CN107311122A - A kind of iron and steel metallurgical industry high throughput nitrogen purifier and method - Google Patents

A kind of iron and steel metallurgical industry high throughput nitrogen purifier and method Download PDF

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Publication number
CN107311122A
CN107311122A CN201710615022.2A CN201710615022A CN107311122A CN 107311122 A CN107311122 A CN 107311122A CN 201710615022 A CN201710615022 A CN 201710615022A CN 107311122 A CN107311122 A CN 107311122A
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China
Prior art keywords
deoxidation
drier
regeneration
hydrogen
gas
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CN201710615022.2A
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Chinese (zh)
Inventor
乐昀
朱玉秋
赵霖
高嵩
邱长春
刘皖南
郑晨达
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Dalian Zhong Ding Chemical Co Ltd
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Dalian Zhong Ding Chemical Co Ltd
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Priority to CN201710615022.2A priority Critical patent/CN107311122A/en
Publication of CN107311122A publication Critical patent/CN107311122A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/04Purification or separation of nitrogen
    • C01B21/0405Purification or separation processes
    • C01B21/0411Chemical processing only
    • C01B21/0416Chemical processing only by oxidation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/04Purification or separation of nitrogen
    • C01B21/0405Purification or separation processes
    • C01B21/0433Physical processing only
    • C01B21/045Physical processing only by adsorption in solids
    • 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
    • C01B2210/0003Chemical processing
    • C01B2210/0004Chemical processing by oxidation
    • 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
    • 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
    • C01B2210/0043Impurity removed
    • C01B2210/0045Oxygen
    • 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
    • C01B2210/0043Impurity removed
    • C01B2210/0051Carbon dioxide
    • 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
    • C01B2210/0043Impurity removed
    • C01B2210/0062Water

Abstract

The present invention relates to fields such as the extensive cold rolling, silicon steel of domestic iron and steel metallurgical industry, galvanized wire productions, a kind of iron and steel metallurgical industry high throughput nitrogen purifier and method are specifically related to.Main technical schemes are as follows:Including mechanical device and control system;Described mechanical device includes unstripped gas entrance, moisture trap, import trace oxygen analyzer, mass flow controller, program-controlled valve, catalytic deoxidation device, deoxidation drier, valve water cooler, product gas outlet, the hydrogen inlet of connection;Described deoxidation drier is two or more.The present invention is exceeded to hydrogen content in nitrogen to be controlled, while by remaining impurity O2、H2O、CO2Even depth is removed, and is solved gaseous impurity influence steel industry product quality stability, is caused the problem of product qualities such as cold-rolled steel sheet, galvanized steel plain sheet decline.

Description

A kind of iron and steel metallurgical industry high throughput nitrogen purifier and method
Technical field
The invention belongs to the fields such as the extensive cold rolling, silicon steel of domestic iron and steel metallurgical industry, galvanized wire production, and in particular to steel The production of iron metallurgy industry with terms of protection gas, more specifically for a kind of iron and steel metallurgical industry high throughput nitrogen purifier and Method.
Background technology
At present, steel production in China is front end hydrogenation deoxidation using a kind of most common technology with nitrogen purification, and rear end is done Dry dehydration.A certain amount of reaction water can be produced in technique deoxidation process, simultaneously because used hydrogen to operate during catalytic deoxidation, Deoxidation effect places one's entire reliance upon the amounts of hydrogen of addition, therefore hydrogenation must be excessive, thus cause hydrogen content in product nitrogen gas serious Exceeded, directly discharge can produce potential safety hazard and very big harm is caused to environment;Particularly excessive hydrogen is cold rolling in steel The danger of blast can be brought in continuous annealing furnace, therefore traditional handicraft can not meet the production such as cold rolling domestic steel, silicon steel, galvanized wire Demand.
The content of the invention
To make up the deficiencies in the prior art, the present invention provide a kind of iron and steel metallurgical industry high throughput nitrogen purifier and Method, it is exceeded to hydrogen content in nitrogen to be controlled, while by remaining impurity O2、H2O、CO2Even depth is removed, and solves gas Body impurity effect steel industry product quality stability, causes the problem of product qualities such as cold-rolled steel sheet, galvanized steel plain sheet decline.
