CN105314607A - Low-sulfur discharging and sulfur recycling process of intermediate concentration acid gas - Google Patents

Low-sulfur discharging and sulfur recycling process of intermediate concentration acid gas Download PDF

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CN105314607A
CN105314607A CN201510865912.XA CN201510865912A CN105314607A CN 105314607 A CN105314607 A CN 105314607A CN 201510865912 A CN201510865912 A CN 201510865912A CN 105314607 A CN105314607 A CN 105314607A
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sulfur
gas
adsorption
elemental sulfur
spleen
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CN105314607B (en
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胡文宾
崔国栋
王强
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SHANDONG XUNDA CHEMICAL GROUP CO Ltd
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SHANDONG XUNDA CHEMICAL GROUP CO Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
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    • Y02P20/584—Recycling of catalysts

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Abstract

The invention provides a low-sulfur discharging and sulfur recycling process of intermediate concentration acid gas. A purpose of desulphurizing low-concentration acid gas with H2S content of 5 to 20 percent can be achieved by treating the low-sulfur acid gas by virtue of a direct oxidation reactor, a selective oxidation reactor and two adsorption desulphurization towers which can be connected in series and parallel; the direct oxidation reactor is filled with a TiO2 sulfur recycling catalyst, the selective oxidation reactor is filled with a H2S selective oxidation catalyst, catalysts in the direct oxidation reactor and selective oxidation reactor are packed in multiple layers, an air inlet and a cooling coil pipe are respectively arranged between two layers, and the adsorption desulphurization tower is filled with a thermally-renewable catalytic oxidation adsorption desulphurization agent; by selecting the appropriate catalyst and desulphurization agent and precisely controlling the process condition of each step, the total sulfur contained in the process discharged gas is that SO2 content is less than or equal to 10mg/m<3>. By virtue of thermal regeneration, the service life of the catalytic oxidation adsorption desulphurization agent is greatly prolonged, and the desulphurization amount of the catalytic oxidation adsorption desulphurization agent is greatly increased. The process has the advantages of low sulfur emission, high sulfur recycling rate (approximate to 100 percent), long service life and large desulphurization amount of the desulphurization agent, fewer replacement times, less expense, good desulphurization agent removal and scrapping condition, safety and the like.

Description

The low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas
Technical field
The present invention relates to a kind of recovery technology of sulfur, be specifically related to a kind of low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas.
Background technology
In petrochemical complex, Coal Chemical Industry, coal gasification course, a part of sulphur contained by raw material can change into H usually 2s, is formed containing H through being separated 2the sour gas of S, this sour gas generally processes through recovery technology of sulfur, by H 2s is converted into elemental sulfur as much as possible.
, in operation process, also there is emptying tail gas and solid waste two problems in described recovery technology of sulfur device.Through the tail gas that chimney is emptying, wherein, SO 2concentration is continuous monitoring project, although the higher limit of existing discharge standard of air pollutants GB16297-1996 is as 700mg/m 3be not difficult to reach, but also may there is more strict emission standard in place industry or location; H 2s is one of odor pollution material included by emission standard for odor pollutants GB14554-93, and emission limit is more strict, the accurate higher limit of factory's boundary mark as three grades be 0.45/0.80mg/m 3, 100 meters of smoke stack emission amount higher limits are 14kg/h.The useless agent that mainly multiple catalysts used, sorbent material drew off after losing efficacy in sulfur recovery facility of described solid waste, due to this kind of useless agent kind, complicated component, not only intractability is large, also exist scrap, transport, a series of environmental pollution of processing and legal risk.
Industrial to H 2the intermediate concentration sour gas of S content 5-20%, by comprise direct oxidation, selective oxidation, oxidation-adsorption combination sulfur removal technology process, H 2s is converted into sulphur, and its principal reaction is:
Generate SO in addition 2side reaction:
S+O 2→SO 2(3)
In this technique, direct oxidation reactor is by the H of the overwhelming majority 2s is converted into elemental sulfur, and selective oxidation reaction device will remain most H 2s is converted into elemental sulfur, and catalyzed oxidation adsorption desulfurize tower is by remaining H 2s is converted into elemental sulfur, by suitably controlling the operational conditions such as the oxygen-supplying amount of each reactor and temperature, the tail gas total sulfur content after desulfurization can be made to reach GB16297-1996 country emission request, emptying by chimney.
But in practice, by the restriction of catalyst reaction performance and technology controlling and process level, the emptying tail gas of this technique, although can reach GB16297-1996 to SO 2the requirement of upper limit of concentration value, GB14554-93 are to H 2the requirements such as S upper limit of concentration value and quantity discharged, but differ and reach the requirement of the existing more strict emission standard of place industry or location surely, such as reaching emptying tail gas total sulfur folding is SO 2≤ 10mg/m 3requirement, its major cause is direct oxidation reactor, the performance of the tectonic sieving of selective oxidation reaction device and catalyzed oxidation adsorption desulfurize tower, catalyzer and sweetening agent, process regulation exist needs improvements.
