CN104986740B - A kind of claus tail-gas clean-up system and processing method - Google Patents
A kind of claus tail-gas clean-up system and processing method Download PDFInfo
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Abstract
The present invention provides a kind of claus tail-gas clean-up system, it includes hydrogenation unit, quenching unit, desulfurization unit and optional hydrolysis unit, molten sulfur degasification gas feed unit.Present invention also offers a kind of claus tail-gas clean-up method.The exhaust treatment system and processing method sulfur removal rate of the present invention can reach more than 99.99%, be discharged into H in the tail gas of air2S concentration is less than 10ppm, is converted to SO2Concentration<50mg/m3, the removal efficiency and concentration of emission can meet current maximum emission limitation standard.In addition, also have the advantages that environmental-friendly, reliable and stable, small investment, operating cost are low etc..
Description
Technical field
The present invention relates to sulfur-containing tail gas process field, and in particular to a kind of processing system of claus sulphur recovery units tail gas
System, and the exhaust gas treating method using the processing system.
Background technology
In the production processes such as petrochemical industry, coal chemical industry, the sulphur in raw material finally changes into Containing Sulfur in process
The sour gas of hydrogen, it is necessary to handled or recycled.Hydrogen sulfide is changed into sulphur by generally use Crouse recovery technology of sulfur at present
Sulphur.
Crouse's recovery technology of sulfur is made of a thermal response section and several catalyst reaction sections, i.e., containing H2The acidity of S
Gas carries out imperfect combustion in combustion furnace with air, strictly controls air quantity, makes H2The SO generated after S burnings2Amount meets H2S/
SO2Molecular proportion is equal or close to 2, H2S and SO2Reaction generation elementary sulfur at high temperature, is limited by thermodynamic condition, remaining
H2S and SO2Into catalyst reaction section under the action of catalyst, continue to generate the reaction of elementary sulfur.In thermal response section and often
A catalyst reaction section downstream is respectively provided with sulfur condenser, will react generation elementary sulfur condensation separation, condensed liquid-state sulfur into
Enter the wait of liquid stream storage tank and directly transport outward or be molded into solid sulfur outward transport with molten sulfur.
In the reaction that thermal response section occurs, the chemical equation of main reaction is as follows：
H2S+3/2O2---SO2+H2O
2H2S+SO2---3/2S2+2H2O
The chemical equation of side reaction is as follows：
CnH(2n+2)+(3n+1)/2O2---(n+1)H2O+n CO2
H2S+CO2---COS+H2O
CH4+2S2---CS2+2H2S
2NH3+3/2O2---3H2O+N2
CO2+3/2S2---CS2+SO2
In the reaction that catalyst reaction section occurs, the chemical equation of main reaction is as follows：
2H2S+SO2---3/xSx+2H2O
Side reaction (mainly COS and CS2Hydrolysis) chemical equation it is as follows：
COS+H2O---CO2+H2S
CS2+2H2O---CO2+2H2S
In Crouse's recovery technology of sulfur, since chemical balance and reversible reaction are limited under by reaction temperature, even if
In the case where equipment and operating condition are good, using the good catalyst of activity and three-level claus process, sulfur recovery rate is most
Height also can only achieve 95%~97%, it is necessary to further reduce discharge using sulfur recovery tail gas treatment process.
So far as many as nearly 20 kinds of industrialized tail gas clean-up technique has been realized.It is broadly divided into low temperature Claus process, selection
The three major types such as property oxidizing process, reducing absorping method.
Low temperature Claus process is the H on solid catalyst in the case of less than sulphur dew point2S and SO2Continue Ke Lao
This reaction, since temperature is than relatively low, after gaseous sulphur condenses, is conducive to direction movement of the reaction balance towards generation sulphur, increase
Sulfur recovery rate, the total sulfur recovery rate of sulfur recovery unit for making vent gas treatment using the technique reach as high as 99%.This method
Comparatively flow is simple, equipment investment and operating cost are relatively low.Since temperature is than relatively low, thus COS, CS2Deng organic sulfide
Thing can not convert decomposition in tail gas, while this method is to front end sulphur technique H2S/SO2Proportion requirement it is stringent.
Selective oxidation method is to increase a reactor that catalyst for selective oxidation is housed after Crouse's sulphur recovery,
The catalyst is by H2Directly selecting property of S is oxidized to elementary sulfur, in order to make the final stage claus reaction device of upstream sulfur recovery facility
SO is substantially free of in outlet2, the vulcanization excess hydrogen operation of sulphur recovery use at this time, rather than conventional control H must be made2S/SO2=2
Operation measure, the hydrogen sulfide of 0.8%~1.5% (v) is contained in the tail gas for the final stage reactor for making to leave sulphur recovery.Using
The total sulfur recovery rate of sulfur recovery unit that the technique makees vent gas treatment is about 99%.
Reducing absorping method is after the reducibility gas such as Claus tail gases and hydrogen are mixed and heated to 220 DEG C or so, into
Enter hydrogenation reactor, under hydrogenation catalyst effect, make the sulphur and sulfide (S in tail gas6、S8、COS、CS2) almost all turn
Become hydrogen sulfide, which enters desulfuration absorbing tower after cooling, and most hydrogen sulfide and partial CO 2 are by hydramine
Solvent absorption, makes total sulfur in tail gas be less than 300ppm, is discharged after tail gas burns.Absorb the rich solution of hydrogen sulfide, carbon dioxide
Into regenerator, as raw material, the lean solution after regeneration returns to absorption tower and recycles regeneration overhead acidity pneumatic transmission to sulfur recovery.Should
Technique is using the sulphur in tail gas of sulphur and sulfide hydrogenating reduction or is hydrolyzed into hydrogen sulfide, and through hydramine solvent absorption to reach
The purpose of cleaning of off-gas, the total sulfur in tail gas can be reduced to below 300ppm, and the overall recovery of sulphur is up to 99.8%.The method technique
Flow is more complicated, and operation and operating cost are very high.