Technical scheme is as follows:A kind of iron and steel metallurgical industry high throughput nitrogen purifier, including machinery dress Put and control system;
Unstripped gas entrance of the described mechanical device including connection, import trace oxygen analyzer, mass flow controller, journey Control valve, catalytic deoxidation device, deoxidation drier, valve water cooler, product gas outlet, hydrogen inlet;Described deoxidation is dried Device is two or more;
Heating system and oxidation catalyst are provided with described catalytic deoxidation device;
Temperature sensor, electric heater, heat accumulation mechanism are provided with described deoxidation drier;
Described control system includes central control unit and the flowmeter being connected respectively with central control unit, journey Control valve, A.C. contactor, pressure sensor, heating element, warning device.
Further, described catalytic deoxidation device is also connected with steam heater, water cooler, moisture trap.
Further, described deoxidation drier is 3 or 4.
Further, described deoxidation drier is 4, and two deoxidation driers are one group, and two groups of circulations are used as deoxidation Reactor and regeneration reactor are used.
The present invention simultaneously be claimed using described device carry out nitrogen purification method, including catalytic hydrogenation process, do Dry deoxidation step, step for regeneration;
Described catalytic hydrogenation process is:Unstripped gas passes through unstripped gas entrance, import trace oxygen analyzer, mass flow control Device processed enters catalytic deoxidation device, the oxygen in catalytic deoxidation device in the presence of oxidation catalyst in unstripped gas and the hydrogen being passed through Generation water is removed;
Described drying deoxidation step is:Unstripped gas after cooling enters deoxidation drier, in the presence of deoxidier Unstripped gas includes O2、H2O、CO2Impurity is adsorbed;Described deoxidation drier is more than 2, and circulation is used as deoxygenation Device and regeneration reactor, described deoxidation drier connect regeneration gas entrance by program-controlled valve;
Described step for regeneration is:Deoxidier in deoxidation drier in a heated condition, in the way of being passed through regeneration gas Regenerated, described deoxidier can be commercially available any one, preferably disclosed in Application No. 201410407743.0 Deoxidier.
Further, described regeneration gas is nitrogen, the mixture of hydrogen.
Further, the amount for being passed through hydrogen is obtained by below equation calculating:
VH=VN×([O]N/106)×2×δ;
VH:Added hydrogen (L/min);
VN:Nitrogen flow (L/min);
[O]N:Raw material oxygen content (ppm);
δ:It is hydrogenated with coefficient.
Hydrogen content of the control system meeting according to the catalytic deoxidation reactor outlet detected, automatic fine tuning hydrogenation coefficient.Root According to hydrogen content value in the unstripped gas detected after catalytic hydrogenation process, one group of hydrogen content value being previously written in contrast program and Coefficient is hydrogenated with, adjustment hydrogenation coefficient ensures that the hydrogen added is not excessive in real time, it is to avoid the blast wind brought because hydrogen is excessive Danger.
Hydrogenation amount is controlled:Hydrogen quality flow of the mass flow controller to detect is opened as foundation by automatic fine tuning valve Degree, the amounts of hydrogen that control is added is equal to theoretical hydrogenation amount.
Beneficial effects of the present invention are as follows:
(1) present invention provides a kind of iron and steel metallurgical industry high throughput nitrogen purifier and method, to hydrogen in nitrogen Content overproof is controlled, and by remaining impurity O2、H2O、CO2Even depth is removed, and solves gaseous impurity influence steel industry production Quality stability, causes the problem of product qualities such as cold-rolled steel sheet, galvanized steel plain sheet decline, while can also solve hydrogen in nitrogen The potential safety hazard that content overproof is brought, and this hidden danger is fundamentally prevented.Purification system dry deoxidation step using two towers, Three towers or four towers purifying flow, the multiple alternations of deoxidation drier and regeneration, so that the continuous purification to unstripped gas can be realized.