Summary of the invention
For overcoming above-mentioned technological deficiency, the invention provides a kind of low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas, H 2the intermediate concentration sour gas of S content 5-20%, through a direct oxidation reactor, a selective oxidation reaction device and two can the adsorption desulfurize tower process of parallel-series, reach desulfurization object;
Wherein, direct oxidation reactor charge TiO 2catalyst for recovering sulfur, catalyst reactor divides multilayer to load, and interlayer establishes gas inlet and temperature-reducing coil, the O that this catalyzer utilizes air to introduce 2by the most of H in sour gas 2s selective oxidation is elemental sulfur, and by product is a small amount of SO 2;
Selective oxidation reaction device filling Fe 2o 3/ silicon oxide selectivity oxidation H 2s catalyzer, catalyst reactor divides multilayer to load, and interlayer establishes gas inlet and temperature-reducing coil, and this catalyzer is by part SO 2and H 2s reaction is converted into elemental sulfur, and the O utilizing air to introduce 2by the most of H in Process Gas 2s selective oxidation is elemental sulfur;
The filling of adsorption desulfurize tower can the catalytic oxidation adsorption desulfurizer of hot recycling, and entrance allocates appropriate air into, by micro-elemental sulfur absorption contained by Process Gas, by the SO of contained minute quantity 2with contained H 2s is converted into elemental sulfur and adsorbs, by the H of remnants 2s is oxidized to elemental sulfur and is adsorbed in endoporus; The desulfurization precision folding of described catalytic oxidation adsorption desulfurizer is SO 2≤ 10mg/m 3, in thionizer entirety, the Sulfur capacity when this desulfurization precision>=100g sulphur/1000g sweetening agent; Purge with 250-300 DEG C of indifferent gas during hot recycling, after sulphur evaporative removal, catalyzed oxidation adsorption desulfurize performance is recovered substantially, is SO at guarantee desulfurization precision folding 2≤ 10mg/m 3condition under, through repeatedly hot recycling reach first Sulfur capacity 3-5 doubly more than total desulfurization amount;
Described recovery technology of sulfur comprises the steps:
1) sour gas and and measure allocate into air, mixing after, heater via is preheating to 180 ~ 200 DEG C, enters direct oxidation reactor by top, and between catalyst layer, entrance sprays into the air of metering; Regulate air capacity and the coil pipe cooling degree of each bed, control upper part bed temperature 200-300 DEG C, lower part bed temperature 300-350 DEG C; Control air total amount and the amount of allocating at each entrance, make the middle H that works off one's feeling vent one's spleen 2the volume content 1.0-2.0% of S, SO 2volume content≤0.20%, not containing COS, CS 2, mercaptan, the organosulfur such as thioether; Work off one's feeling vent one's spleen and enter the first condenser, be cooled to 140-160 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
2) the first condenser overhead is worked off one's feeling vent one's spleen, and measures the air mixed allocated into, and after heater via is preheating to 180 ~ 210 DEG C, enter selective oxidation reaction device by top, between catalyst layer, entrance sprays into the air of metering; Regulate air capacity and the coil pipe cooling degree of each bed, control bed temperature 200-230 DEG C, by most of H 2s selective oxidation is elemental sulfur, makes the middle H that works off one's feeling vent one's spleen 2the volume content 0.10-0.20% of S, SO 2volume content≤0.04%; Work off one's feeling vent one's spleen and enter the second condenser, be cooled to 140-160 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
3) the second condenser overhead is worked off one's feeling vent one's spleen, then is cooled to after 40-60 DEG C of remove portion water and the condensation of residue elemental sulfur through the 3rd condenser, and measures the air mixed allocated into, enters adsorption desulfurize tower, carry out desulfurization process by top; Adsorption desulfurize tower works off one's feeling vent one's spleen total sulfur folding for SO 2≤ 10mg/m 3, emptying through chimney;
