CN104555939A - Purified gas treatment process of sulfur recovery device - Google Patents
Purified gas treatment process of sulfur recovery device Download PDFInfo
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- CN104555939A CN104555939A CN201310481980.7A CN201310481980A CN104555939A CN 104555939 A CN104555939 A CN 104555939A CN 201310481980 A CN201310481980 A CN 201310481980A CN 104555939 A CN104555939 A CN 104555939A
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Abstract
The invention relates to a purified gas treatment process of a sulfur recovery device. The purified gas treatment process comprises a thermal reaction phase, a catalytic reaction phase and a tail gas purifying treatment phase, wherein in the tail gas purifying treatment phase, the Claus tail gas generated in the catalytic reaction phase is sequentially subjected to a hydrogenation reaction, cooling in a rapid quenching tower and amine liquid absorption, then the purified tail gas is fed to alkali liquor to be subjected to H2S removal treatment, and the tail gas removed from H2S is combusted and then discharged; the amine liquid amine-rich liquid absorbing H2S is fed to a regeneration tower to be regenerated, the regenerated acid gas is mixed with the acid gas, and then returned to the thermal reaction phase to further recover elemental sulfur; the exhausted lye removed from H2S is subjected to caustic dross biological treatment or acidic water stripping treatment. With adoption of the purified gas treatment process disclosed by the invention, H2S in the purified gas can be removed to 5 mg/m<3> below, the SO2 content in the smoke is obviously reduced within the reduction range of 100-1000 mg/m<3>; the exhausted lye treatment method is further provided, and the exhausted lye is subjected to the caustic dross biological treatment or the acidic water stripping treatment, so that pollution can be reduced.
Description
Technical field
The invention belongs to technical field of sulfur recovery, specifically, relate to a kind of sulfur recovery facility purified gas treatment process.
Background technology
Along with the development of society, problem of environmental pollution has become the restraining factors of rapid economic development, is that national governments make laws requisite important content.Industrially developed country requires very strict to sulphur emissions, Federal Government Bureau for Environmental Protection rules and regulations petroleum refining industry flue gas of heating furnace, tail gas of sulphur and regeneration fume from catalytic cracking SO
2concentration of emission limit value is 50ppm (v), about amounts to 143mg/m
3.
Current Chinese sulfur recovery facility flue gas SO
2concentration of emission performs GB16297-1996 " discharge standard of air pollutants ", standard regulation SO
2concentration of emission is less than 960mg/m
3.Within 2014, be about to the new environmental protection standard performed, regulation sulfur recovery facility flue gas SO
2concentration of emission is less than 400mg/m
3, area discharge is less than 200mg/m especially
3.SO in the most of sulfur recovery facility flue gas of current China
2though content is at 960mg/m
3below, but be difficult to reach 200mg/m
3standard-required.Affect sulfur recovery facility flue gas SO
2the factor of concentration of emission is mainly in Claus cleaning of off-gas containing a certain amount of sulfide.
The conversion ratio (particularly organic sulfur content) of the total sulfur content of cleaning of off-gas and the degree of purification of desulfurizing agent and catalyst is closely related, and cleaning of off-gas is mainly containing unabsorbed H
2s and organic sulfur, be converted into SO after incinerator burns
2, increase flue gas SO
2concentration of emission 150-500mg/m
3.If remove H2S process to purified gas, purified gas medium sulphide content is down to below 10ppm, SO in flue gas
2concentration will significantly decline.At present, the purified gas of sulfur recovery facility generally directly enters incinerator and burns, and does not carry out the desulfurization process of other modes.
Technical scheme described in CN98114460.8 " a kind of processing method of industrial waste gas containing sulphur oxide " cleaning of off-gas absorbing out through absorption tower in sulfur recovery facility is directly introduced incinerator to burn, and after burning, gas introducing catalytic oxidation tower carries out oxidative absorption by SO
2become SO
3, then by SO
3with alkali lye (Ca (OH)
2, or Mg (OH)
2) contact by-product gypsum.But increase catalytic oxidation tower and need increase equipment and cost of investment.