(2) deoxidier absorption and regeneration of the present invention have the characteristics that:Regeneration temperature is higher, regeneration pressure is lower, regeneration Effect is better, so that aerogenesis index is better.Traditional lossless regeneration, regeneration with pressure, regeneration effect are carried out using unstripped gas It is relatively poor, it is impossible to preferably to play the performance of deoxidier, improve aerogenesis purity;Traditional external heat form, it is necessary to use gas Carry heat to heat filler, regeneration gas flow is at least 15~25%.Power and gas waste are big, cause unnecessary wave Take, and filler can not be heated to higher temperature.Interior electric heater is respectively mounted in every deoxidation drier of the present invention. Compared with traditional lossless regeneration and external heating mode, while ensure that purification depth, consume energy less, regenerate tolerance Save;Using interior heat form, deoxidier is directly heated, regeneration temperature is high, and the energy is not wasted;Being passed through the gas of regeneration need to only play Heat balance and the water for producing regeneration carry out reactor, and regeneration tolerance is saved.
Brief description of the drawings
Fig. 1 is the structural representation of embodiment 1;
Wherein:11st, catalytic deoxidation device, 12, deoxidation drier A, 13, deoxidation drier B, 14, valve water cooler A, 15, Valve water cooler B, 16, hydrogen inlet, 17, unstripped gas entrance, 18, cooling water inlet, 19, instrument supply gas entrance, 100, cooling Backwater, 110, Waste gas outlet, 120, product gas outlet.
Fig. 2 is the structural representation of embodiment 2;
Wherein:201st, catalytic deoxidation device, 202, deoxidation drier A, 203, deoxidation drier B, 204, deoxidation drier C, 205th, hydrogen flowmeter is regenerated, 206, regeneration gas flow, 207, valve water cooler A, 208, valve water cooler B, 209, valve Door water cooler C, 210, servo gas entrance, 211, coolant outlet, 212, unstripped gas entrance, 213, product gas outlet, 214, Analyze gas outlet, 215, hydrogen inlet, 216, cooling water inlet.
Fig. 3 is the structural representation of embodiment 3;
Wherein:301st, steam heater, 302, catalytic deoxidation device, 303, water cooler, 304, moisture trap, 305, de- Oxygen drier A, 306, deoxidation drier B, 307, deoxidation drier C, 308, deoxidation drier D, 309, valve water cooler A, 310th, valve water cooler B, 311, product gas outlet, 312, the outlet of analysis gas, 313, hydrogen inlet, 314, low-pressure steam enters Mouthful, 315, unstripped gas entrance, 316, cooling water inlet, 317, Waste gas outlet, 318, cooling backwater outlet, 319, condensed water goes out Mouthful.
Embodiment
The present invention will be further described by 1-3 below in conjunction with the accompanying drawings:
The purification process of the present invention is by catalytic hydrogenation process (H) and two towers (W), three towers (VV) or four tower deoxidation drying processes (VW) process is constituted.Raw nitrogen gas initially enters catalytic hydrogenation process, in the presence of hydrogenation catalyst, by the O in gas2It is miscellaneous Matter is acted on hydrogen, is converted into H2O and remove;Subsequently into the O in deoxidation drying process deep removal gas2、H2O、CO2Deng Impurity.Deoxidation drying process has certain capacity using the deoxidier imurity-removal used, and saturation is reached when deoxidier absorbs impurity Afterwards, nitrogen and hydrogen mixture being passed through at high temperature, activating and regenerating is carried out to it.Dry deoxidation step according to purification nitrogen flow not Flow is purified with Liang Ta, three towers or four towers can be respectively adopted.Two-tower process is generally used for gas flow less than 5000Nm3/ h's Operating mode, one of deoxidation drier work (absorption impurity) in two-tower process, another deoxidation drier is then regenerated (or pressurize is stand-by), two such deoxidation drier alternation and regeneration, so that the continuous purification to raw nitrogen gas can be realized; Three-column process flow is generally used for gas flow more than 5000Nm3/ h and less than 10000Nm3/ h operating mode, is used in three-column process flow Cascade towers purify (absorption impurity), the technique of another tower activating and regenerating, and the technique can be solved under big flow or oxygen in unstripped gas Content fluctuates the problem that gas index is fluctuated under more frequent operating mode;Four-column process flow is generally used for gas flow and is more than 10000Nm3/ h operating mode, in four-column process flow, is divided into two groups of purifying columns, every group of cascade towers are used, one group of tower work purification, Another group of tower activating and regenerating, continuous uninterrupted purification gas and regeneration, every kind of flow are specifically divided into following steps:
1) catalytic hydrogenation process is main by catalytic deoxidation device, mass flow controller, flowmeter, trace oxygen analyzer, journey The equipment such as valve composition is controlled, catalytic deoxidation device apparatus with catalyst inside is main processing apparatus, and its impurity removal mechanism of catalyst is: H2Reacted in the presence of catalyst with the oxygen in gas and obtain conversion removing:
cat/Pd
Catalytic deoxidation:H2+O2——→H2O
Chemical deoxidation:AO+O2——→AO2
(" cat/ " acute pyogenic infection of finger tip noble metal catalyst.)