4) when adsorption desulfurize tower exit procedure gas total sulfur folding is SO 2soon more than 10mg/m 3time, this adsorption desulfurize tower cuts out, and carries out in-situ heat regeneration with 250-300 DEG C of indifferent gas, after hot recycling completes, be cooled to less than 80 DEG C for subsequent use, or without cooling namely incision carry out desulfurization; Reactivation outlet gas is mixed into the second condenser with working off one's feeling vent one's spleen from selective oxidation reaction device, be cooled to 140-160 DEG C, elemental sulfur condensation separation in gas mixture enters Molten sulphur groove, the gas mixture of removing elemental sulfur is again after the 3rd condenser, the second online adsorption desulfurize tower process, emptying through chimney again, the emptying tail gas total sulfur folding of thionizer regeneration period is SO 2≤ 10mg/m 3.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, catalytic oxidation adsorption desulfurizer can adopt Na 2cO 3/ gac, NaOH/ gac, K 2cO 3/ gac, KOH/ gac, Fe 2o 3/ gac, Na 2cO 3/ aluminum oxide, K 2cO 3/ aluminum oxide, Fe 2o 3/ aluminum oxide, Fe 2o 3one or more in/silicon oxide and ferric oxide desulfurizer, all can reach the desulfurization precision of total sulfur≤10ppm.Fill whole sweetening agent in thionizer, the first Sulfur capacity when this desulfurization precision >=100g sulphur/1000g sweetening agent, through 250-300 DEG C of indifferent gas repeatedly hot recycling can reach first Sulfur capacity 3-5 doubly more than total desulfurization amount.In low sulphur emissions recovery technology of sulfur of the present invention, catalytic oxidation adsorption desulfurizer used, first Sulfur capacity before total sulfur≤10ppm penetrates, preferably >=200g sulphur/1000g sweetening agent, preferably >=300g sulphur/1000g sweetening agent, more preferably >=400g sulphur/1000g sweetening agent, and through repeatedly hot recycling can reach first Sulfur capacity 3-5 doubly more than total desulfurization amount.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, adopt the catalytic oxidation adsorption desulfurizer of desulfurization precision≤5ppm, the total sulfur of emptying tail gas can be low to moderate≤5ppm, whole sweetening agent is filled in thionizer, when this desulfurization precision, first Sulfur capacity preferably >=100g sulphur/1000g sweetening agent, preferably >=200g sulphur/1000g sweetening agent, more preferably >=300g sulphur/1000g sweetening agent, and through repeatedly hot recycling can reach first Sulfur capacity 3-5 doubly more than total desulfurization amount.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, adopt the catalytic oxidation adsorption desulfurizer of desulfurization precision≤2ppm, the total sulfur of emptying tail gas can be low to moderate≤2ppm, whole sweetening agent is filled in thionizer, when this desulfurization precision, first Sulfur capacity >=100g sulphur/1000g sweetening agent, preferably >=200g sulphur/1000g sweetening agent, preferably >=300g sulphur/1000g sweetening agent, and through repeatedly hot recycling can reach first Sulfur capacity 3-5 doubly more than total desulfurization amount.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, catalytic oxidation adsorption desulfurizer used, preferred suitably prepd Na 2cO 3the Na of the 5-10% of charge capacity 2cO 3/ gac, Fe 2o 3the Fe of charge capacity 5-15% 2o 3/ gac, or with Fe 2o 3for the ferric oxide desulfurizer of main component, fill whole sweetening agent in thionizer, at desulfurization precision≤10ppm, SO 2≤ 5ppm, SO 2under the condition of≤2ppm, the first Sulfur capacity of these three kinds of sweetening agents can reach>=200g sulphur/1000g sweetening agent, and even>=300g sulphur/1000g sweetening agent, 400g sulphur/1000g sweetening agent, 500g sulphur/1000g sweetening agent, the Sulfur capacity of first Sulfur capacity more than 95% can be reached after first hot recycling, the Sulfur capacity of first Sulfur capacity more than 80% can be reached after five hot recycling, ten times regeneration after can reach first Sulfur capacity more than 65% Sulfur capacity, namely five hot recycling can reach total desulfurization amount of first Sulfur capacity more than 4 times, ten hot recycling can reach total desulfurization amount of first Sulfur capacity more than 7 times.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, catalytic oxidation adsorption desulfurizer regenerates at thionizer situ, resurgent gases can with nitrogen or superheated vapour, preferably work off one's feeling vent one's spleen with thionizer and do resurgent gases, by heater heats to 250-300 DEG C, after reactivation outlet gas gets back to selective oxidation reaction device, the second condenser is mixed into from selective oxidation reaction device Process Gas out, be cooled to 140-160 DEG C, elemental sulfur condensation separation in gas mixture enters Molten sulphur groove, the gas mixture of removing elemental sulfur is again through the 3rd condenser, the second online adsorption desulfurize tower process, emptying.The emptying tail gas total sulfur of i.e. this technique of working off one's feeling vent one's spleen of regeneration period on-line adsorption thionizer, can reach conversion for SO 2≤ 10mg/m 3,≤5mg/m 3,≤2mg/m 3level.The advantage of superheated vapour is not containing O 2, not ablation absorbent charcoal carrier in regenerative process, does not produce the SO that may need to consider process yet 2, all collect after the elemental sulfur in reactivation outlet gas and steam (water) cooling, adsorption desulfurize tower enter the flow of implication, composition do not change substantially.