To sum up, in this three classes processing method, though selective oxidation processes and low-temperature Claus technique have technique
The advantages such as flow is simple, small investment, operating cost are low, but sulfur recovery rate is low, can only achieve 99%, it is impossible to meet existing country
To SO in source of atmospheric pollution discharge standard2Concentration of emission is less than 550mg/m3Requirement.Reduction-absorption process flow is complicated, investment
High, operating cost height, though can meet the requirement of existing national discharge standard of air pollutants, desulfurization degree can only achieve
99.8%, it is impossible to meet the environmental protection standard of higher, for example, even if using special formulation alcohol amine solvent, increase solvent internal circulating load and
Depth is regenerated, can not also meet key area SO in petroleum refining industry pollutant emission standard2<100mg/m3, petrochemistry work
General area SO in industry pollutant emission standard2<100mg/m3Requirement, it is even more impossible to reach petro chemical industry pollutant emission
Key area SO in standard2<50mg/m3Standard.
In recent years, due to the limitation of environmental carrying capacity, requirement of the local governments at all levels to the concentration of emission of sulfur recovery rate and sulphur
Higher, drug in some provinces have required SO2Concentration of emission is less than 50mg/m3, this proposes higher to sulfur recovery tail gas treatment process
It is required that.
A small amount of H is generally dissolved with addition, being pooled to from every grade of sulfur condenser in the molten sulfur of molten sulfur storage tank2S, in order to ensure to pacify
Full processing or transport, it is necessary to which first removing is dissolved in H therein from molten sulfur2S is general to use circulation spray processing or stripping work
Skill, is stirred or is passed through that hydrogen sulfide content is extremely low or gas of not sulfur-bearing carries out the means removing vulcanization such as stripping using the sprinkling of molten sulfur
Hydrogen, in these removings H2It can be formed containing H during S2The exhaust gas of S, is known as molten sulfur degasification gas, the sulphur in usual molten sulfur degasification gas
Compound is to SO in exhaust emissions2Contribution up to 100~200mg/m3, therefore, it is also desirable to which the gas is handled.
The content of the invention
In view of drawbacks described above present in domestic and international current Crouse's sulfur recovery tail gas treatment process, of the invention one
A purpose is to provide a kind of claus tail-gas clean-up system.
It is a further object to provide a kind of claus tail-gas clean-up method.
A kind of claus tail-gas clean-up system provided by the invention, including following processing unit：
Hydrogenation unit, for pending Claus tail gases and reducibility gas to be reacted, makes wherein sulfur-bearing component transformation
For H2S；
Hydrolysis unit, for by remaining COS, CS in the tail gas of the hydrogenation unit2H is changed into by hydrolysis2S；
Quenching unit, for the tail gas of the hydrolysis unit to be cooled；And
Desulfurization unit, for the tail gas of the quenching unit to be carried out oxidation sweetening processing, makes H therein2S is changed into list
Matter sulphur.
In claus tail-gas clean-up system provided by the invention, the processing system is further included to be taken off for providing the molten sulfur
Gas gas carries out the molten sulfur degasification gas feed unit of oxidation sweetening processing, it is connected with the desulfurization unit.
In claus tail-gas clean-up system provided by the invention, the molten sulfur degasification gas feed unit includes sulphur mist washing dress
Put and injection apparatus, the sulphur mist wash mill are used to wash away the sulphur in the molten sulfur degasification gas, the spray using shower water
Injection device is used to the molten sulfur degasification gas after washing being pumped into the desulfurization unit.
In claus tail-gas clean-up system provided by the invention, the hydrolysis unit includes desuperheating device and hydrolysis is anti-
Device is answered, wherein, the desuperheating device is used to the tail gas of the hydrogenation unit carrying out desuperheating processing, its cooling medium is
Reaction is hydrolyzed in water vapour, the tail gas that the hydrolysis reaction device is used for the hydrogenation unit after desuperheating is handled, wherein
It is filled with hydrolyst.
Another kind claus tail-gas clean-up system provided by the invention, including following processing unit：
Hydrogenation unit, for pending Claus tail gases and reducibility gas to be reacted, makes wherein sulfur-bearing component transformation
For H2S；
Quenching unit, for the tail gas of the hydrogenation unit to be cooled；
Desulfurization unit, for the tail gas of the quenching unit to be carried out oxidation sweetening processing, makes H therein2S is changed into list
Matter sulphur；And
Molten sulfur degasification gas feed unit, it is connected with the desulfurization unit, and stating molten sulfur degasification gas for offer is aoxidized
Desulfurization process.
In claus tail-gas clean-up system provided by the invention, the processing system further includes hydrolysis unit, it is between institute
State between hydrogenation unit and the quenching unit, for by remaining COS, CS in the tail gas of the hydrogenation unit2Pass through hydrolysis
Reaction is changed into H2S。
In claus tail-gas clean-up system provided by the invention, the hydrolysis unit includes desuperheating device and hydrolysis is anti-
Device is answered, wherein, the desuperheating device is used to the tail gas of the hydrogenation unit carrying out desuperheating processing, its cooling medium is
Reaction is hydrolyzed in water vapour, the tail gas that the hydrolysis reaction device is used for the hydrogenation unit after desuperheating is handled, wherein
It is filled with hydrolyst.
In claus tail-gas clean-up system provided by the invention, the molten sulfur degasification gas feed unit includes sulphur mist washing dress
Put and injection apparatus, the sulphur mist wash mill are used to wash away the sulphur in the molten sulfur degasification gas, the spray using shower water
Injection device is used to the molten sulfur degasification gas after washing being pumped into the desulfurization unit.
In above-mentioned claus tail-gas clean-up system, the hydrogenation unit includes preheating device and hydrogenation reaction device,
Wherein, the preheating device is used to preheat the pending Claus tail gases, and the hydrogenation reaction device is used to be hydrogenated with
Reaction, wherein being filled with hydrogenation catalyst.