By the nitrogen of catalyst, O therein2Below 1ppm is removed to Deng impurity;
2) after catalytic process steps, raw nitrogen gas, which enters, dries deoxidation step.Application No. is used in this process 201410407743.0 disclosed in deoxidier, impurity removal depth is high, and anti-fluctuation ability is strong;The integrated internal heater of reactor, Programming rate is fast, built-in heat accumulation mechanism, short time power-off, and aerogenesis index is not influenceed.Process is by deoxidation absorber, valve group (oneself Dynamic equipment uses gas opening ball valve), the composition such as the flowmeter instrument of regeneration Gas Cooler and correlation.
Deoxidier of the oxygen at normal temperatures with reduction-state in the built-in deoxidation adsorbent of deoxidation drier, gas reacts And removed:Deoxidation:O2+AO——AO2
Deoxidier adsorbing contaminant has certain capacity, after deoxidier adsorption saturation, can heat logical hydrogen and it is regenerated.
Regeneration:AO2+H2——AO+H2O
This process uses deoxidier to possess oxygen gas and water and CO in deep removal nitrogen2Function, after adsorption saturation It is renewable, recover adsorption activity.
Deoxidation drier alternately works and regenerates to realize the continuous purification to raw nitrogen gas.So as to ensure using enterprise Continuous, the uninterrupted production of industry.
3) whole system using Siemens companies S7 series of PLC 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.Can be achieved remote monitoring or access client central control system (INTERNET or MODBUS), and dual control platform can be realized.
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 that the temperature to each reactor is controlled.With adding The reactor of hot merit energy has 3 temperature controls, and usual any of which a little reaches that the alarm of setting or interlocking temperature can all send report Alert or interlocking.Control system can the abnormal conditions such as real temperature of reactor, pressure, flow, condensate water cutoff when alarm and root Automatic interlock etc. is carried out according to situation.
Alarm explanation:The feedback signal obtained as PLC is abnormal, and is continued above the time of set alarming value and 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 alarm.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, will not interrupt aerogenesis, but regeneration step etc. will stop.
Above automatic control schemes reliably ensure that the safety of filler regeneration effect and whole system.
1 liang of tower absorption of embodiment
As shown in figure 1, raw nitrogen gas is by unstripped gas entrance 17, inlet valve, flowmeter metering and inlet gas analysis Enter catalytic deoxidation device 11 after instrument detection, oxygen controls what is added with being calculated by program precision in catalytic deoxidation device 11 Hydrogen is mixed, under normal temperature condition, and converting the oxygen to water by the catalytic action of catalyst removes, then enters by outlet valve Enter deoxidation drier A12, remnants O is removed in the presence of deoxidier2、H2O、CO2Deng impurity, when deoxidation drier A12 conducts When reactor works, deoxidation drier B13 is regenerated.Every deoxidation absorber undergoes identical step procedure.Control hydrogenation Process can ensure that the hydrogen of addition can meet deoxidation requirement, and not excessive a large amount of hydrogenation.