CN201010139106.1 " make sulphur processed and the exhaust gas treating method of intermediate of ammonium bisulfite " described in technical scheme be by the NH of sewage stripping unit in original recovery technology of sulfur
3separate and obtain gas ammonia or ammoniacal liquor, then by the tail gas (SO after burning
2) introduce and wherein react, generate NH
4hSO
3(NH
4)
2sO
3introduce the reaction of Claus reacting furnace after atomization again, so circulate, cleaning of off-gas qualified discharge.But generate NH
4hSO
3(NH
4)
2sO
3introduce the reaction of Claus reacting furnace after atomization again, the temperature of reacting furnace can be reduced, increase the energy consumption of device.
Summary of the invention
The present invention is intended to put forward the low technique of a kind of small investment altogether, operating cost to process sulfur recovery facility purified gas, removes the H in purified gas
2s, thus reduce SO in sulfur recovery facility flue gas
2concentration, solves SO in sulphur recovery
2discharge technical problem not up to standard.
Technical scheme of the present invention is: a kind of sulfur recovery facility purified gas treatment process, and its step comprises:
1) the thermal response stage:
Containing H
2sour gas partial combustion in reacting furnace of S is converted into SO
2, at high temperature H
2s and SO
2claus occurs and reacts generting element sulphur and reacting furnace tail gas, elementary sulfur enters the recovery of molten sulfur pond and obtains Molten sulphur, and reacting furnace tail gas enters catalytic reaction stages; Described reacting furnace ignition temperature is 900-1400 DEG C.
2) catalytic reaction stages:
Reacting furnace tail gas enters the one-level converter of catalytic reaction stages, react under catalyst action, generting element sulphur and one-level converter tail gas, elementary sulfur enters the recovery of molten sulfur pond and obtains Molten sulphur, one-level converter tail gas enters secondary reformer reaction, under catalyst action after Claus catalyzed conversion, elementary sulfur enters the recovery of molten sulfur pond and obtains Molten sulphur, the processing stage that the Claus tail gas after catalytic reaction entering tail gas clean-up;
3) processing stage of tail gas clean-up:
First Claus tail gas heating enters hydrogenation reactor after 200-300 DEG C, and under hydrogenation catalyst effect, sulfur-containing compound hydro-conversion is H
2s, is then cooled to 25-42 DEG C through quench tower, enters amine absorption tower, the H in amine absorption hydrogenation tail gas
2after S; Cleaning of off-gas is introduced in alkali lye and carry out removing H
2s process, removes H
2discharge after tail gas after S burns; Absorb H
2the amine liquid rich amine solution of S is introduced regenerator and is regenerated, regenerated acidic gas and step 1) in raw material sour gas mix, returning to the thermal response stage reclaims elementary sulfur further; Carry out removing H
2spent lye after S carries out harmless treatment.
The described thermal response stage is mixed combustion in reacting furnace by sour gas and air, control combustion temperature 900-1400 DEG C, the H of 1/3rd
2s burning conversion is SO
2, and at high temperature there is Claus reaction.
2H
2S+3O
2→2SO
2+2H
2O （1）
SO
2＋2H
2S→2H
2O＋3S （2）
Formed containing elementary sulfur, H
2s, SO
2with COS, CS
2process Gas.Elementary sulfur wherein enters molten sulfur pond through condensation, and Process Gas enters catalyst reaction section.
Described catalytic reaction stages refers to the Process Gas that the thermal response stage produces, and enters one-level converter and the secondary reformer of filling Claus reforming catalyst, under the effect of catalyst, occurs to react as follows:
SO
2＋2H
2S→2H
2O＋3S （3）
COS+H
2O→H
2S+CO
2（4）
CS
2+2H
2O→2H
2S+CO
2（5）
After Claus catalyzed conversion, elementary sulfur enters molten sulfur pond through condensation, and reacted Claus tail gas contains micro-sulphur, H
2s, SO
2with COS, CS
2sulfides, enters Tail gas cleanup unit.