In above-mentioned claus tail-gas clean-up system, it is single that the hydrogenation reaction device is also associated with reducibility gas supply
Member, for providing reducibility gas to the hydrogenation reaction device.
In above-mentioned claus tail-gas clean-up system, the quenching unit includes quenching apparatus, circulating pump and cooling dress
Put, the liquid distribution trough for spraying chilled water (chw) is provided with the quenching apparatus, the chilled water (chw) of spray is with from bottom to top conveying
Tail gas counter current contacting carry out chilling, the circulating pump is connected with the bottom of the quenching apparatus, the cooling device respectively with
The liquid distribution trough of the circulating pump and the quenching apparatus is connected.
In above-mentioned claus tail-gas clean-up system, the circulating pump is also connected with the sulphur mist wash mill, for
The sulphur mist wash mill make-up water.
In above-mentioned claus tail-gas clean-up system, the desulfurization unit includes the desulfurization reactor containing catalyst solution
And sulphur filtration apparatus, the tail gas of the quenching unit and/or the molten sulfur degasification gas are aoxidized in the desulfurization reactor
Elemental sulfur is generated, is discharged after then the elemental sulfur is filtered by the sulphur filtration apparatus.
In above-mentioned claus tail-gas clean-up system, the desulfurization unit further includes connected liquid distributing device and supercharging dress
Put, the liquid distributing device is connected with the quenching unit, the moisture in tail gas for removing the quenching unit, the supercharging
Device is connected with the desulfurization reactor, for being passed through the desulphurization reaction after the tail gas of the quenching unit is pressurized
Device.
A kind of claus tail-gas clean-up method provided by the invention comprises the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：Reaction is hydrolyzed in the tail gas of the S1 steps, makes remaining COS, CS2It is changed into H2S；
S3：By the tail gas quenching of the S2 steps to 30~90 DEG C；
S4：The tail gas of the S3 steps is subjected to oxidation sweetening processing, makes H therein2S is changed into elemental sulfur.
Wherein, in the S3 steps by the tail gas quenching of the S2 steps to 40~80 DEG C, be preferably chilled to 50~70 DEG C.
Wherein, the S4 steps further include：By the molten sulfur degasification gas from Cross unit and the tail gas of the S3 steps
It is carried out at the same time oxidation sweetening processing.
Another kind claus tail-gas clean-up method provided by the invention comprises the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：By the tail gas quenching of the S1 steps to 30~90 DEG C；
S3：The tail gas of the S2 steps and the molten sulfur degasification gas from Cross unit are subjected to oxidation sweetening processing,
Make H therein2S is changed into elemental sulfur.
Wherein, in the S2 steps by the tail gas quenching of the S1 steps to 40~80 DEG C, be preferably chilled to 50~70 DEG C.
Wherein, the S1 steps are further included pending Claus tail gases and reducibility gas reaction and then carried out
Hydrolysis, makes remaining COS, CS2It is changed into H2S。
Claus tail-gas clean-up system and processing method provided by the invention have the following advantages：
(1) exhaust treatment system of the invention and processing method by being hydrogenated with, hydrolyzing, the processing such as oxidation sweetening, can
The sulfur-bearing component in Claus tail gases is set farthest to be changed into H2S, then be changed into solid-state elemental sulfur and recycled, can be most
The sulphur in exhaust gas is set to bigization to be removed and recycled, sulfur removal rate can reach more than 99.99%, be discharged into the tail gas of air
Middle H2S concentration is less than 10ppm, is converted to SO2Concentration<50mg/m3, the removal efficiency and concentration of emission can meet current highest row
Put limitation standard.
(2) exhaust treatment system of the invention and processing method can make to come from while Claus tail gases are handled
The molten sulfur degasification gas of molten sulfur storage tank carries out desulfurization process in the lump, further increases the quality of claus process exhaust gas discharge, subtracts
Light environmental pollution.
(3) in exhaust treatment system of the invention and processing method, the waste water produced for system can be subject to profit again
With not only reducing the dosage of external water resource, decrease the discharge of waste water, so as to further mitigate environmental pressure.
(4) processing system of the invention is reliable and stable, small investment, operating cost is low, has a extensive future.
Brief description of the drawings
Fig. 1 is the structure diagram of claus tail-gas clean-up system of the present invention；
Wherein, the reference numerals are as follows：11st, preheating device；12nd, hydrogenation reaction device；21st, desuperheating device；22nd, water
Solve reaction unit；31st, quenching apparatus；32nd, circulating pump；33rd, cooling device；34th, fluid level control valve；41st, desulfurization reactor；42、
Sulphur filtration apparatus；43rd, liquid distributing device；44th, supercharging device；51st, sulphur mist wash mill；511st, sulphur mist washer；512nd, washing follows
Ring pumps；52nd, injection apparatus；521st, injector；522nd, jet pump；A, Claus tail gases；B, reducibility gas；C, hydrogenation unit
Tail gas；D, the tail gas of hydrolysis unit；E, the tail gas of quenching unit；F, elemental sulfur；G, the tail gas of desulfurization unit；H, molten sulfur degasification
Gas；I, low pressure water vapor；J, oxygen-containing gas.
Embodiment
In the following, with reference to attached drawing, the present invention will be described in detail.
One aspect of the present invention provides a kind of claus tail-gas clean-up system, it includes adding successively according to process flow
Hydrogen unit, hydrolysis unit, quenching unit and desulfurization unit, wherein, hydrogenation unit be used for by pending Claus tail gases with
Reducibility gas reaction makes wherein sulfur-bearing component be changed into H2S, hydrolysis unit is used for will be remaining in the tail gas of hydrogenation unit
COS、CS2H is further transformed to by hydrolysis2S, quenching unit are used to cool down the tail gas quenching of hydrolysis unit, desulfurization list
Member is used to the tail gas of quenching unit carrying out oxidation sweetening processing, makes H therein2S is changed into elemental sulfur, thus completes Crouse
The processing procedure of tail gas.