The calculating of hydrogenation amount:By the raw gas flow and raw material oxygen content detected, control is calculated by below equation Go out theoretical hydrogenation amount:
VH=VN×([O]N/106)×2×δ
VH:Added hydrogen (L/min or Nm3/h)
VN:Nitrogen flow (L/min or Nm3/h)
[O]N:Raw material oxygen content (ppm)
δ:It is hydrogenated with coefficient
The hydrogen content that control system can be exported according to the catalytic deoxidation device detected, automatic fine tuning hydrogenation coefficient:Contrast is urged Change hydrogen content value and the one group of hydrogen content value and hydrogenation coefficient that are previously written in program in the unstripped gas detected after reaction, in real time Adjustment hydrogenation coefficient ensures that the hydrogen added is not excessive, it is to avoid the risk of explosion brought due to excess hydrogen.
Hydrogenation amount is controlled:Hydrogen quality flow controller, the hydrogen quality flow using detection passes through automatic fine tuning as foundation Valve opening, the amounts of hydrogen that control is added is equal to theoretical hydrogenation amount.
Illustrate the course of work of every absorber by taking deoxidation drier A12 as an example below
Following steps fully automatic operation under PLC control, the temperature of all heating, the time of each sequential can be carried out Setting:
1) (A) is adsorbed
Unstripped gas is from bottom to top by deoxidation drier, the adsorbed separation of oxygen, carbon dioxide, water in unstripped gas.Absorption The time of work is the work period, and the work period can be set according to device parameter, and is needed in real work according to reality Border situation is adjusted.
Pressure process:Operating pressure.
Process temperature:Normal temperature.
Step performs the time:Half period
2) switch
After the deoxidation drier A12 absorption aerogenesis times that work switching time is reached, tower is cut to standby deoxidation drier B13 Work, the absorber of power cut-off is regenerated.Handover operation procedure declaration is as follows:
Cut tower (operation):2 minutes
Confirm standby 3 temperature (TIC1/2/3) of deoxidation drier B13 < switching permissive temperatures (60 DEG C), PLC is sent Standby deoxidation drier B13 entrances, outlet valve signal are opened, confirms to open according to writing in reply, the deoxidation for closing power cut-off is done Dry device A12 entrance and exit valves.
Such as standby 3 temperature (TIC1/2/3) of deoxidation drier B13 have any point > to switch permissive temperature (60 DEG C), then Do not switch, 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 switching sequence suspends, C towers continue to keep heated condition, and send alarm signal.After failture evacuation, pause manually is returned Continue to run with, still first determine whether whether valve letter in reply position is correct, and correct sequential is continued executing with.
The deoxidation drier of power cut-off then enters regeneration stage.Regeneration step it is general by release, regenerate, blow cold, pressurising Etc. several steps composition, total time is about 24~36 hours (each time of regeneration can set).After adsorber regeneration is finished, protect Pressure is stand-by, when another deoxidation drier power cut-off, switches to carry out Feedstock treating.
Illustrate regeneration step by taking deoxidation drier A12 as an example below:
Pressure process:Operating pressure.
Process temperature:Normal temperature.
Step performs the time:2 minutes.
3) release (A)
Confirm that regeneration deoxidation drier A12 enters, outlet valve is write in reply and is shown as closing, open regenerative adsorption device regeneration vent Valve, is slowly unloaded by the bypass pipe of release flow-limiting valve and is depressed into normal pressure, to avoid the big ups and downs of deoxidation drier A12 pressure from influenceing filler Life-span, the execution time reached after the step execution time, confirms that (standard setting is absorber pressure < regeneration authouized pressure Regeneration step is performed after 0.1Mpa).Such as not < regeneration pressures, then continue release, postpone and perform next step, until regeneration deoxidation is done Dry device A12 pressure < regeneration pressures.
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 20min.
4) regenerate
The electric heater for opening regeneration deoxidation drier A12 is heated to it, is determined while opening regeneration nitrogen valve and extracting Product nitrogen gas is measured, the hydrogen that regenerated hydrogen air valve is incorporated determination amount is opened, regenerative adsorption device regeneration gas inlet valve is opened, opens and unload Pressure flow-limiting valve, regenerative adsorption device regeneration gas outlet valve are passed through regeneration nitrogen, hydrogen and deoxidation drier A12 are regenerated.Use hand Dynamic valve regulation regeneration nitrogen, hydrogen flowing quantity to metered flow.
The water of deoxidier generation and the water and CO that desorb during regeneration2It is reproduced gas and carries out deoxidation drier A12, then emptying after cooler cooling is protected by valve.
