CN102031480B - Ferrous sulfide gas-phase passivation method - Google Patents
Ferrous sulfide gas-phase passivation method Download PDFInfo
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Abstract
The invention discloses a ferrous sulfide gas-phase passivation method, comprising the steps of monitoring, feeding air, passivating, sealing and discharging, wherein the passivating is implemented as follows: vapor carrying oxygen enriched air enter a container for carrying out gas phase passivation on ferrous sulfide. The vapor is water vapor, the pressure of the water vapor is 0.1-0.9 Mpa, and the oxygen enriched air contains 21-50 percent of oxygen by volume. Compared with the ferrous sulfide liquid-phase passivation method, the ferrous sulfide gas-phase passivation method has low cost, is easy to implement, mainly adopts oxygen enriched air which is convenient to use and has low cost for gas phase passivation, ensures uniform ferrous sulfide passivation, is free from channeling phenomenon and dead corners due to gas-phase action and boasts of easy treatment of waste gas which is produced in ferrous sulfide gas-phase passivation and can reach the emission standard after being treated simply, and has short treatment time.
Description
Technical field
The present invention relates to a kind for the treatment of process technical field of metallic sulfide, particularly a kind of ferrous sulfide gas-phase passivation method of metallic surface.
Background technology
Iron sulfuret is that sulphur in oil and derived prods thereof is to the corrosion product of petrochemical equipment, often occur because the Iron sulfuret oxidation causes spontaneous combustion or explosion hazard in the Maintenance And Modification of Petrochemical Plants process, so must carry out passivation or the clean of Iron sulfuret before Maintenance And Modification of Petrochemical Plants.
At present, all adopt the method for liquid phase passivation for the treatment process of Iron sulfuret in petrochemical equipment, be about to that liquid phase passivator circulates and then the abundant reaction of realization and Iron sulfuret in device, thereby the oxide compound that makes Iron sulfuret be converted into more stable iron reaches the purpose of preventing the Iron sulfuret oxidation and spontaneous combustion.
The metallic surface is converted into and is difficult for oxidized state, and the method that delays corrosion of metal speed is called passivation.If metal is because the corrosion product of the effect generation of medium has fine and close structure, formed thin film (invisible often), closely cover metallic surface, changed the metallic surface state, make the electropotential of metal greatly to positive dirction transition, and become anti-corrosion passive state.During as Fe → Fe++, standard potential is-0.44V, jumps to after passivation+0.5～1V, and demonstrates corrosion resistant precious metal performance, and this layer film just is passive film.
The passivation of metal may be also spontaneous process (as generating the insoluble compound of one deck, i.e. oxide film at metallic surface).Industrial be with passivator (being mainly oxygenant), metal to be carried out Passivation Treatment, form layer protecting film.
Iron, aluminium are at rare HNO
3Or rare H
2SO
4In can dissolve very soon, but at dense HNO
3Or dense H
2SO
4Middle dissolution phenomena has almost completely stopped, and carbon steel is easy to get rusty usually, if add appropriate Ni, Cr in steel, has just become stainless steel.Metal or alloy is affected by some factors, and the phenomenon that chemical stability obviously strengthens is called passivation.By the caused metal passivation phenomenon of some passivator (pharmaceutical chemicals), be called chemical passivation.As dense HNO
3, dense H
2SO
4, HClO
3, K
2Cr
2O
7, KMnO
4All can make metal passivation in oxygenant.After metal passivation, its electrode potential moves to positive dirction, makes it lose original characteristic, as passivation iron copper can not be displaced in mantoquita.In addition, also can make metal passivation with electrochemical method, as Fe is placed in H
2SO
4As anode, make anodic polarization with impressed current in solution, adopt certain instrument that ferroelectric position is raise to a certain degree, Fe just has been passivated.By the metal passivation phenomenon that anodic polarization causes, be anode passivation or electrochemical passivation.
Metal is in passive state and can protects metal to prevent corrosion, and people once studied the mechanicalness scraped finish to the impact of the metal that is in passive state.Experiment shows, continuous scraped finish metallic surface during measurement, and the electromotive force of metal acutely moves to negative direction, and namely the finishing metal surface can cause the activation that is in passive metal.Prove that namely passivation phenomenon is a kind of surface phenomenon.It is under certain condition, changes on the interface that metal and medium are in contact with one another.When electrochemical passivation was anodic polarization, the current potential of metal changed and form metal oxide or salt on electrode surface.These materials closely cover become passive film on the metallic surface and cause metal passivation, chemical passivation be the picture dense HNO
3Directly the effect of metal is formed oxide film on the surface in oxygenant, or add the metal of easy passivation to cause as Cr, Ni etc.During chemical passivation, the oxidant concentration that adds should be not less than a certain threshold value, not so not only can not cause passive state, will cause that on the contrary metal dissolves faster.
