method for purifying hydrogen, and system for producing hydrogen by means of water electrolysis

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