With thionizer work off one's feeling vent one's spleen do resurgent gases time, suitably should control the air flow quantity of selective oxidation reaction device, the second online adsorption desulfurize tower, thionizer is worked off one's feeling vent one's spleen the O of i.e. resurgent gases 2content controls within 200ppm, otherwise O 2the SO generated is reacted with elemental sulfur 2excessive concentration, can exceed the processing power of the second online adsorption desulfurize tower; Elected when being the sweetening agent of carrier in order to gac, the O of resurgent gases 2content should control within 100ppm, to avoid the scaling loss of absorbent charcoal carrier.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, separately can establish heater element in catalyzed oxidation adsorption desulfurize tower, to improve reproduction speed.
In the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, in thionizer non-renewable period, preferably two adsorption desulfurize towers parallel operation, to alleviate bed resistance; Use before also preferably the thionizer soon regenerated being serially connected in another thionizer, to improve the desulfurization amount in a front desulfurization cycle of tower sweetening agent, thus extend regeneration period and the work-ing life of sweetening agent; Certainly, all will under the prerequisite arranging regeneration opportunity properly, when namely ensureing that a tower regenerates, another tower still can ensure desulfurization precision.
The low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas of the present invention, has the following advantages:
1) low sulphur emissions is maintained
In common sour gas, contained H 2sulfide outside S, general COS, SO that only may have trace 2, substantially can't detect more unmanageable CS 2, the TiO of COS in direct oxidation reactor of trace 2catalyst for recovering sulfur is all hydrolyzed, and thus in low sulphur emissions recovery technology of sulfur of the present invention, the process postcure thing through direct oxidation reactor, selective oxidation reaction device, adsorption desulfurize tower removes substantially, air-discharging total sulfur≤10mg/m 3.Thionizer enters implication main component and only comprises N 2, CO 2, H 2o, a small amount of O 2, a small amount of H 2s, minute quantity SO 2with micro-elemental sulfur, not containing the material that obviously can reduce above-mentioned catalytic oxidation adsorption desulfurizer regenerability, catalytic oxidation adsorption desulfurizer only carries out the reaction generating elemental sulfur, and deposit, be adsorbed in the endoporus of sweetening agent, and the high performance of the catalytic oxidation adsorption desulfurizer desulfurization precision loaded in thionizer and feature, its put into operation after long period in, i.e. sulfur recovery facility worked off one's feeling vent one's spleen by thionizer will through the emptying tail gas of chimney, it is very low containing sulphur concentration, as lower than 10mg/m 3and even, lower than 5mg/m 3, 2mg/m 3, 1mg/m 3, until emptying tail gas containing sulphur concentration close to or switch immediately after reaching this concentration value or cut out regeneration, thus continue to ensure air-discharging total sulfur≤10ppm.If containing a small amount of NH in sour gas 3, then final meeting is substantially with (NH 4) 2sO 3or (NH 4) 2sO 4mode be deposited in the catalytic oxidation adsorption desulfurizer of thionizer, only can shorten the work-ing life of sweetening agent.
2) sulfur recovery rate is bordering on 100%
In above-mentioned low sulphur emissions recovery technology of sulfur of the present invention, the H of the elemental sulfur deposited in catalytic oxidation adsorption desulfurizer in regenerative sulfur binding tower, top sweetening agent bed adsorption 2the evaporation of S, blow to the second condenser, mix with from selective oxidation reaction device Process Gas out, elemental sulfur condensation separation is entered Molten sulphur groove, and the gas mixture of removing elemental sulfur, again through the 3rd condenser, the second online adsorption desulfurize tower process, regenerates the H of desorption 2s is oxidized to elemental sulfur and deposits in the second thionizer, and tail gas is emptying through chimney.Such circulation is gone down, and in sweetening agent, comprises the elemental sulfur deposited in the sweetening agent through repeatedly regenerating, will scrapping, the H adsorbed 2s finally can be converted into sulphur, enters Molten sulphur groove, and maintains low sulphur emissions.Because air-discharging total sulfur folding is SO 2≤ 10mg/m 3and even, lower than 5mg/m 3, 2mg/m 3, 1mg/m 3, and the H of 3-5% in sour gas 2s concentration is compared, and the sulfur recovery rate of this technique is bordering on 100%, and the sulphur especially reclaimed all enters Molten sulphur groove.
3) life-span of sweetening agent is long, desulfurization amount is large, and change number of times few, expense is low
In above-mentioned low sulphur emissions recovery technology of sulfur of the present invention, as long as sour gas raw material, catalyzed oxidation adsorption desulfurize tower entrance is not containing the material that obviously may reduce above-mentioned catalytic oxidation adsorption desulfurizer regenerability, catalytic oxidation adsorption desulfurizer just only carries out the reaction generating elemental sulfur, the elemental sulfur generated also deposits, be adsorbed in the endoporus of sweetening agent, thus after 250-300 DEG C of indifferent gas hot recycling, deposition, the evaporation of absorption elemental sulfur, blow away, and the active ingredient of sweetening agent, pore structure is recovered as newly substantially, desulfurization process can be continued on for, through repeatedly hot recycling reach first Sulfur capacity 3-5 doubly more than total desulfurization amount, and even more than 10 times, thus the life-span of sweetening agent is long, desulfurization amount is large, replacing number of times is few, expense is low.