Existing liquid phase passivating technique defective: (1) consumption is large.The passivator consumption of the crude still of a routine does not wait from several tons to tens tons, and cost is higher.(2) channeling is serious.Because the unhomogeneity of installing interior dirt layer causes liquid serious in its surperficial channeling, the dead angle easily appears.(3) liquid waste disposal difficulty, the Mn that contains in existing passivator
2+, Cr
2+Etc. heavy metal ion, environmental energy is caused severe contamination, contain Cl in the passivator that also has
-Stainless steel is formed stress cracking.(4) treatment time is long.Existing liquid phase passivating technique passivation time is generally at the tail gas valve about 24 hours, and the maintenance duration of complete assembly is shorter, causes overhauling the hysteresis of other work.
Summary of the invention
Technical problem to be solved by this invention is, a kind of ferrous sulfide gas-phase passivation method is provided, and can effectively overcome the following defective that in prior art, the liquid phase passivation exists: (1) consumption is large, and cost is high.Gaseous passivation mainly uses oxygen-rich air, and is easy to use, and cost is lower.(2) channeling is serious.Owing to being gas phase action, therefore there are not channeling and dead angle.(3) liquid waste disposal difficulty.Waste gas after gaseous passivation can reach emission standard after simple process.(4) treatment time is long.Gaseous passivation can carry out in steaming tower (light constituent in the steaming out tower) middle and later periods, can greatly shorten passivation time.
For solving the problems of the technologies described above, the invention provides a kind of ferrous sulfide gas-phase passivation method, comprise the step of the step of monitoring, the step of supplying gas and passivation.
Described method may further include the step of sealing and the step of discharging.
The step of described passivation is preferably: carry oxygen-rich air by steam and enter the gaseous passivation of implementing Iron sulfuret in container.
Described steam can be water vapor, and the pressure of described steam is 0.1～0.9Mpa.
Described oxygen-rich air is that the volume percent oxygen level can be 21%～50% air.
Described steam can be water vapor, and the pressure of described steam is preferably 0.3～0.4Mpa; Described oxygen-rich air is that the volume percent oxygen level is preferably 21%～35% air.
The step of described discharging can for: start vapour generator, produce water vapor, open successively valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the interior medium force feed of packing tower to gathering tank.The medium of packing tower is crude oil, and its effect is that active sulphur and the reaction of 20# Carbon steel stuffing material in crude oil forms Iron sulfuret.
The step of described monitoring can for: open successively moisture eliminator air intake valve 25, on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration; SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～8 hours, and SO
2Concentration of volume percent be down to 0.002% left and right from 0.237%, and when no longer changing within 30～80 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
The step of described monitoring may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 160～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.
Described method preferably further comprises:
Water inlet; Water is entered vapour generator 5 by valve;
Discharging; Start vapour generator and produce water vapor, open the valve 18 that is connected with steam-flow meter, then open successively upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 20 and gathering tank valve 22 after discharging is complete, unlatching lower inlet valve door 27, alkali liquid tank air intake valve 23 will steam tower tail gas and be delivered to exhaust gas processing device and data analysis set-up, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open gas meter air intake valve 17, the gas meter valve 19 of giving vent to anger, oxygen-rich air is carried, and give vent to anger by regulating oxygen pressure reducing valve, gas meter air intake valve 17, gas meter that to keep vapor pressures be 0.25～0.45Mpa for valve 19 and steam valve 18, steam flow is 0.8～1.2m
3/ h, compression oxygen-rich air pressure 0.25～0.45Mpa, flow is upper air valve 200～600ml/h;
Passivation; Open tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～8 hours, and SO
2Volumetric concentration be down to 0.003%～0.09%, and when no longer changing within 25～85 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
For solving the problems of the technologies described above, the present invention also provides a kind of gas phase deactivation method for petrochemical device, comprises the step of supplying gas and the step of passivation.
Described method may further include the step of monitoring and the step of discharging.
The step of described passivation can for: carry oxygen-rich air by steam and enter in container the gaseous passivation of implementing Iron sulfuret.
Described steam is preferably water vapor, and the pressure of described steam is 0.2～0.8Mpa.
Described oxygen-rich air is that the volume percent oxygen level is preferably 22%～55% air.
Described steam can be water vapor, and the pressure of described steam is 0.25～0.45Mpa; Described oxygen-rich air is that the volume percent oxygen level is 21%～35% air.
The step of described discharging is preferably: start vapour generator, produce water vapor, measure the flow of water vapor by the steam-flow meter that is connected with vapour generator, open steam valve valve 18, open successively again upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.The medium of packing tower is crude oil, and its effect is that active sulphur and the reaction of 20# Carbon steel stuffing material in crude oil forms Iron sulfuret.