Refer to that Claus tail gas is heated to 200-300 DEG C and enters hydrogenation reactor processing stage of described tail gas clean-up, under the effect of hydrogenation catalyst, the elementary sulfur carried in tail gas, SO
2all H is converted into Deng hydrogenation
2s, COS, CS
2hydrolysis is H
2s.Containing H
2the hydrogenation tail gas of S is cooled to 25-42 DEG C through quench tower, enters amine absorption tower, H
2s, by amine absorption, absorbs H
2cleaning of off-gas H after S
2s content generally arrives hundreds of ppm (v) tens.Absorb H
2the amine liquid (rich amine solution) of S enters regenerator and regenerates, and regenerated acidic gas mixes with sour gas, returns to thermal response section and reclaims elementary sulfur further.
Described cleaning of off-gas is introduced in alkali lye and is carried out removing H
2s process refers to be introduced in alkali lye by cleaning of off-gas, and alkali lye is NaOH or ammoniacal liquor, reaction below occurring in alkali lye:
H
2s+2NH
4oH → (NH
4)
2s+2H
2o or H
2s+2NaOH → Na
2s+2H
2o (6)
(NH
4)
2s+H
2s → 2NH
4hS or Na
2s+H
2s → 2NaHS (7)
In alkali lye, the H in purified gas
2s and alkali lye (or ammoniacal liquor) react and generate NaHS (or ammonia) or vulcanized sodium (or ammonia), make the H in purified gas
2the amount of S is lower than 5mg/m
3below.The H of organic sulfur and the trace be not hydrolyzed in catalytic converter on a small quantity is only contained in cleaning of off-gas after alkali liquor absorption
2s, introduces cleaning of off-gas after incinerator burns and discharges, SO in flue gas
2content can significantly reduce, and the amplitude that reduces is generally at 100-800mg/m
3between.
After alkali lye uses certain hour, assimilation effect can be deteriorated, and should regularly replace alkali lye or note ammonia.
Described spent lye harmless treatment refers to delivers to alkaline residue biological treatment device by spent lye or acidic water stripping device processes.
Acidic water stripping device is oil plant common apparatus.
Spent lye carries out alkaline residue biological treatment and refers to, under the effect of air and microorganism, the inorganic sulphide in spent lye is oxidized to thiosulfate, sulphite and sulfate, then through microbial degradation, make water outlet CODCr<500mg/L, reach the Con trolling index of two stage biological treatment system influent quality.
Spent lye carries out sewage stripping process and refers to spent lye steam normal heating to 124 DEG C, utilizes NH
3and H
2s dissolubility difference at different temperatures, destroys NH
3and H
2the balance of S in water, impels them to shift in vapour phase by liquid phase, containing NH
3and H
2the sour gas of S introduces sulphur unit sulphur stove Recovered sulphur again, the acid water NH after stripping
3and H
2the concentration of S in water reaches the requirement of index of purifying waste water.
In the process of sewage stripping, because the weak acid in acid water and strong acid can chemically fixed ammonia and sulphur, make it to be difficult to be gone out by stripping, injecting alkali [as NaOH] can make ammonia, ammonium sulfide and sulphur hydrogenation ammonia ratio be easier to from water stripping to sour gas, spent lye injection acid water, is reduced into free ammonia by the ammonium be fixed and free molecule state sulfide stripping is gone out.
The alkali lye used in the present invention is preferably NaOH or ammoniacal liquor, has that price is low, the feature of good absorbing effect.Naoh concentration is generally 10-40%, is preferably 20-30%; Ammonia concn is generally 3-25%, is preferably 5-15%.The absorption temperature of alkali lye is normal temperature, is generally 25-42 DEG C; Purified gas and alkali lye volume ratio are generally 1000-1:1, ensure de-after-purification tail gas H
2s content is less than 5mg/m
3.
Use Alkali absorption process sulfur recovery facility cleaning of off-gas to have good absorbing effect, simple to operate, the feature that expense is low, spent lye delivers to alkaline residue biological treatment device or acidic water stripping device, can accomplish harmless treatment, has the feature of environmental protection.By the process to sulfur recovery facility cleaning of off-gas, guarantee that in tail gas, H2S content is lower than 5mg/m3, final sulfur recovery facility smoke SO 2 concentration of emission can significantly reduce, and has significant environmental benefit.