During above-mentioned claus tail-gas clean-up system work, it is single that the tail gas A from Crouse's processing unit initially enters hydrogenation
Member, the SO in tail gas2、COS、CS2Deng sulfur-bearing component and reducibility gas B (predominantly H2) reaction, generate H2S、CO2And H2O。
SO2+3H2---H2S+2H2O
S+H2---H2S
CO is also usually included in reducibility gas B, it participates in that following reaction occurs：
SO2+CO---COS+O2
S+CO---COS
Meanwhile the tail gas A of Crouse's processing unit also occurs that following reaction：
COS+H2O---H2S+CO2
CS2+2H2O---2H2S+CO2
In the tail gas C of hydrogenation unit, most of sulfur-bearing component has been converted to H2S-shaped state, but still may remain a small amount of COS and
CS2, total amount is typically smaller than 100ppm, H further converted it into subsequently into hydrolysis unit2S, in hydrolysis unit, occurs as follows
Reaction：
COS+H2O---H2S+CO2
CS2+2H2O---2H2S+CO2
The tail gas typical temperature of hydrolysis unit is higher, carries out desulfurization process again after need to carrying out cooling processing, therefore hydrolyze single
The tail gas D of member enters quenching unit and carries out cooling treatment.The temperature of tail gas E after quenching unit processing can be 30~90 DEG C,
Preferably 40~80 DEG C, be most preferably 50~70 DEG C.In currently used Claus tail gases amine absorption technique, exhaust temperature leads to
Often it is 35~40 DEG C, its main purpose is that (such as at 35~40 DEG C) amine liquid has hydrogen sulfide preferable absorption when temperature is relatively low
Effect, and it is of the invention since amine absorption technique need not be carried out, can be according to production status tune so there is no need to strictly control exhaust temperature
Section, advantageously reduces the usage amount of cooling medium.
Tail gas E after quenching unit processing is sent into desulfurization unit, by the oxidation processes of desulfurization unit, by H2S changes
For elemental sulfur F, solid elemental sulfur F can be used as byproduct to collect and recycle, the tail gas G of desulfurization unit directly discharge or burning at
Reason.
In an embodiment of claus tail-gas clean-up system according to the present invention, at Claus tail gases of the invention
Reason system further includes molten sulfur degasification gas feed unit, it is connected with desulfurization unit, the molten sulfur that will can be produced in Cross unit
Degassing gas H is delivered to desulfurization unit and removes H therein2S。
In an embodiment of claus tail-gas clean-up system according to the present invention, as shown in Figure 1, molten sulfur degasification gas
Feed unit includes sequentially connected sulphur mist wash mill 51 and injection apparatus 52, and spray is provided with sulphur mist wash mill 51
Water, for washing away the sulphur in molten sulfur degasification gas H, injection apparatus 52 is used to the molten sulfur degasification gas after washing being pumped into desulfurization unit.
In one preferred embodiment, as shown in Figure 1, sulphur mist wash mill 51 include sulphur mist washer 511 and
Cleaning circulation pump 512, the top in sulphur mist washer 511 are provided with spray thrower, from top to bottom spray washing water, molten sulfur degasification gas
H is washed with its counter current contacting from bottom to top, is removed sulfur vapor contained in molten sulfur degasification gas H by spraying, and make liquid
The temperature of sulphur degassing gas H is reduced to less than 120 DEG C, and sulphur changes into solid-state by liquid, is stored in 511 bottom of sulphur mist washer.Washing
Circulating pump 512 is used to extract out the washings of 511 bottom of sulphur mist washer, and is delivered to spray thrower circulation and is sprayed.In liquid
While sulphur degassing temperature degree reduces, the acid water vapor after portion washes is entered in molten sulfur degasification gas, therefore must be supplemented and be washed
Water is washed, the washings may be from the supply outside processing system, the waste water of the other units of processing system can also be used, such as chilling list
The cooling water of member.The present invention is not particularly limited for sulphur mist washer, this area can be used arbitrarily to possess same or similar work(
The equipment of energy, such as scrubbing tower etc..
In one preferred embodiment, as shown in Figure 1, injection apparatus 52 includes injector 521 and jet pump
522, the tail gas H after injector 521 can wash sulphur mist wash mill 51 is pumped among desulfurization unit, and jet pump 522 is for being
Injector 521 provides suction power.The present invention is not particularly limited for injector, jet pump, this area can be used arbitrarily to have
The equipment of standby same or similar function.
In an embodiment of claus tail-gas clean-up system according to the present invention, as shown in Figure 1, hydrogenation unit bag
Include preheating device 11 and hydrogenation reaction device 12.Preheating device 11 is used to preheat pending Claus tail gases A to suitable
Reaction temperature, preheating device 11 can arbitrarily possess the equipment of same or similar function, such as heat exchanger for this area.Hydrogenation is anti-
Device 12 is answered to be used to be reacted the Claus tail gases A after preheating and reducibility gas B, hydrogenation reaction device 12 can be this
The equipment that field arbitrarily possesses same or similar function, such as hydrogenation reactor.Hydrogenation is filled with hydrogenation reaction device 12 to urge
Agent, hydrogenation catalyst therein are not particularly limited, such as can be selected using aluminium oxide as the cobalt of carrier, molybdenum catalyst etc.,
It is preferred that low temperature hydrogenation catalyst, it can run in 200 DEG C to 220 DEG C of inlet temperature, so as to using steam
Heating response device, saves equipment investment.
In one preferred embodiment, hydrogenation reaction device 12 is also associated with reducibility gas air supply unit, is used for
Reducibility gas B is provided to hydrogenation reaction device 12.