The step of described passivation can be tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then starts online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 7～19 hours, and SO
2Volumetric concentration be down to 0.001%～0.09%, and when no longer changing within 30～60 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
The step of described passivation may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 180～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.
Described method may further include:
Water inlet; Tap water is sent into water softener, by water softener, tap water is softened, the tap water after softening enters vapour generator by valve;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, then open successively upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close air intake valve 20 and gathering tank valve 22 after discharging is complete, open lower inlet valve door 27 and alkali liquid tank air intake valve 23 and will steam the tower steam tail gas and be delivered to and be attached thereto exhaust gas processing device and the data analysis set-up that connects, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when inflammable gas content in packing tower is not in its limits of explosion scope, open gas meter air intake valve 17 and gas meter air outlet valve door 19, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulate oxygen pressure reducing valve, gas meter air intake valve 17, gas meter and give vent to anger that to keep vapor pressures be 0.3～0.4Mpa for valve 19 and steam valve 18, steam flow is 0.9～1.1m
3/ h, compression oxygen-rich air pressure 0.2～0.5Mpa, flow is 150～550ml/h;
Passivation; Open tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 8～10 hours, and SO
2Volumetric concentration be down to 0.001%～0.07%, and when no longer changing within 30～80 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
For solving the problems of the technologies described above, the present invention provides again a kind of gas-phase passivation system for petrochemical device, comprises gas phase passivation device, exhaust gas processing device and data analysis set-up.
Described exhaust gas processing device can be connected with described gas phase passivation device, for the treatment of the obnoxious flavour that produces in passivating process.
Described exhaust gas processing device may further include: the lye vat 13, alkali liquid tank air intake valve 23 and the tail gas valve 24 that contain 10% sodium hydroxide solution.
Described data analysis set-up,
Can be connected with described gas phase passivation device, be used for the front inflammable gas Data Detection of gaseous passivation;
And, in the gaseous passivation process, to the SO of passivation generation
2The online detection of concentration.
Described data analysis set-up may further include: gas flow dryer, gas chromatograph, computer, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26.
Described gas phase passivation device can be connected with data analysis set-up with described exhaust gas processing device respectively, is used for petrochemical equipment is carried out gaseous passivation.
Described gas phase passivation device preferably further comprises: steam supply parts, oxygen supply part and sealing element.
Described steam supply parts may further include: water softener, vapour generator, steam-flow meter and valve.
Described oxygen supply part may further include: compression oxygen-rich air bottle, gas meter, valve.
Described sealing element may further include: packing tower, give vent to anger valve and gathering tank valve 22.
Described phase passivation system in use, the step of discharging can for: start vapour generator, produce water vapor, measure the flow of water vapor by the steam-flow meter that is connected with vapour generator, open steam valve 18, on supply gas valve 20 and gathering tank valve 22, utilize steam will simulate in packing tower the medium force feed to the gathering tank that is connected with gathering tank valve 22.
Described phase passivation system in use, the step of passivation can for: open tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～15 hours, and SO
2Volumetric concentration be down to 0.005%～0.01%, and when no longer changing within 35～55 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Described phase passivation system in use, the step of passivation may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 180～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.。
Described phase passivation system method in use can comprise:
Water inlet; Water is sent into water softener, by water softener, water is softened, the water after softening enters vapour generator;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22; The medium of packing tower is crude oil, and its effect is that active sulphur and the reaction of 20# Carbon steel stuffing material in crude oil forms Iron sulfuret.
Monitoring; Close upper air valve 20 and gathering tank valve 22 after discharging is complete, unlatching lower inlet valve door 27 will steam the tower steam tail gas with alkali liquid tank air intake valve 23 and be disposed to exhaust gas processing device and the data analysis set-up that is connected with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when inflammable gas content in packing tower is not in its limits of explosion scope, open gas meter air intake valve 17 and gas meter air outlet valve door 19, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulate oxygen pressure reducing valve and steam valve 18, gas meter and give vent to anger that to keep vapor pressures be 0.2～0.5Mpa to valve 19, steam flow is 0.8～1.2m
3/ h, compression oxygen-rich air pressure 0.2～0.4Mpa, flow is 120～580ml/h;
Passivation; Open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 9～12 hours, and SO
2Volumetric concentration be down to 0.002%～0.1%, and when no longer changing within 40～70 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
For solving the problems of the technologies described above, the present invention provides a kind of ferrous sulfide gas phase passivation device again, comprises steam supply parts, oxygen supply part and sealing element.