Pressure process:Normal pressure.
Regeneration temperature:Control as 260 DEG C.
Step performs the time:About 16hr.
5) purging cooling (B → A)
After deoxidier regeneration is finished, stop heating.Regeneration hydrogen inlet valve is closed, stops adding regeneration hydrogen, continues Deoxidation drier A12 is purged with regeneration gas, after Step Time terminates, deoxidation drier A12 3 temperature are confirmed (TICA1/2/3) temperature is below switching permissive temperature (60 DEG C), performs next step;As the verification step time terminates deoxidation drying The temperature that device A12 3 temperature (TICA1/2/3) have any point is more than 60 DEG C, then continues to purge, and postpones execution next step straight It is below starting to perform next step after 60 DEG C to 3 temperature (TICA1/2/3) temperature for confirming deoxidation drier A12.
Pressure process:Normal pressure.
Process temperature:From 260 DEG C to normal temperature.
Step performs the time:About 14hr.
6) pressurising:
Operating pressure is boosted to deoxidation drier A12 with product gas after regeneration ending, to avoid pressure oscillation during switching Excessive influence sorbent life.
Deoxidation drier A12 regeneration vents valve, release flow-limiting valve are closed, is boosted with product gas to its deoxidation drier A12,
Pressure process:Normal pressure is to operating pressure.
Process temperature:Normal temperature;
Step performs the time:About 20min.
7) it is standby:
Pressure rising time closes regeneration nitrogen valve, regenerative adsorption device regeneration gas inlet valve after terminating.Into pressurize standby step. So far deoxidation drier A12 completes a working cycles, and then the absorber is in pressurize dormant state, waits the half period Terminate.Begin preparing for carrying out next circulation.
Pressure process:Normal pressure is to operating pressure.
Process temperature:Normal temperature;
Step performs the time:Terminate to the work deoxidation drier work period
To sum up, the ultra-pure nitrogen purifying system of high throughput is realized to raw nitrogen gas by robot control system(RCS) Automatic Control Purifying.
The tower of embodiment 2 three is adsorbed
As shown in Fig. 2 raw nitrogen gas is by unstripped gas entrance 212, inlet valve, flowmeter metering and inlet gas analysis Enter catalytic deoxidation device 201 after instrument detection, oxygen controls to add with calculating by program precision in catalytic deoxidation device 201 Hydrogen mixing, under normal temperature condition, water is converted the oxygen to by the catalytic action of catalyst and removed, then by gas-water separation Device, deoxidation drier A202, deoxidation drier B203 are sequentially entered by outlet valve remnants are removed in the presence of deoxidier O2、H2O、CO2Deng impurity, when connect two tower deoxidation drier A202, deoxidation drier B203 work as reactor, take off Oxygen drier C204 is regenerated.Every deoxidation absorber undergoes identical step procedure.Three deoxidation driers are alternately Work and regenerate to realize the continuous purification to raw nitrogen gas.So as to ensure continuous, the uninterrupted production using enterprise.
The amount and control method be the same as Example 1 of hydrogen are passed through, three tower work schedules see the table below 1, and (A, B, C distinguish in table 1 below Represent deoxidation drier A202, deoxidation drier B203, deoxidation drier C204):
Table 1
Deoxidation drier A12 in the course of work be the same as Example 1 of every deoxidation drier in the present embodiment.
The tower of embodiment 3 four is adsorbed
As shown in figure 3, raw nitrogen gas is by unstripped gas entrance 315, inlet valve, flowmeter metering and inlet gas analysis Enter catalytic deoxidation device 302 after instrument detection, oxygen controls to add with calculating by program precision in catalytic deoxidation device 302 Hydrogen mixing, under normal temperature condition, water is converted the oxygen to by the catalytic action of catalyst and removed, then by gas-water separation Device, deoxidation drier A305, deoxidation drier B306 are sequentially entered by outlet valve remnants are removed in the presence of deoxidier O2、H2O、CO2Deng impurity, when connect two tower deoxidation drier A305, deoxidation drier B306 work as reactor, take off Oxygen drier C307 and deoxidation drier D308 are regenerated.Every deoxidation absorber undergoes identical step procedure.Four take off Oxygen drier is divided into two groups, and two groups alternately work and regenerate to realize the continuous purification to raw nitrogen gas.So as to ensure to make With continuous, the uninterrupted production of enterprise.In winter operation, first pass through steam heater 301 and preheated again to unstripped gas Into catalytic deoxidation device 302, after catalytic deoxidation, deoxidation drier is entered after water cooled but device 303, moisture trap 304 A305 and deoxidation drier B306.