Beneficial effect of the present invention is: 1, can make cleaning of off-gas H
2s is removed to 5mg/m
3below, SO in flue gas
2content can significantly reduce, and the amplitude that reduces is at 100-1000mg/m
3; 2, provide the processing method of spent lye, spent lye delivers to alkaline residue biological treatment device or acidic water stripping device, can accomplish harmless treatment.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is the process chart of prior art;
Wherein, 1, sour gas; 2, reacting furnace; 3, one-level converter; 4, secondary reformer; 5, Claus tail gas; 6, hydrogenation reactor; 7, quench tower; 8, amine absorption tower; 9, cleaning of off-gas; 10, regenerator; 11, regenerated acidic gas; 12, incinerator; 13, chimney; 14 alkali liquid tanks; 15, tail gas after alkali liquor absorption; 16, harmless treatment device.
Detailed description of the invention
The present invention is illustrated below in conjunction with drawings and Examples.
Embodiment 1:
Technological process as shown in Figure 1, comprise the thermal response stage, catalytic reaction stages and tail gas clean-up processing stage.
1) the thermal response stage:
Containing H
2s90(v/v) partial combustion in reacting furnace (2) of the sour gas (1) of % is converted into SO
2, at high temperature 1250 DEG C of H
2s and SO
2there is claus reaction generting element sulphur and Process Gas.Process Gas sulfur-containing compound volume content is: H
2s:6%, SO
2: 2.5%, organic sulfur: 0.5%.
2) catalytic reaction stages:
Reacting furnace tail gas enters one-level converter (the 3) (reaction condition: temperature 320 DEG C, air speed 800h of catalyst reaction section
-1) and secondary reformer (4) (reaction condition: temperature 250 DEG C, air speed 800h
-1), after Claus catalyzed conversion, reacted Claus tail gas (5) enters Tail gas cleanup unit.Claus tail gas sulfur-containing compound volume content is: H
2s:3%, SO
2: 1.5%, organic sulfur: 0.1%.
3) processing stage of tail gas clean-up:
Under the effect of Claus tail gas hydrogenation catalyst in hydrogenation reactor (6), sulfur-containing compound hydro-conversion is H
2s, is then cooled to 40 DEG C through quench tower (7), enters amine absorption tower (8); H in amine absorption hydrogenation tail gas
2s, makes cleaning of off-gas (9) H
2s content is down to 108ppm (v), cleaning of off-gas (9) is introduced alkali liquid tank (14), and in alkali liquid tank (14), the sodium hydroxide solution that concentration is 25% is housed, the absorption temperature of alkali liquid tank (14) is 30 DEG C, purified gas and alkali lye volume ratio are 500:1, de-after-purification tail gas H
2s content is 2mg/m
3, SO in flue gas can be reduced
2concentration is at 300mg/m
3above.
The device that spent lye in alkali liquid tank carries out harmless treatment is alkaline residue biological treatment device, alkaline residue index: sulfide 8000ppm, CODCr300000mg/L.Index after spent lye process: water outlet CODCr:400mg/L, ammonia nitrogen 9mg/L.
Embodiment 2:
Technological process as shown in Figure 1, comprise the thermal response stage, catalytic reaction stages and tail gas clean-up processing stage.
1) the thermal response stage:
Containing H
2s84(v/v) partial combustion in reacting furnace (2) of the sour gas (1) of % is converted into SO
2, at high temperature 1250 DEG C of H
2s and SO
2there is claus reaction generting element sulphur and Process Gas.Process Gas sulfur-containing compound volume content is: H
2s:5.7%, SO
2: 2.3%, organic sulfur: 0.4%.