Described gas phase passivation device can be connected with data analysis set-up with exhaust gas processing device respectively, is used for petrochemical equipment is carried out gaseous passivation.
Described steam supply parts may further include: water softener, vapour generator, steam-flow meter and valve.
Described oxygen supply part may further include: compression oxygen-rich air bottle, gas meter, valve.
Described sealing element may further include: packing tower, emptying valve 21 and gathering tank valve 22.
Described ferrous sulfide gas phase passivation device in use, the step of discharging can for: start vapour generator, produce water vapor, measure the flow of water vapor by the steam-flow meter that is connected with vapour generator, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.
Described ferrous sulfide gas phase passivation device in use, the step of passivation can for: open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～15 hours, and SO
2Volumetric concentration be down to 0.005%～0.01%, and when no longer changing within 35～55 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Described ferrous sulfide gas phase passivation device in use, the step of passivation can further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, as when simulating temperature in packing tower 1 higher than 180～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously.
Described ferrous sulfide gas phase passivation device method in use can comprise the following steps:
Water inlet; Tap water is sent into water softener, by water softener, tap water is softened, the tap water after softening enters vapour generator;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 20, gathering tank valve 22 after discharging is complete, unlatching alkali liquid tank air intake valve 23, tail gas valve 24 will steam the tower exhaust emissions to the exhaust gas processing device and the data analysis set-up that are connected with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process.
Described ferrous sulfide gas phase passivation device method in use can further include following steps:
Supply gas; When the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open oxygen air intake valve 17, the gas meter valve 19 of giving vent to anger, oxygen-rich air is carried, and pressure, flow indication by gas meter, tensimeter and steam-flow meter, regulating oxygen pressure reducing valve, steam valve 18 and gas meter air outlet valve door 19 maintenance vapor pressures is 0.3～0.5Mpa, and steam flow is 0.8～1.0m
3/ h, compression oxygen-rich air pressure 0.25～0.45Mpa, flow is 110～580ml/h;
Passivation; Open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～14 hours, and SO
2Volumetric concentration be down to 0.0015%～0.095%, and when no longer changing within 40～100 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Liquid phase passivating method compared to existing technology, the present invention has following useful technique effect:
(1) cost is low, implements simple.Gaseous passivation mainly uses oxygen-rich air, and is easy to use, and cost is lower.(2) passivation is even, does not have channeling.Owing to being gas phase action, therefore there are not channeling and dead angle.(3) off gas treatment is easy.Waste gas after gaseous passivation can reach emission standard after simple process.(4) treatment time is short.Gaseous passivation can carry out in steaming tower (light constituent in the steaming out tower) middle and later periods, and passivation time has reduced approximately 16 hours.
Description of drawings
Fig. 1 is the described simulation packing tower of embodiment of the present invention gas phase passivation device figure;
Fig. 2 is SO in passivation tail gas in the described gaseous passivation engineering of the embodiment of the present invention
2Concentration graph of a relation over time;
Fig. 3 is the photo of tower wall before the described gaseous passivation of the embodiment of the present invention;
Fig. 4 is the photo of tower wall after the described gaseous passivation of the embodiment of the present invention.
Embodiment
Gaseous passivation is its inner Iron sulfuret generation spontaneous combustion and the generation of explosion hazard when preventing opening unit before Maintenance And Modification of Petrochemical Plants, utilizes the method for the controlled oxidation of oxidizing gas take water vapor as carrier to what Iron sulfuret was implemented.
The gaseous passivation method of Iron sulfuret in petrochemical equipment of the present invention, to steam the tower middle and later periods, (0.3～0.4Mpa) oxygen-rich air that carries certain oxygen level (21%～35%) enters the gaseous passivation of implementing Iron sulfuret in distillation tower by low-pressure steam, the heat that passivation discharges is absorbed by the larger steam of thermal capacitance can not cause gathering of heat in tower, and the part sulfur dioxide gas that passivation generates is carried out by steam and can directly discharge after tower absorbs by the alkali lye condensation.
As shown in Figure 1, be the described simulation packing tower of embodiment of the present invention gas phase passivation device figure, wherein each Reference numeral is:
1, packing tower; 2, compression oxygen-rich air bottle; 3, gas meter; 4, water softener; 5, vapour generator; 6, steam-flow meter; 7, tensimeter; 8,20# Carbon steel stuffing material; 9,10,11, thermopair (attached not shown in FIG., actual be connected with computer 16); 12, steam distributor; 13, lye vat (containing 10% sodium hydroxide solution); 14, gas flow dryer (containing vitriol oil siccative); 15, on-line gas chromatography; 16, computer; 17～27, valve;
17～27 valve is respectively:
17, gas meter air intake valve; 18, steam valve; 19, the gas meter valve of giving vent to anger; 20, upper air valve; 21, blow-off valve; 22, the gathering tank valve 22; 23, alkali liquid tank air intake valve; 24, tail gas valve; 25, moisture eliminator air intake valve; 26, on-line chromatograph air intake valve; 27, lower inlet valve door.