The amount and control method be the same as Example 1 of hydrogen are passed through, four tower work schedules see the table below 2 (A, B, C, D points in table 2 below Deoxidation drier A305, deoxidation drier B306, deoxidation drier C307, deoxidation drier D308 are not represented):
Table 2
Deoxidation drier A12 in the course of work be the same as Example 1 of every deoxidation drier in the present embodiment.

Claims (7)

1. a kind of iron and steel metallurgical industry high throughput nitrogen purifier, it is characterised in that:Including mechanical device and control system;
Described mechanical device includes unstripped gas entrance, import trace oxygen analyzer, mass flow controller, the sequencing valve of connection Door, catalytic deoxidation device, deoxidation drier, valve water cooler, product gas outlet, hydrogen inlet;Described deoxidation drier is Two or more;
Heating system and oxidation catalyst are provided with described catalytic deoxidation device;
Temperature sensor, electric heater, heat accumulation mechanism are provided with described deoxidation drier;
Described control system includes central control unit and the flowmeter, the sequencing valve that are connected respectively with central control unit Door, A.C. contactor, pressure sensor, heating element, warning device.
2. a kind of iron and steel metallurgical industry high throughput nitrogen purifier as claimed in claim 1, it is characterised in that:Described Catalytic deoxidation device is also connected with steam heater, water cooler, moisture trap.
3. a kind of iron and steel metallurgical industry high throughput nitrogen purifier as claimed in claim 1, it is characterised in that:Described Deoxidation drier is 3 or 4.
4. a kind of iron and steel metallurgical industry high throughput nitrogen purifier as claimed in claim 1, it is characterised in that:Described Deoxidation drier is 4, and two deoxidation driers are one group, and two groups of circulations are used as deoxidation reactor and regeneration reactor.
5. a kind of method that nitrogen purification is carried out using device as claimed in claim 1, it is characterised in that:Including catalytic hydrogenation work Sequence, dry deoxidation step, step for regeneration;
Described catalytic hydrogenation process is:Unstripped gas passes through unstripped gas entrance, import trace oxygen analyzer, mass flow controller Into catalytic deoxidation device, oxygen in catalytic deoxidation device in the presence of oxidation catalyst in unstripped gas and the hydrogen being passed through are generated Water is removed;
Described drying deoxidation step is:Unstripped gas after cooling enters deoxidation drier, the unstripped gas in the presence of deoxidier Include O2、H2O、CO2Impurity is adsorbed;Described deoxidation drier is more than 2, and circulation is as deoxidation reactor and again Raw reactor, described deoxidation drier connects regeneration gas entrance by program-controlled valve;
Described step for regeneration is:Deoxidier in deoxidation drier in a heated condition, is carried out in the way of being passed through regeneration gas Regeneration.
6. the method purified as claimed in claim 5, it is characterised in that:Described regeneration gas is nitrogen, the mixture of hydrogen.
7. the method purified as claimed in claim 5, it is characterised in that:The amount for being passed through hydrogen is obtained by below equation calculating:
VH=VN×([O]N/106)×2×δ;
VH:Added hydrogen (L/min);
VN:Nitrogen flow (L/min);
[O]N:Raw material oxygen content (ppm);
δ:It is hydrogenated with coefficient.
CN201710615022.2A 2017-07-25 2017-07-25 A kind of iron and steel metallurgical industry high throughput nitrogen purifier and method Pending CN107311122A (en)

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CN109179346A (en) * 2018-10-15 2019-01-11 杭州博大净化设备有限公司 A kind of nitrogen purification equipment
CN110655174A (en) * 2019-10-25 2020-01-07 上海铱钶环保科技有限公司 Device and method for rotary injection of concentrated ozone water
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