4) sweetening agent unloads agent, scraps that treatment condition are good, safety
In above-mentioned low sulphur emissions recovery technology of sulfur of the present invention, before described catalytic oxidation adsorption desulfurizer unloads agent, by manipulation of regeneration, by the elemental sulfur of deposition, the H of absorption 2a S 250-300 DEG C indifferent gas blows off, no longer containing sulphur and H 2, thus there is not obvious peculiar smell in S, sweetening agent mobility of bed is without caking, and unload agent easily, site environment is better, and safe operating conditions is better; Institute draws off not containing sulphur in waste desulfurizing agent, nonflammable in storage, transportation, can not burn and release SO 2cause environmental pollution, useless agent process is much relatively easy, and it is also comparatively simple to scrap formality.
Accompanying drawing explanation
Accompanying drawing 1,2 is the concise and to the point flow process of the present invention's low sulphur emissions recovery technology of sulfur, and wherein Fig. 1 thionizer is worked off one's feeling vent one's spleen and done resurgent gases, and Fig. 2 superheated vapour does resurgent gases.
Device numbering is followed successively by 1 direct oxidation reactor, 2 first condensers, 3 selective oxidation reaction devices, 4 second condensers, 5 the 3rd condensers, 6 Molten sulphur grooves, 7 adsorption desulfurize towers, 8 well heaters, 9 regeneration blower fans, 10 chimneys.
Embodiment
Embodiment 1
The sulfur recovery facility of a set of 10,000 tons/year, comprises a direct oxidation reactor, a selective oxidation reaction device and two can series-parallel adsorption desulfurize tower; Wherein direct oxidation reactor charge TiO 2catalyst for recovering sulfur 60m 3, catalyzer divides 6 layers of filling, and interlayer establishes gas inlet and temperature-reducing coil; Selective oxidation reaction device filling Fe 2o 3/ SiO 2selective oxidation H 2s catalyzer 60m 3, catalyzer divides 6 layers of filling, and interlayer establishes gas inlet and temperature-reducing coil; Two adsorption desulfurize towers load Na respectively 2cO 3/ activated carbon catalysis oxidation-adsorption sweetening agent 200m 3; The elementary operation condition of this device is:
1) sour gas 20000m 3/ hr, H 2s volume content 5.0%, all the other are CO mainly 2, COS≤20mg/m 3, SO 2≤ 100mg/m 3, without CS 2, with the air 2200m allocated in direct oxidation reactor 3about/hr reacts; Sour gas allocates 1000m into 3the air of about/hr, enters direct oxidation reactor by top after being preheating to 200 DEG C, all the other 1200m 3the air of about/hr is distributed by entrance between catalyst layer, and metering sprays into; Regulate air capacity and the coil pipe cooling degree of each bed, control upper part bed temperature 260-300 DEG C, lower part bed temperature 300-350 DEG C, makes the middle H that works off one's feeling vent one's spleen 2the volume content 1.0%, SO of S 2volume content 0.10%, not containing COS, CS 2, mercaptan, the organosulfur such as thioether; Work off one's feeling vent one's spleen and enter the first condenser, be cooled to 150 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
2) the first condenser overhead is worked off one's feeling vent one's spleen, the air total amount 180m allocated into 3about/hr, reacts at selective oxidation reaction device; First condenser overhead is worked off one's feeling vent one's spleen and is measured the air mixed allocated into, after heater via is preheating to 180 DEG C, enters selective oxidation reaction device by top, regulates air capacity and the coil pipe cooling degree of each bed, controls bed temperature 210 DEG C, by most of H 2s selective oxidation is elemental sulfur, and work off one's feeling vent one's spleen middle H 2the volume content 0.10%, SO of S 2volume content 0.04%; Work off one's feeling vent one's spleen and enter the second condenser, be cooled to 150 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
3) the second condenser overhead is worked off one's feeling vent one's spleen, then is cooled to after 40 DEG C of remove portion water and the condensation of residue elemental sulfur through the 3rd condenser, and 25m is allocated in metering into 3the air mixed of about/hr, enter an adsorption desulfurize tower (another does not put into operation) by top, carry out desulfurization process, the catalytic oxidation adsorption desulfurizer loaded is by SO 2and H 2s reaction is converted into elemental sulfur, by remaining H 2s is oxidized to elemental sulfur, and the elemental sulfur of generation is deposited in the endoporus of sweetening agent; Adsorption desulfurize tower works off one's feeling vent one's spleen total sulfur folding for SO 2≤ 10mg/m 3, emptying through chimney.In plant running process, adsorption desulfurize tower can't detect H in giving vent to anger 2s, SO 2other S-contained substance in addition.