A specific embodiments of the present invention is:
1. open water softener 4 Inlet and outlet water valves and start vapour generator 5, opening steam valve 18, upper air valve 20 and gathering tank valve 22, utilizing steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with valve 22.
2. discharging is closed upper air valve 20, gathering tank valve 22 after complete, opens emptying valve 21, lower inlet valve door 27 will steam tower tail gas and be disposed to pipe network by the pipeline that is connected with emptying valve 21, and monitors inflammable gas content in discharge process.
3. when inflammable gas content in packing tower is not in its limits of explosion scope, to open gas meter air intake valve 17, the gas meter valve 19 of giving vent to anger, and keep vapor pressure 0.3～0.4Mpa, steam flow is 1m
3/ h left and right, compression oxygen-rich air pressure 0.3～0.4Mpa, gas flow is the 400ml/h left and right.Open successively tail gas valve 24, moisture eliminator air intake valve 25, on-line chromatograph air intake valve 26, lower inlet valve door 27, then start the SO of online gas-chromatography monitoring
2Concentration (seeing Fig. 2) is also simulated the temperature in packing towers by thermopair 9,10,11 monitorings.
As shown in Figure 2, be SO in passivation tail gas in the described gaseous passivation process of the embodiment of the present invention
2Concentration graph of a relation over time; In figure, X-coordinate is the time of online gas-chromatography monitoring, and unit is minute; Ordinate zou is the SO of online gas-chromatography monitoring
2Concentration of volume percent.SO in tail gas when the gaseous passivation process has just begun as seen from Figure 2
2Content is higher, reaches 0.215%, is down to 0.016% and also no longer changes after 8h, illustrates that the tower internal reaction finishes substantially, and gaseous passivation is complete, each valve playback.
As shown in Figure 3, Figure 4, be respectively the photo of tower wall after the photo of tower wall before the described gaseous passivation of the embodiment of the present invention and gaseous passivation.
Do not find that by three thermopairs 9,10,11 in tower, temperature has obvious variation in passivating process, illustrate because the thermal capacitance of steam is larger, the shortage of heat that the Iron sulfuret oxidation discharges so that the temperature of system change.Also can find out the photo contrast before and after passivation, adhere to black precipitate on tower wall and tower tray before passivation, after passivation, black precipitate has become sorrel, illustrates that Iron sulfuret has been transformed into the oxide compound of the iron such as ferric oxide.
Another specific embodiments of the present invention is:
1, water inlet; Tap water is sent into water softener 4, softened by 4 pairs of tap water of water softener, the tap water after softening enters vapour generator 5.
2, discharging; Start vapour generator 5, produce water vapor, measure the flow of water vapors by the steam-flow meter 6 that is connected with vapour generator 5, open the steam valve 18 that directly is connected with steam-flow meter 6, open successively again upper air valve 20 and gathering tank valve 22, utilize steam will simulate the interior medium force feed of packing tower 1 to gathering tank.
3, monitoring; Close upper air valve 20 and gathering tank valve 22 after discharging is complete, the valve 27 of supplying gas under unlatching will steam the tower exhaust emissions to the exhaust gas processing device and the data analysis set-up that are connected with alkali liquid tank intake valve 23 with alkali liquid tank intake valve 23, and monitor inflammable gas content in discharge process.
4, supply gas; When the monitoring according to data analysis set-up, when the interior inflammable gas content of packing tower 1 is not in its limits of explosion scope, open gas meter air intake valve 17 and gas meter air outlet valve door 19, oxygen-rich air in compression oxygen-rich air bottle 2 is carried by gas meter 3, and pressure, flow indication by tensimeter 7 and steam-flow meter 6, adjusting gas flow meter air intake valve 17, gas meter are given vent to anger, and to keep vapor pressures be 0.3～0.4Mpa to valve 19, steam valve 18, and steam flow is 1m
3/ h left and right, compression oxygen-rich air pressure 0.3～0.4Mpa, flow is the 400ml/h left and right.
5, passivation; Open successively tail gas valve 24, moisture eliminator air intake valve 25, on-line chromatograph air intake valve 26 and lower inlet valve door 27, then start online gas-chromatography 15 monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 5～20 hours, and SO
2Volumetric concentration be down to a certain lower level (being generally 0.001%～0.1%) and when no longer changing, illustrate that the tower internal reaction finishes substantially within 20～90 minute, gaseous passivation is complete, each valve playback.In passivating process, can pass through simultaneously the temperature in thermopair 9,10,11 monitoring simulation packing towers 1, as when simulating temperature in packing tower 1 higher than a certain predefined threshold value (being for example 160～240 degrees centigrade), the flow that increases steam reduces the flow of oxygen-rich air simultaneously.