In an embodiment of claus tail-gas clean-up system according to the present invention, as shown in Figure 1, hydrolysis unit bag
Include the hydrolysis reaction device 22 in 21 downstream of desuperheating device 21 and desuperheating device.Steamed in desuperheating device 21 using low pressure water
Vapour I can provide water as reaction raw materials as cooling medium to follow-up hydrolysis.It is filled with hydrolysis reaction device 22
Hydrolyst, hydrolyst are not particularly limited, such as can select support type organic sulfur hydrolyst or titanium-based water
Solve catalyst, it is preferred to use titanium-based hydrolyst, the tempreture organic sulphur hydrolysis that titanium-based hydrolyst can keep very high for a long time convert
Rate.The tail gas C of hydrogenation unit initially enters desuperheating device 21 and cools down, so that follow-up hydrolysis is in preferable temperature
Lower generation, the gas water entrainment after cooling enter in hydrolysis reaction device 22, and reaction is hydrolyzed under hydrolyst catalysis.
The present invention is not particularly limited for desuperheating device, hydrolysis reaction device, this area can be used arbitrarily to possess same or similar
The equipment of function, such as usual heat exchanger, reactor.
In an embodiment of claus tail-gas clean-up system according to the present invention, as shown in Figure 1, quenching unit master
To include quenching apparatus 31, it includes lower part air inlet, top gas outlet, top water inlet and bottom discharge mouth, inside and sets
It is equipped with the liquid distribution trough for spraying chilled water (chw).The tail gas D of hydrolysis unit is entered in quenching apparatus 31 by lower part air inlet, anxious
Cold water is entered in quenching apparatus 31 by top water inlet to be sprayed by liquid distribution trough, tail gas D in uphill process with spray
The chilled water (chw) counter current contacting of leaching carries out chilling, and the tail gas E after chilling is discharged by top gas outlet, the chilling coolant-temperature gage liter after chilling
Height, is extracted by bottom discharge mouth.Quenching unit further includes the circulating pump 32 and cooling device 33 being connected, circulating pump 32
It is connected with the bottom discharge mouth of quenching apparatus 31, the chilled water (chw) of 31 bottom of quenching apparatus is extracted out, in order to maintain the temperature of chilled water (chw)
Degree, cooling treatment, the top water inlet and liquid that cooling device 33 passes through quenching apparatus 31 are carried out by it by cooling device 33
Distributor is connected, and can be used chilled water (chw) after cooling again.The present invention is for quenching apparatus, circulating pump, cooling device
It is not particularly limited, this area can be used arbitrarily to possess the equipment of same or similar function, such as chilling tower, heat exchanger.Such as make
With chilling tower, wherein can be with built-in filler or empty spray tower.
In one preferred embodiment, as shown in Figure 1, circulating pump 32 can be with the sulphur of molten sulfur degasification gas feed unit
Mist washer 511 is connected, and is washed using chilled water (chw) as make-up water for sulphur mist.In quenching unit, with the tail of hydrolysis unit
The cooling of gas D, water cooling contained therein congeal into liquid, and the bottom of quenching apparatus 31 is gathered in together with chilled water (chw), chilled water (chw)
Liquid level is stepped up, it is necessary to by excessive water discharge quenching apparatus 31, to be used to part chilled water (chw) feed the washing of sulphur mist at this time
Device 511.It can be exported in circulating pump 32 and fluid level control valve 34 is set, sulphur mist washer is transported to adjust by fluid level control valve 34
The flow of 511 chilled water (chw), so as to control the liquid level of quenching apparatus 31, can also save the water consumption of processing system.
In an embodiment of claus tail-gas clean-up system according to the present invention, as shown in Figure 1, desulfurization unit bag
Desulfurization reactor 41 and sulphur filtration apparatus 42 containing catalyst solution are included, the tail gas E of quenching unit is in desulfurization reactor 41
In be oxidized to elemental sulfur F, the elemental sulfur F generated in order to prevent excessive accumulations in desulfurization reactor 41, using sulphur filter fill
Put 42 pairs of catalyst solutions containing elemental sulfur F to filter, elemental sulfur F is separated with catalyst solution, elemental sulfur F is as secondary
Product discharges processing system, and filtrate returns to desulfurization reactor 41 and continues cycling through use.The catalyst of filling in desulfurization reactor 41
Solution can be by H2S is oxidized to elemental sulfur, and the catalyst solution after reaction can be made with oxygen-containing gas J oxidation regenerations to circulate
With.Catalyst solution is simultaneously not limited, and this area can be used to possess any kind of same or similar function, as long as can be by H2S oxygen
Elemental sulfur is melted into, such as can be complexing iron catalyst commonly used in the art, can also be vanadium series catalyst etc..
In one preferred embodiment, as shown in Figure 1, desulfurization reactor 41 also with molten sulfur degasification gas feed unit
Jet pump 522 is connected, and working fluid of the solution as jet pump 522 can be extracted from desulfurization reactor 41.
In one preferred embodiment, as shown in Figure 1, desulfurization unit further include the liquid distributing device 43 that is connected and
Supercharging device 44, liquid distributing device 43 are connected with quenching unit, the moisture carried secretly in the tail gas E for removing quenching unit, supercharging
Device 44 is connected with desulfurization reactor 41, for the tail gas E of quenching unit to be pressurized, be then injected into desulfurization reactor 41 into
Row reaction.
The present invention has no especially for the desulfurization reactor in desulfurization unit, sulphur filtration apparatus, liquid distributing device, supercharging device
Limit, this area can be used arbitrarily to possess the equipment of same or similar function.Such as desulfurization reactor can use blistering reaction
Device, can also use the spray tower reactor of built-in filler.