This sulfur recovery facility, before operation in 1200hr, adsorption desulfurize tower can't detect H in giving vent to anger 2s and SO 2, start afterwards to detect, during 1300hr, total sulfur folding is SO 21mg/m 3, during 1400hr, total sulfur folding is SO 22mg/m 3, during 1520hr, total sulfur folding is SO 25mg/m 3, during 1700hr, total sulfur folding is SO 210mg/m 3, this adsorption desulfurize tower is cut out regeneration, and another incision puts into operation.
During the regeneration of adsorption desulfurize tower, start regeneration blower fan and interchanger, online adsorption desulfurize tower exit procedure gas is heated to 250 DEG C, in-situ heat regeneration is carried out to sweetening agent, control regeneration tolerance and be about 13000m 3/ hr, reactivation outlet gas is mixed into the second condenser with from selective oxidation reaction device Process Gas out, be cooled to 150 DEG C, elemental sulfur condensation separation in gas mixture enters Molten sulphur groove, the gas mixture of removing elemental sulfur is again after the 3rd condenser, online adsorption desulfurize tower process, a part recycles as resurgent gases, and another part is emptying through chimney; Namely be regenerated to that temperature of working off one's feeling vent one's spleen is identical with temperature in continues 20hr after 250 DEG C, stop interchanger cooling, regenerated to when being cooled to 150 DEG C, the about 100hr of regenerative process.Regeneration period, online thionizer is worked off one's feeling vent one's spleen, and namely emptying tail gas total sulfur folding is SO 2lower than 10mg/m 3, O 2content 100ppm.。
After having regenerated, thionizer incision after regeneration put into operation immediately, another cuts out for subsequent use, carries out 8 runnings and 7 regeneration continuously by above-mentioned elementary operation condition.
Following table 1 lists the total sulfur of working off one's feeling vent one's spleen of thionizer in these 8 operation process and reaches the runtime of each concentration and corresponding desulfurization amount.
In table 1 operation process, thionizer total sulfur of working off one's feeling vent one's spleen reaches the runtime of different concns and corresponding desulfurization amount
After 8th running terminates, carry out manipulation of regeneration, take out about 100L sweetening agent check from thionizer top, find that sweetening agent very easily takes out, not caking, the difference of outward appearance and new sweetening agent is not obvious, free from extraneous odour, and without efflorescence, calcination is without sulfur burning smell.Can inference, when scrapping after re-using for some time, unload agent after manipulation of regeneration, can not there is obvious peculiar smell, it is little to unload agent difficulty, and site environment is better, and safe operating conditions is better.
Embodiment 2
The sulfur recovery facility of a set of 10,000 tons/year, comprises a direct oxidation reactor, a selective oxidation reaction device and two can series-parallel adsorption desulfurize tower; Wherein direct oxidation reactor charge TiO 2catalyst for recovering sulfur 40m 3, catalyzer divides 6 layers of filling, and interlayer establishes gas inlet and temperature-reducing coil; Selective oxidation reaction device filling Fe 2o 3/ SiO 2selective oxidation H 2s catalyzer 40m 3, catalyzer divides 6 layers of filling, and interlayer establishes gas inlet and temperature-reducing coil; Two adsorption desulfurize towers load Fe respectively 2o 3/ activated carbon catalysis oxidation-adsorption sweetening agent 125m 3; The elementary operation condition of this device is:
1) sour gas 5000m 3/ hr, H 2s volume content 20%, all the other are CO mainly 2, SO 2≤ 100mg/m 3, not containing COS, CS 2, mercaptan, the organosulfur such as thioether, in direct oxidation reactor and the air 2200m allocated into 3about/hr reacts; Sour gas allocates 1000m into 3the air of about/hr, enters direct oxidation reactor by top after being preheating to 180 DEG C, all the other 1200m 3the air of about/hr is distributed by entrance between catalyst layer, and metering sprays into; Regulate air capacity and the coil pipe cooling degree of each bed, control upper part bed temperature 260-300 DEG C, lower part bed temperature 300-350 DEG C, makes the middle H that works off one's feeling vent one's spleen 2the volume content 2.0%, SO of S 2volume content 0.20%, not containing COS, CS 2, mercaptan, the organosulfur such as thioether; Work off one's feeling vent one's spleen and enter the first condenser, be cooled to 150 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
2) the first condenser overhead is worked off one's feeling vent one's spleen, the air total amount 285m allocated into 3about/hr, reacts at selective oxidation reaction device; First condenser overhead is worked off one's feeling vent one's spleen and is measured the air mixed allocated into, after heater via is preheating to 180 DEG C, enters selective oxidation reaction device by top, regulates air capacity and the coil pipe cooling degree of each bed, controls bed temperature 210 DEG C, by most of H 2s selective oxidation is elemental sulfur, and work off one's feeling vent one's spleen middle H 2the volume content 0.15%, SO of S 2volume content 0.03%; Work off one's feeling vent one's spleen and enter the second condenser, be cooled to 150 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
3) the second condenser overhead is worked off one's feeling vent one's spleen, then is cooled to after 40 DEG C of remove portion water and the condensation of residue elemental sulfur through the 3rd condenser, and 17m is allocated in metering into 3the air mixed of about/hr, enter an adsorption desulfurize tower (another does not put into operation) by top, carry out desulfurization process, the catalytic oxidation adsorption desulfurizer loaded is by SO 2and H 2s reaction is converted into elemental sulfur, by remaining H 2s is oxidized to elemental sulfur, and the elemental sulfur of generation is deposited in the endoporus of sweetening agent; Adsorption desulfurize tower works off one's feeling vent one's spleen total sulfur folding for SO 2≤ 10mg/m 3, emptying through chimney.In plant running process, adsorption desulfurize tower can't detect H in giving vent to anger 2s, SO 2other S-contained substance in addition.