In general, can not find that by three thermopairs 9,10,11 in tower, temperature has obvious variation in passivating process, this is because the thermal capacitance of steam is larger, the shortage of heat that the Iron sulfuret oxidation discharges so that the temperature of system change.
Another embodiment of the present invention is a kind of ferrous sulfide gas-phase passivation method, comprises the step of the step of monitoring, the step of supplying gas and passivation.
Described method may further include the step of sealing and the step of discharging.
The step of described passivation is preferably: carry oxygen-rich air by steam and enter the gaseous passivation of implementing Iron sulfuret in sealed vessel.
Described steam can be water vapor, and the pressure of described steam is 0.1～0.9Mpa.
Described oxygen-rich air is that the volume percent oxygen level can be 21%～50% air.
Described steam can be water vapor, and the pressure of described steam is preferably 0.3～0.4Mpa; Described oxygen-rich air is that the volume percent oxygen level is preferably 21%～35% air.
The step of described discharging can for: start vapour generator, produce water vapor, open the steam valve 18 that directly is connected with steam-flow meter, open successively again upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.
The step of described passivation can for: open successively valve alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration; SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～18 hours, and SO
2Volumetric concentration be down to 0.002%～0.08%, and when no longer changing within 30～80 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
The step of described passivation may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 160～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.
Described method preferably further comprises:
Sealing; To treat that passivating material is positioned in the simulation packing tower of sealing;
Water inlet; Water is entered vapour generator by the Inlet and outlet water valve;
Discharging; Start vapour generator and produce water vapor, open the steam valve 18 that is connected with steam-flow meter, then open successively upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 22 and gathering tank valve 22 after discharging is complete, open lower inlet valve door 27 and will steam the tower exhaust emissions to the exhaust gas processing device and the data analysis set-up that are connected with alkali liquid tank air intake valve 23 with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open gas meter air intake valve 17 and gas meter air outlet valve door 19, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulating oxygen air intake valve, air intake valve 17, steam valve 18 and gas meter air outlet valve door 19 maintenance vapor pressures is 0.25～0.45Mpa, and steam flow is 0.8～1.2m
3/ h, compression oxygen-rich air pressure 0.25～0.45Mpa, flow is 200～600ml/h;
Passivation; Open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～16 hours, and SO
2Volumetric concentration be down to 0.003%～0.09%, and when no longer changing within 25～85 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
An embodiment more of the present invention is a kind of gas phase deactivation method for petrochemical device, comprises the step of supplying gas and the step of passivation.
Described method may further include the step of monitoring and the step of discharging.
The step of described passivation can for: carry oxygen-rich air by steam and enter in sealed vessel the gaseous passivation of implementing Iron sulfuret.
Described steam is preferably water vapor, and the pressure of described steam is 0.2～0.8Mpa.
Described oxygen-rich air is that the volume percent oxygen level is preferably 22%～55% air.
Described steam can be water vapor, and the pressure of described steam is 0.25～0.45Mpa; Described oxygen-rich air is that the volume percent oxygen level is 23%～36% air.
The step of described discharging is preferably: start vapour generator, produce water vapor, calculate the flow of water vapor by the steam-flow meter that is connected with vapour generator, open and steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.
The step of described passivation can for: open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 7～19 hours, and SO
2Volumetric concentration be down to 0.001%～0.09%, and when no longer changing within 30～60 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
The step of described passivation may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 160～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.
Described method may further include:
Water inlet; Tap water is sent into water softener, by water softener, tap water is softened, the tap water after softening enters vapour generator by the Inlet and outlet water valve;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 20, gathering tank valve 22 after discharging is complete, unlatching lower inlet valve door 27 will steam the tower steam tail gas with alkali liquid tank air intake valve 23 and be disposed to exhaust gas processing device and the data analysis set-up that is connected with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when inflammable gas content in packing tower is not in its limits of explosion scope, open gas meter air intake valve 17, the gas meter valve 19 of giving vent to anger, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulate oxygen air intake valve, gas meter air intake valve 17, steam valve 18, gas meter and give vent to anger that to keep vapor pressures be 0.3～0.4Mpa to valve 19, steam flow is 0.9～1.1m
3/ h, compression oxygen-rich air pressure 0.2～0.5Mpa, flow is 150～550ml/h;
Passivation; Open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 8～14 hours, and SO
2Volumetric concentration be down to 0.001%～0.07%, and when no longer changing within 30～80 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Another embodiment of the present invention is a kind of gas-phase passivation system for petrochemical device, comprises gas phase passivation device, exhaust gas processing device and data analysis set-up.