2) catalytic reaction stages:
Reacting furnace tail gas enters one-level converter (the 3) (reaction condition: temperature 300 DEG C, air speed 800h of catalyst reaction section
-1) and secondary reformer (4) (reaction condition: temperature 250 DEG C, air speed 800h
-1), after Claus catalyzed conversion, reacted Claus tail gas (5) enters Tail gas cleanup unit.Claus tail gas sulfur-containing compound volume content is: H
2s:2.8%, SO
2: 1.3%, organic sulfur: 0.1%.
3) processing stage of tail gas clean-up:
Under the effect of Claus tail gas hydrogenation catalyst in hydrogenation reactor (6), sulfur-containing compound hydro-conversion is H
2s, is then cooled to 40 DEG C through quench tower (7), enters amine absorption tower (8); H in amine absorption hydrogenation tail gas
2s, makes cleaning of off-gas (9) H
2s content is down to 76ppm (v), cleaning of off-gas (9) is introduced alkali liquid tank (14), and alkali liquid tank (14) is equipped with the sodium hydroxide solution that concentration is 40%, and the absorption temperature of alkali liquid tank (14) is 35 DEG C, purified gas and alkali lye volume ratio are 600:1, de-after-purification tail gas H
2s content is 1mg/m
3, SO in flue gas can be reduced
2concentration is at 200mg/m
3above.
The device that spent lye in alkali liquid tank carries out harmless treatment is acidic water stripping device, alkaline residue index: sulfide 10000ppm, CODCr280000mg/L.Index after spent lye process: water outlet CODCr260mg/L, ammonia nitrogen 6.5mg/L.
Embodiment 3:
Divided by outside lower difference, other are with embodiment 2.
3) processing stage of tail gas clean-up:
Alkali liquid tank (14) is equipped with the sodium hydroxide solution that concentration is 10%, de-after-purification tail gas H
2s content is 4mg/m
3.
The device that spent lye in alkali liquid tank carries out harmless treatment is alkaline residue biological treatment device: alkaline residue index: sulfide 8000ppm, CODCr300000mg/L.Index after spent lye process: water outlet CODCr:420mg/L, ammonia nitrogen 9mg/L.
Embodiment 4:
Divided by outside lower difference, other are with embodiment 2.
3) processing stage of tail gas clean-up:
Alkali liquid tank (14) is equipped with the sodium hydroxide solution that concentration is 20%, and purified gas and alkali lye volume ratio are 100:1, de-after-purification tail gas H
2s content is 1mg/m
3.
The device that spent lye in alkali liquid tank carries out harmless treatment is alkaline residue biological treatment device, alkaline residue index: sulfide 10000ppm, CODCr300000mg/L.Index after spent lye process: water outlet CODCr410mg/L, ammonia nitrogen 8mg/L.
Embodiment 5:
Divided by outside lower difference, other are with embodiment 2.
3) processing stage of tail gas clean-up:
Alkali liquid tank (14) is equipped with the sodium hydroxide solution that concentration is 30%, and purified gas and alkali lye volume ratio are 1000:1, de-after-purification tail gas H
2s content is 4mg/m
3.
The device that spent lye in alkali liquid tank carries out harmless treatment is acidic water stripping device, alkaline residue index: sulfide 2000ppm, CODCr15000mg/L.Index after spent lye process: water outlet CODCr:120mg/L, ammonia nitrogen 5mg/L.
Embodiment 6:
According to embodiment 5 technological process and operating condition, the sodium hydroxide solution of alkali liquid tank is replaced by the ammoniacal liquor that concentration is 5%, de-after-purification tail gas H
2s content is 6mg/m
3.
Embodiment 7:
According to embodiment 6 technological process and operating condition, ammonia concn in alkali liquid tank is increased to 15%, de-after-purification tail gas H
2s content is 3mg/m
3.
Comparative example:
Technological process as shown in Figure 2.This technique contains thermal response section, catalyst reaction section and tail gas clean-up processing section.
1) the thermal response stage:
Containing H
2s90(v/v) partial combustion in reacting furnace (2) of the sour gas (1) of % is converted into SO
2, at high temperature 1250 DEG C of H
2s and SO
2there is claus reaction generting element sulphur and Process Gas.Process Gas sulfur-containing compound volume content is: H
2s:6%, SO
2: 2.5%, organic sulfur: 0.5%.