In above-mentioned claus tail-gas clean-up system, H after hydrogenation unit is handled2When S conversion ratios are higher, it can also not include
Hydrolysis unit, therefore, present invention also offers another claus tail-gas clean-up system, it includes hydrogenation list according to process flow
Member, quenching unit, desulfurization unit and molten sulfur degasification gas feed unit, wherein, hydrogenation unit is used for pending Crouse
Tail gas makes wherein sulfur-bearing component be changed into H with reducibility gas reaction2S, quenching unit are used for the tail gas quenching of hydrolysis unit
Cooling, desulfurization unit are used to the tail gas of quenching unit carrying out oxidation sweetening processing, make H therein2S is changed into elemental sulfur, liquid
Sulphur degassing gas feed unit is connected with desulfurization unit, and state molten sulfur degasification gas for offer carries out oxygen together with the tail gas of quenching unit
Change desulfurization process.
Each embodiment of above-mentioned claus tail-gas clean-up system can be found in Fig. 1 and described above.
The second aspect of the invention provides a kind of claus tail-gas clean-up method, using processing system of the present invention
System, comprises the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：Reaction is hydrolyzed in the tail gas of S1 steps, makes remaining COS, CS2It is changed into H2S；
S3：By the tail gas quenching of S2 steps to 30~90 DEG C；
S4：The tail gas of S3 steps is subjected to oxidation sweetening processing, makes H therein2S is changed into elemental sulfur.
In one preferred embodiment, in S3 steps by the tail gas quenching of S2 steps to 40~80 DEG C.At one more
In preferred embodiment, by the tail gas quenching of S2 steps to 50~70 DEG C.
In one preferred embodiment, S4 steps further include：By the molten sulfur degasification gas from Cross unit at the same time
Carry out oxidation sweetening processing.
The claus tail-gas clean-up method of the present invention further includes another embodiment, specifically, comprises the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：By the tail gas quenching of S1 steps to 30~90 DEG C；
S3：The tail gas of S2 steps and the molten sulfur degasification gas from Cross unit are subjected to oxidation sweetening processing, make it
In H2S is changed into elemental sulfur.
In one preferred embodiment, in S2 steps by the tail gas quenching of S1 steps to 40~80 DEG C.At one more
In preferred embodiment, by the tail gas quenching of S1 steps to 50~70 DEG C.
In one preferred embodiment, S1 steps further include pending Claus tail gases and reducibility gas are anti-
And then reaction should be hydrolyzed, make remaining COS, CS2It is changed into H2S。
Treatment in accordance with the present invention system and/or processing method, can be with to the removal efficiency of the hydrogen sulfide in Claus tail gases
Reach more than 99.9%, the molten sulfur degasification gas of Cross unit can also be handled at the same time, be discharged into the tail gas of air
H2S concentration is less than 10ppm, is converted to SO2Concentration<50mg/m3, the conversion ratio and concentration of emission can meet current maximum emission
Limitation standard, and drastically reduce the area the acid water for needing outer row's processing.
In the following, the present invention is further described by embodiment.
Embodiment
Claus tail gases and molten sulfur degasification gas are handled as steps described below.
A, unstripped gas includes the molten sulfur degasification gas of Claus tail gases and Cross unit, and Claus tail gases come from two-stage gram
The third level sulfur condenser of Louth device, its component and property are：H2S contents 1.36% (V), SO2Content 0.34%, H2Content
1.59%th, COS contents 0.08% (V), CO contents 5.05%, CO2Content 44.45% (V), N2Content 10.72% (V), H2O contains
Measure 36.3%, SXContent 0.1%, temperature are 160 DEG C, pressure 114Kpa；Molten sulfur degasification gas comes from liquid sulfur pit, its component and
Property is：H2S contents 0.844% (V), H2O content 3.74% (V), N2Content 75.4% (V), O2Content 20.0%, SXContent
0.01%, temperature is 138 DEG C, pressure 90KPa.
B, Claus tail gases initially enter preheater, and gas temperature is increased to 238 DEG C using middle pressure steam, subsequently into
Hydrogenation reactor, has loaded low temperature Co-Mo hydrogenation catalysts TG-107 (Axens Products) in hydrogenation reactor, has been hydrogenated with
In reactor, under the action of catalyst, the SO in Claus tail gases2、COS、CS2With H2, CO reaction, generate H2S、CO2With
H2O.These reactions are exothermic reactions, and therefore, hydrogenation reactor outlet temperature reaches 308 DEG C.
C, hydrogenation reactor tail gas enters desuperheater, is reduced to exhaust temperature about by spraying into low-pressure saturated steam
180 DEG C, and extra water is provided at the same time and is used for hydrolysis, subsequently into hydrolysis reactor, it is filled with hydrolysis reactor is built-in
TiO2Base hydrolyst CRS31 (Axens Products), under catalyst action, the COS and H that are hydrogenated with tail gas2O is further
Generation hydrolysis, generates H2S and CO2。
D, hydrolysis reactor tail gas enters chilling tower, in chilling tower, tail gas and the chilled water (chw) counter current contacting recycled,
Temperature is reduced to about 50 DEG C, circulating pump from chilling tower bottom extract chilled water (chw) and send to chilling tower top liquid distribution trough it
In, excessive heat is taken out by chilling water cooler, and chilled water (chw) is cooled down using recirculated cooling water, is cooled down
Excess acid water is transported in sulphur mist washer, and by Liquid level valve regulation, tail gas after cooling enters follow-up single its flow
Member.
E, the molten sulfur degasification gas from liquid sulfur pit enters sulphur mist washer, and cleaning circulation pump is extracted from sulphur mist washer bottom
Acid water is simultaneously sent to the nozzle on sulphur mist washer top, is carried out spray washing to molten sulfur degasification gas, is made molten sulfur degasification gas
Temperature is reduced to about 90 DEG C, and the sulphur carried secretly in molten sulfur degasification gas changes into solid-state by liquid, comes from the excessive chilling of chilling tower
Water supplements and maintains the acid water liquid level of sulphur mist washer bottom.