Described exhaust gas processing device can be connected with described gas phase passivation device, for the treatment of the obnoxious flavour that produces in passivating process.
Described exhaust gas processing device may further include: the lye vat 13, alkali liquid tank air intake valve 23 and the tail gas valve 24 that contain 10% sodium hydroxide solution.
Described data analysis set-up can be connected with described gas phase passivation device, is used for the front inflammable gas Data Detection of gaseous passivation; And, in the gaseous passivation process, to the SO of passivation generation
2The linearity test of concentration.
Described data analysis set-up may further include: gas flow dryer, gas chromatograph, computer, monitoring air intake valve and the monitoring valve of giving vent to anger.
Described gas phase passivation device can be connected with data analysis set-up with described exhaust gas processing device respectively, is used for petrochemical equipment is carried out gaseous passivation.
Described gas phase passivation device preferably further comprises: steam supply parts, oxygen supply part and sealing element.
Described steam supply parts may further include: water softener, vapour generator, steam-flow meter and valve.
Described oxygen supply part may further include: compression oxygen-rich air bottle, gas meter, oxygen valve.
Described sealing element may further include: packing tower, give vent to anger valve and gathering tank valve.
Described phase passivation system in use, the step of discharging can for: start vapour generator, produce water vapor, measure the flow of water vapor by the steam-flow meter that is connected with vapour generator, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.
Described phase passivation system in use, the step of passivation can for: open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～15 hours, and SO
2Volumetric concentration be down to 0.005%～0.01%, and when no longer changing within 35～55 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Described phase passivation system in use, the step of passivation may further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, during higher than 160～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously as the temperature in simulation packing tower 1.
Described phase passivation system method in use can comprise:
Water inlet; Water is sent into water softener, by water softener, water is softened, the water after softening enters vapour generator;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 20 and gathering tank valve 22 after discharging is complete, open lower inlet valve door 27 and will steam the tower exhaust emissions to the exhaust gas processing device and the data analysis set-up that are connected with alkali liquid tank air intake valve 23 with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process;
Supply gas; When the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open oxygen air intake valve and oxygen valve, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulate oxygen pressure reducing valve door, gas meter air intake valve 17, steam valve 18, gas meter and give vent to anger that to keep vapor pressures be 0.2～0.5Mpa to valve 19, steam flow is 0.8～1.2m
3/ h, compression oxygen-rich air pressure 0.2～0.4Mpa, flow is 120～580ml/h;
Passivation; Open successively tail gas valve alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 9～12 hours, and SO
2Volumetric concentration be down to 0.002%～0.1%, and when no longer changing within 40～70 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Another embodiment of the present invention is a kind of ferrous sulfide gas phase passivation device, comprises steam supply parts, oxygen supply part and sealing element.
Described gas phase passivation device can be connected with data analysis set-up with exhaust gas processing device respectively, is used for petrochemical equipment is carried out gaseous passivation.
Described steam supply parts may further include: water softener, vapour generator, steam-flow meter and valve.
Described oxygen supply part may further include: compression oxygen-rich air bottle, gas meter, valve.
Described sealing element may further include: packing tower, give vent to anger valve and gathering tank valve.
Described ferrous sulfide gas phase passivation device in use, the step of discharging can for: start vapour generator, produce water vapor, calculate the flow of water vapor by the steam-flow meter that is connected with vapour generator, open steam steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22.
Described ferrous sulfide gas phase passivation device in use, the step of passivation can for: open alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～15 hours, and SO
2Volumetric concentration be down to 0.005%～0.01%, and when no longer changing within 35～55 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Described ferrous sulfide gas phase passivation device in use, the step of passivation can further include: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, as when simulating temperature in packing tower 1 higher than 160～240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously.
Described ferrous sulfide gas phase passivation device method in use can comprise the following steps:
Water inlet; Tap water is sent into water softener, by water softener, tap water is softened, the tap water after softening enters vapour generator;
Discharging; Start vapour generator and produce water vapor, open steam valve 18, upper air valve 20 and gathering tank valve 22, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with gathering tank valve 22;
Monitoring; Close upper air valve 20 and gathering tank valve 22 after discharging is complete, open lower inlet valve door 27 and will steam the tower exhaust emissions to the exhaust gas processing device and the data analysis set-up that are connected with alkali liquid tank air intake valve 23 with alkali liquid tank air intake valve 23, and monitor inflammable gas content in discharge process.