This sulfur recovery facility, before operation in 1400hr, adsorption desulfurize tower can't detect H in giving vent to anger 2s and SO 2, start afterwards to detect, during 1550hr, total sulfur folding is SO 21mg/m 3, during 1700hr, total sulfur folding is SO 22mg/m 3, during 1900hr, total sulfur folding is SO 25mg/m 3, during 2050hr, total sulfur folding is SO 210mg/m 3, this adsorption desulfurize tower is cut out regeneration, and another incision puts into operation.In plant running process, adsorption desulfurize tower can't detect H in giving vent to anger 2s, SO 2other S-contained substance in addition.
During the regeneration of adsorption desulfurize tower, with steam as regeneration source of the gas, be heated to 280 DEG C, in-situ heat regeneration is carried out to sweetening agent, control quantity of steam and be about 10000m 3/ hr, reactivation outlet gas is mixed into the second condenser with from selective oxidation reaction device Process Gas out, be cooled to 150 DEG C, elemental sulfur condensation separation in gas mixture enters Molten sulphur groove, and the gas mixture of removing elemental sulfur is emptying through chimney after the 3rd condenser, online adsorption desulfurize tower process again; Continue 20hr after being regenerated to temperature 280 DEG C of working off one's feeling vent one's spleen, stop steam and regenerative heater, regeneration completes, the about 90hr of regenerative process.Regeneration period, online thionizer is worked off one's feeling vent one's spleen, and namely emptying tail gas total sulfur folding is SO 2lower than 2mg/m 3.
After having regenerated, thionizer incision after regeneration put into operation immediately, another cuts out for subsequent use, carries out 10 runnings and 9 regeneration continuously by above-mentioned elementary operation condition.
Following table 2 lists the total sulfur of working off one's feeling vent one's spleen of thionizer in these 10 operation process and reaches the runtime of each concentration and corresponding desulfurization amount.
After 10th running terminates, carry out manipulation of regeneration, take out about 100L sweetening agent check from thionizer top, find that sweetening agent very easily takes out, not caking, the difference of outward appearance and new sweetening agent is not obvious, free from extraneous odour, and without efflorescence, calcination is without sulfur burning smell.Can inference, when scrapping after re-using for some time, unload agent after manipulation of regeneration, can not there is obvious peculiar smell, it is little to unload agent difficulty, and site environment is better, and safe operating conditions is better.