F, tail gas enters the drop that liquid separation tank isolates entrainment after chilling, then boosts to 65KPa (G) by booster fan,
Then desulfurization reactor is entered by the gas distributor of desulfurization reactor bottom, the molten sulfur degasification gas come out from sulphur mist washer
Enter desulfurization reactor bottom after being mixed under the suction of injector with catalyst solution, in this two strands of gases and desulfurization reactor
The network and iron catalyst solution of filling contact, and the hydrogen sulfide in gas is hanged with network and ferrous solution reaction generation elemental sulfur, elemental sulfur
Float in catalyst solution, filtered out from catalyst solution elemental sulfur using sulphur filter.Used network and iron are molten
Liquid is regenerated using air oxidation, about 50 DEG C of desulfurization reactor temperature.
G, the exhaust gas of outflow burns into incinerator at the top of desulfurization reactor, after testing, sulphur in desulfurization reactor tail gas
Change hydrogen content is 2ppm, SO after burning2Content 10mg/m3。
Although with reference to exemplary embodiment describing the present invention, it is to be understood that, term used be explanation and it is exemplary,
And nonrestrictive term.Since the present invention can be embodied without departing from the spiritual or substantive of the present invention in a variety of forms,
So it is also understood that above-described embodiment is not limited to any foregoing details, and should be in the spirit that appended claims are limited
With widely explained in scope, therefore the whole changes fallen into claim or its equivalent scope and remodeling all should be appended power
Profit requires to be covered.
Claims (24)
1. a kind of claus tail-gas clean-up system, it is characterised in that include being sequentially connected the following processing connect according to process flow
Unit：
Hydrogenation unit, for pending Claus tail gases and reducibility gas to be reacted, makes wherein sulfur-bearing component be changed into H2S；
Hydrolysis unit, for by remaining COS, CS in the tail gas of the hydrogenation unit2H is changed into by hydrolysis2S；
Quenching unit, for the tail gas of the hydrolysis unit to be cooled；And
Desulfurization unit, for the tail gas of the quenching unit to be carried out oxidation sweetening processing, makes H therein2S is changed into elemental sulfur,
Including the desulfurization reactor containing catalyst solution and sulphur filtration apparatus, the tail gas of the quenching unit is in the desulphurization reaction
Elemental sulfur is generated by oxidation in device, is discharged after then the elemental sulfur is filtered by the sulphur filtration apparatus.
2. claus tail-gas clean-up system according to claim 1, it is characterised in that the processing system, which further includes, to be used for
The molten sulfur degasification gas feed unit that molten sulfur degasification gas carries out oxidation sweetening processing is provided, it is connected with the desulfurization unit.
3. claus tail-gas clean-up system according to claim 2, it is characterised in that the molten sulfur degasification gas feed unit
Including sulphur mist wash mill and injection apparatus, the sulphur mist wash mill is used to wash away the molten sulfur degasification gas using shower water
In sulphur, the injection apparatus is used to the molten sulfur degasification gas after washing being pumped into the desulfurization unit.
4. according to claim 1-3 any one of them claus tail-gas clean-up systems, it is characterised in that the hydrolysis unit bag
Desuperheating device and hydrolysis reaction device are included, wherein, the desuperheating device is used to carry out in the tail gas of the hydrogenation unit
Desuperheating processing, it is water vapour that it, which cools down medium, and the hydrolysis reaction device is used for the hydrogenation unit after desuperheating is handled
Tail gas reaction is hydrolyzed, wherein being filled with hydrolyst.
5. according to claim 1-3 any one of them claus tail-gas clean-up systems, it is characterised in that the hydrogenation unit bag
Preheating device and hydrogenation reaction device are included, wherein, the preheating device is used to preheat the pending Claus tail gases, institute
State hydrogenation reaction device to be used to carry out hydrogenation reaction, wherein being filled with hydrogenation catalyst.
6. claus tail-gas clean-up system according to claim 5, it is characterised in that the hydrogenation reaction device is also connected with
There is reducibility gas air supply unit, for providing reducibility gas to the hydrogenation reaction device.
7. according to claim 1-3 any one of them claus tail-gas clean-up systems, it is characterised in that the quenching unit bag
Quenching apparatus, circulating pump and cooling device are included, the liquid distribution trough for spraying chilled water (chw) is provided with the quenching apparatus,
The chilled water (chw) of spray and the tail gas counter current contacting from bottom to top conveyed carry out chilling, the bottom of the circulating pump and the quenching apparatus
Portion is connected, and liquid distribution trough of the cooling device respectively with the circulating pump and the quenching apparatus is connected.
8. claus tail-gas clean-up system according to claim 7, it is characterised in that the circulating pump also with the sulphur mist
Wash mill is connected, for the sulphur mist wash mill make-up water.
9. according to claim 1-3 any one of them claus tail-gas clean-up systems, it is characterised in that the desulfurization unit is also
Including connected liquid distributing device and supercharging device, the liquid distributing device is connected with the quenching unit, for removing the urgency
Moisture in the tail gas of cold unit, the supercharging device are connected with the desulfurization reactor, for by the tail of the quenching unit
Gas is passed through the desulfurization reactor after being pressurized.
10. a kind of claus tail-gas clean-up system, it is characterised in that include being sequentially connected the hydrogenation list connect according to process flow
Member, quenching unit and desulfurization unit, wherein：
Hydrogenation unit, for pending Claus tail gases and reducibility gas to be reacted, makes wherein sulfur-bearing component be changed into H2S；
Quenching unit, for the tail gas of the hydrogenation unit to be cooled；
Desulfurization unit, for the tail gas of the quenching unit to be carried out oxidation sweetening processing, makes H therein2S is changed into elemental sulfur；
The processing system further includes molten sulfur degasification gas feed unit, it is connected with the desulfurization unit, and molten sulfur is stated for providing
The gas that deaerates carries out oxidation sweetening processing；
The desulfurization unit includes the desulfurization reactor containing catalyst solution and sulphur filtration apparatus, the tail of the quenching unit
Gas and the molten sulfur degasification gas generate elemental sulfur in the desulfurization reactor by oxidation, then will by the sulphur filtration apparatus
Discharged after the elemental sulfur filtering.