Described ferrous sulfide gas phase passivation device method in use can further include following steps:
Supply gas; When the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open gas meter air intake valve 17 and gas meter air outlet valve door 19, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulate oxygen air intake valve, gas meter air intake valve 17, steam valve 18, gas meter and give vent to anger that to keep vapor pressures be 0.3～0.5Mpa to valve 19, steam flow is 0.8～1.0m
3/ h, compression oxygen-rich air pressure 0.25～0.45Mpa, flow is 110～580ml/h;
Passivation; Open successively alkali liquid tank air intake valve 23, tail gas valve 24, moisture eliminator air intake valve 25 and on-line chromatograph air intake valve 26, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 10～14 hours, and SO
2Volumetric concentration be down to 0.0015%～0.095%, and when no longer changing within 40～100 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
Claims (3)
1. a ferrous sulfide gas-phase passivation method, is characterized in that, comprises the step of the step of monitoring, the step of supplying gas and passivation
Described method further comprises the step of sealing and the step of discharging;
The step of described passivation is: carry oxygen-rich air by steam and enter the gaseous passivation of implementing Iron sulfuret in sealed vessel;
Described steam is water vapor, and the pressure of described steam is 0.1 ~ 0.9MPa;
Described oxygen-rich air is that the volume percent oxygen level is 21% ~ 50% air;
The step of described discharging is: start vapour generator, produce water vapor, open the steam valve that directly is connected with steam-flow meter, then open successively supply gas valve and gathering tank valve, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with the gathering tank valve;
The step of described passivation is: open successively tail gas valve, drain tap, monitoring air intake valve and the monitoring valve of giving vent to anger, then start online gas-chromatography monitoring SO
2Concentration; SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～18 hours, and SO
2Volumetric concentration be down to 0.002%～0.08%, and when no longer changing within 30～80 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
2. ferrous sulfide gas-phase passivation method according to claim 1, it is characterized in that, the step of described passivation further comprises: in passivating process, simulate temperature in packing tower by thermocouple monitoring simultaneously, as when simulating temperature in packing tower 1 higher than 160 ~ 240 ℃, the flow that increases steam reduces the flow of oxygen-rich air simultaneously.
3. ferrous sulfide gas-phase passivation method according to claim 1, is characterized in that, described method further comprises:
Sealing: will treat that passivating material is positioned in the simulation packing tower of sealing;
Water inlet: water is entered vapour generator by the Inlet and outlet water valve;
Discharging: start vapour generator and produce water vapor, open the steam valve that is connected with steam-flow meter, then open successively supply gas valve and gathering tank valve, utilize steam will simulate the gathering tank that in packing tower, the medium force feed extremely is connected with the gathering tank valve;
Monitoring: air delivery valve door and gathering tank valve are closed in discharging complete rear pass, the valve of supplying gas under unlatching steams the tower steam tail gas with the air outlet valve goalkeeper and is disposed to exhaust gas processing device and the data analysis set-up that is connected with the valve of giving vent to anger, and monitors inflammable gas content in discharge process;
Supply gas: when the monitoring according to data analysis set-up, when in packing tower, inflammable gas content is not in its limits of explosion scope, open gas meter air intake valve and gas meter air outlet valve door, oxygen-rich air is carried, and pressure, flow indication by tensimeter and steam-flow meter, regulating oxygen pressure reducing valve door, gas meter air intake valve, steam valve and gas meter air outlet valve door maintenance vapor pressure is 0.25 ~ 0.45MPa, and steam flow is 0.8 ~ 1.2m
3/ h, compression oxygen-rich air pressure 0.25 ~ 0.45MPa, flow is 200 ~ 600ml/h;
Passivation: open successively alkali liquid tank air intake valve, tail gas valve, moisture eliminator air intake valve and on-line chromatograph air intake valve, then start online gas-chromatography monitoring SO
2Concentration, SO in tail gas when the gaseous passivation process has just begun
2Content is higher, when after 6～16 hours, and SO
2Volumetric concentration be down to 0.003%～0.09%, and when no longer changing within 25～85 minutes, the tower internal reaction finishes, gaseous passivation is complete, each valve playback.
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| CN103952657B (en) * | 2014-04-11 | 2016-03-23 | 中国石油化工股份有限公司 | Ferrous sulfide gas phase passivation device |
| CN104804766B (en) * | 2015-05-07 | 2017-03-08 | 安庆市新城防腐清洗有限公司 | A kind of ferrous sulfide gas-phase passivation method |
| CN105463365A (en) * | 2015-11-19 | 2016-04-06 | 北京石油化工学院 | Spontaneous-combustion active ferrous sulfide gaseous phase passivation device and method |
| CN116143178A (en) * | 2023-04-23 | 2023-05-23 | 北京石油化工学院 | Vapor phase passivation system and method for iron-sulfur compounds |
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