In table 2 operation process, thionizer total sulfur of working off one's feeling vent one's spleen reaches the runtime of different concns and corresponding desulfurization amount

Claims (6)

1. a low sulphur emissions recovery technology of sulfur for intermediate concentration sour gas, H 2the intermediate concentration sour gas of S content 5-20%, through a direct oxidation reactor, a selective oxidation reaction device and two can the adsorption desulfurize tower process of parallel-series, reach desulfurization object;
Wherein, direct oxidation reactor charge TiO 2catalyst for recovering sulfur, catalyst reactor divides multilayer to load, and interlayer establishes gas inlet and temperature-reducing coil, the O that this catalyzer utilizes air to introduce 2by the most of H in sour gas 2s selective oxidation is elemental sulfur, and by product is a small amount of SO 2;
Selective oxidation reaction device filling Fe 2o 3/ silicon oxide selectivity oxidation H 2s catalyzer, catalyst reactor divides multilayer to load, and interlayer establishes gas inlet and temperature-reducing coil, and this catalyzer is by part SO 2and H 2s reaction is converted into elemental sulfur, and the O utilizing air to introduce 2by the most of H in Process Gas 2s selective oxidation is elemental sulfur;
The filling of adsorption desulfurize tower can the catalytic oxidation adsorption desulfurizer of hot recycling, and entrance allocates appropriate air into, by micro-elemental sulfur absorption contained by Process Gas, by the SO of contained minute quantity 2with contained H 2s is converted into elemental sulfur and adsorbs, by the H of remnants 2s is oxidized to elemental sulfur and is adsorbed in endoporus; The desulfurization precision folding of described catalytic oxidation adsorption desulfurizer is SO 2≤ 10mg/m 3, in thionizer entirety, the Sulfur capacity when this desulfurization precision>=100g sulphur/1000g sweetening agent; Purge with 250-300 DEG C of indifferent gas during hot recycling, after sulphur evaporative removal, catalyzed oxidation adsorption desulfurize performance is recovered substantially, is SO at guarantee desulfurization precision folding 2≤ 10mg/m 3condition under, through repeatedly hot recycling reach first Sulfur capacity 3-5 doubly more than total desulfurization amount;
Described recovery technology of sulfur comprises the steps:
1) sour gas and and measure allocate into air, mixing after, heater via is preheating to 180 ~ 200 DEG C, enters direct oxidation reactor by top, and between catalyst layer, entrance sprays into the air of metering; Regulate air capacity and the coil pipe cooling degree of each bed, control upper part bed temperature 200-300 DEG C, lower part bed temperature 300-350 DEG C; Control air total amount and the amount of allocating at each entrance, make the middle H that works off one's feeling vent one's spleen 2the volume content 1.0-2.0% of S, SO 2volume content≤0.20%, not containing COS, CS 2, mercaptan, the organosulfur such as thioether; Work off one's feeling vent one's spleen and enter the first condenser, be cooled to 140-160 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
2) the first condenser overhead is worked off one's feeling vent one's spleen, and measures the air mixed allocated into, and after heater via is preheating to 180 ~ 210 DEG C, enter selective oxidation reaction device by top, between catalyst layer, entrance sprays into the air of metering; Regulate air capacity and the coil pipe cooling degree of each bed, control bed temperature 200-230 DEG C, by most of H 2s selective oxidation is elemental sulfur, makes the middle H that works off one's feeling vent one's spleen 2the volume content 0.10-0.20% of S, SO 2volume content≤0.04%; Work off one's feeling vent one's spleen and enter the second condenser, be cooled to 140-160 DEG C, the elemental sulfur of generation is separated and enters Molten sulphur groove;
3) the second condenser overhead is worked off one's feeling vent one's spleen, then is cooled to after 40-60 DEG C of remove portion water and the condensation of residue elemental sulfur through the 3rd condenser, and measures the air mixed allocated into, enters adsorption desulfurize tower, carry out desulfurization process by top; Adsorption desulfurize tower works off one's feeling vent one's spleen total sulfur folding for SO 2≤ 10mg/m 3, emptying through chimney;
4) when adsorption desulfurize tower exit procedure gas total sulfur folding is SO 2soon more than 10mg/m 3time, this adsorption desulfurize tower cuts out, and carries out in-situ heat regeneration with 250-300 DEG C of indifferent gas, after hot recycling completes, be cooled to less than 80 DEG C for subsequent use, or without cooling namely incision carry out desulfurization; Reactivation outlet gas is mixed into the second condenser with working off one's feeling vent one's spleen from selective oxidation reaction device, be cooled to 140-160 DEG C, elemental sulfur condensation separation in gas mixture enters Molten sulphur groove, the gas mixture of removing elemental sulfur is again after the 3rd condenser, the second online adsorption desulfurize tower process, emptying through chimney again, the emptying tail gas total sulfur folding of thionizer regeneration period is SO 2≤ 10mg/m 3.
2. the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas as claimed in claim 1, it is characterized in that, described catalytic oxidation adsorption desulfurizer is Na 2cO 3/ gac, NaOH/ gac, K 2cO 3/ gac, KOH/ gac, Fe 2o 3one or more in/gac and ferric oxide desulfurizer.
3. the low sulphur emissions recovery technology of sulfur of intermediate concentration sour gas as claimed in claim 2, it is characterized in that, described catalytic oxidation adsorption desulfurizer is the Na of charge capacity 5-10% 2cO 3the Fe of/gac, charge capacity 5-20% 2o 3/ gac, or with Fe 2o 3for the ferric oxide desulfurizer of main component.
4. the low sulphur emissions recovery technology of sulfur of the arbitrary intermediate concentration sour gas as described in claim 1-3, is characterized in that, in thionizer non-renewable period, and the parallel operation of two adsorption desulfurize towers.
5. the low sulphur emissions recovery technology of sulfur of the arbitrary intermediate concentration sour gas as described in claim 1-3, is characterized in that, in thionizer non-renewable period, uses before the thionizer soon penetrated is serially connected in another thionizer.
6. the low sulphur emissions recovery technology of sulfur of the arbitrary intermediate concentration sour gas as described in claim 1-3, is characterized in that, separately establishes heater element in catalyzed oxidation adsorption desulfurize tower.
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