2) catalytic reaction stages:
Reacting furnace tail gas enters one-level converter (the 3) (reaction condition: temperature 320 DEG C, air speed 800h of catalyst reaction section
-1) and secondary reformer (4) (reaction condition: temperature 250 DEG C, air speed 800h
-1), after Claus catalyzed conversion, reacted Claus tail gas (5) enters Tail gas cleanup unit.Claus tail gas sulfur-containing compound volume content is: H
2s:3%, SO
2: 1.5%, organic sulfur: 0.1%.
3) processing stage of tail gas clean-up:
Under the effect of Claus tail gas hydrogenation catalyst in hydrogenation reactor (6), sulfur-containing compound hydro-conversion is H
2s, is then cooled to 40 DEG C through quench tower (7), enters amine absorption tower (8); H in amine absorption hydrogenation tail gas
2s, makes cleaning of off-gas (9) H
2s content is down to 108ppm (v), and cleaning of off-gas (9) is directly introduced incinerator burning disposal, and after process, flue gas directly enters air, H in cleaning of off-gas
2s is all converted into SO after burning
2, SO in flue gas
2concentration is increased in 300mg/m
3above.
Claims (7)
1. a sulfur recovery facility purified gas treatment process, comprise the thermal response stage, catalytic reaction stages and tail gas clean-up processing stage, it is characterized in that, tail gas clean-up processing stage, cleaning of off-gas after hydrogenation reaction, quench tower cooling, amine absorption, is introduced in alkali lye and is carried out removing H by Claus tail gases that catalytic reaction stages produces successively
2s process, removes H
2discharge after tail gas after S burns; Absorb H
2the amine liquid rich amine solution of S is introduced regenerator and is regenerated, and regenerated acidic gas mixes with sour gas, returns to the thermal response stage to reclaim elementary sulfur further;
Described carrying out removes H
2spent lye after S carries out alkaline residue biological treatment or sewage stripping process.
2. sulfur recovery facility purified gas treatment process according to claim 1, it is characterized in that, the biological treatment of described alkaline residue refers to: under the effect of air and microorganism, the inorganic sulphide in spent lye is oxidized to thiosulfate, sulphite and sulfate, then through microbial degradation, water outlet is made to reach CODCr<500mg/L.
3. sulfur recovery facility purified gas treatment process according to claim 1, is characterized in that, described sewage stripping process refers to: after being mixed with acid water by spent lye, enter acidic water stripping device, and the balance in water, impels NH
3and H
2s is shifted to vapour phase by liquid phase, containing NH
3and H
2the sour gas of S introduces sulphur unit sulphur stove Recovered sulphur again.
4. sulfur recovery facility purified gas treatment process according to claim 1, is characterized in that, described purified gas and alkali lye volume ratio are 1-1000:1.
5. the sulfur recovery facility purified gas treatment process according to claim 1 or 4, is characterized in that, the sodium hydroxide solution of described alkali lye to be concentration be 10-40%.
6. the sulfur recovery facility purified gas treatment process according to claim 1 or 4, is characterized in that, the ammonia spirit of described alkali lye to be concentration be 3-25%.
7. the sulfur recovery facility purified gas treatment process according to claim 1 or 4, is characterized in that, the reaction temperature of described alkali lye and purified gas is 25-42 DEG C.
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| CN106586972A (en) * | 2015-10-15 | 2017-04-26 | 中国石油化工股份有限公司 | Energy-saving, environmental-protection and low-emission sulfur recovery process |
| CN107315845A (en) * | 2016-06-12 | 2017-11-03 | 中国石油化工股份有限公司 | Sulphur unit tail gas method up to standard |
| CN107500253A (en) * | 2017-09-08 | 2017-12-22 | 中冶焦耐(大连)工程技术有限公司 | A kind of claus tail-gas clean-up technique |
| CN107537302A (en) * | 2016-06-29 | 2018-01-05 | 中国石油化工股份有限公司 | Sulfur recovery facility tail gas from absorption tower handling process and its absorbing liquid used |
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| 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 |
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