11. claus tail-gas clean-up system according to claim 10, it is characterised in that the molten sulfur degasification gas supply is single
Member includes sulphur mist wash mill and injection apparatus, and the sulphur mist wash mill is used to wash away the molten sulfur degasification using shower water
Sulphur in gas, the injection apparatus are used to the molten sulfur degasification gas after washing being pumped into the desulfurization unit.
12. claus tail-gas clean-up system according to claim 10, it is characterised in that the hydrogenation unit includes preheating
Device and hydrogenation reaction device, wherein, the preheating device is used to preheat the pending Claus tail gases, the hydrogenation
Reaction unit is used to carry out hydrogenation reaction, wherein being filled with hydrogenation catalyst.
13. claus tail-gas clean-up system according to claim 12, it is characterised in that the hydrogenation reaction device also connects
Reducibility gas air supply unit is connected to, for providing reducibility gas to the hydrogenation reaction device.
14. claus tail-gas clean-up system according to claim 10, it is characterised in that the quenching unit includes chilling
Device, circulating pump and cooling device, the liquid distribution trough for spraying chilled water (chw) is provided with the quenching apparatus, spray
Chilled water (chw) and the tail gas counter current contacting from bottom to top conveyed carry out chilling, the bottom phase of the circulating pump and the quenching apparatus
Even, liquid distribution trough of the cooling device respectively with the circulating pump and the quenching apparatus is connected.
15. claus tail-gas clean-up system according to claim 11, it is characterised in that the quenching unit includes chilling
Device, circulating pump and cooling device, the liquid distribution trough for spraying chilled water (chw) is provided with the quenching apparatus, spray
Chilled water (chw) and the tail gas counter current contacting from bottom to top conveyed carry out chilling, the bottom phase of the circulating pump and the quenching apparatus
Even, liquid distribution trough of the cooling device respectively with the circulating pump and the quenching apparatus is connected.
16. claus tail-gas clean-up system according to claim 15, it is characterised in that the circulating pump also with the sulphur
Mist wash mill is connected, for the sulphur mist wash mill make-up water.
17. claus tail-gas clean-up system according to claim 10, it is characterised in that the desulfurization unit further includes phase
Liquid distributing device and supercharging device even, the liquid distributing device is connected with the quenching unit, for removing the quenching unit
Tail gas in moisture, the supercharging device is connected with the desulfurization reactor, for the tail gas of the quenching unit to be carried out
The desulfurization reactor is passed through after supercharging.
A kind of 18. claus tail-gas clean-up method, it is characterised in that comprise the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：Reaction is hydrolyzed in the tail gas of the S1 steps, makes remaining COS, CS2It is changed into H2S；
S3：By the tail gas quenching of the S2 steps to 30~90 DEG C；
S4：The tail gas of the S3 steps is subjected to oxidation sweetening processing, makes H therein2S is changed into elemental sulfur, filters the list of gained
Matter sulphur；Wherein, the desulfurization process uses Complexing Iron catalyst solution.
19. claus tail-gas clean-up method according to claim 18, it is characterised in that by the S2 in the S3 steps
The tail gas quenching of step is to 40~80 DEG C.
20. claus tail-gas clean-up method according to claim 19, it is characterised in that by the S2 in the S3 steps
The tail gas quenching of step is to 50~70 DEG C.
21. according to claim 18-20 any one of them claus tail-gas clean-up methods, it is characterised in that the S4 steps
Further include：The tail gas of molten sulfur degasification gas from Cross unit and the S3 steps is carried out at the same time oxidation sweetening processing.
A kind of 22. claus tail-gas clean-up method, it is characterised in that comprise the following steps：
S1：Pending Claus tail gases and reducibility gas are reacted, wherein sulfur-bearing component is changed into H2S；
S2：By the tail gas quenching of the S1 steps to 30~90 DEG C；
S3：The tail gas of the S2 steps and the molten sulfur degasification gas from Cross unit are subjected to oxidation sweetening processing, make it
In H2S is changed into elemental sulfur, filters the elemental sulfur of gained；Wherein, the desulfurization process uses Complexing Iron catalyst solution.
23. claus tail-gas clean-up method according to claim 22, it is characterised in that by the S1 in the S2 steps
The tail gas quenching of step is to 40~80 DEG C.
24. claus tail-gas clean-up method according to claim 23, it is characterised in that by the S1 in the S2 steps
The tail gas quenching of step is to 50~70 DEG C.
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| US10188988B2 (en) * | 2016-03-23 | 2019-01-29 | Exxonmobil Research And Engineering Company | Claus unit treatment of shutdown tail gas |
| CN106853323B (en) * | 2016-12-19 | 2019-12-10 | 宁波市化工研究设计院有限公司 | Ultralow-emission sulfur recovery tail gas absorption system |
| CN106829875A (en) * | 2017-03-08 | 2017-06-13 | 安徽宣城金宏化工有限公司 | A kind of handling process and equipment for carbon disulphide production Process Gas |
| CN110732238A (en) * | 2018-07-19 | 2020-01-31 | 中国石油天然气股份有限公司 | sulfur-containing tail gas treatment method and system |
| CN110817809B (en) * | 2018-08-14 | 2023-09-15 | 中国石油化工股份有限公司 | Claus tail gas treatment method and treatment system |
| CN109181784B (en) * | 2018-09-27 | 2020-06-12 | 中国成达工程有限公司 | Device and process for converting multi-component complex organic sulfur in crude synthesis gas into hydrogen sulfide |
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| CN1230134A (en) * | 1996-08-22 | 1999-09-29 | 国际壳牌研究有限公司 | Process for reducing total sulphur content in gases containing hydrogen sulphide and other sulphur components |
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