CN101791517A - Method for recycling sulfur from acid gases containing hydrogen sulfide - Google Patents
Method for recycling sulfur from acid gases containing hydrogen sulfide Download PDFInfo
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- CN101791517A CN101791517A CN201010141678A CN201010141678A CN101791517A CN 101791517 A CN101791517 A CN 101791517A CN 201010141678 A CN201010141678 A CN 201010141678A CN 201010141678 A CN201010141678 A CN 201010141678A CN 101791517 A CN101791517 A CN 101791517A
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- molten sulfur
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 93
- 239000011593 sulfur Substances 0.000 title claims abstract description 92
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000007789 gas Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 73
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 29
- 239000002253 acid Substances 0.000 title abstract description 8
- 238000004064 recycling Methods 0.000 title abstract 2
- 230000008569 process Effects 0.000 claims abstract description 48
- 230000003647 oxidation Effects 0.000 claims abstract description 24
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 24
- 230000003197 catalytic effect Effects 0.000 claims abstract description 19
- 238000009833 condensation Methods 0.000 claims abstract description 16
- 230000005494 condensation Effects 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000007872 degassing Methods 0.000 claims abstract description 4
- 239000005864 Sulphur Substances 0.000 claims description 64
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 239000003054 catalyst Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 230000001105 regulatory effect Effects 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 239000003426 co-catalyst Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229920001021 polysulfide Polymers 0.000 claims description 3
- 239000005077 polysulfide Substances 0.000 claims description 3
- 150000008117 polysulfides Polymers 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 239000002912 waste gas Substances 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 239000000809 air pollutant Substances 0.000 abstract description 3
- 231100001243 air pollutant Toxicity 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000003303 reheating Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 235000001508 sulfur Nutrition 0.000 description 66
- 238000005516 engineering process Methods 0.000 description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 239000003245 coal Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 230000008901 benefit Effects 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000012495 reaction gas Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- GVGLGOZIDCSQPN-PVHGPHFFSA-N Heroin Chemical compound O([C@H]1[C@H](C=C[C@H]23)OC(C)=O)C4=C5[C@@]12CCN(C)[C@@H]3CC5=CC=C4OC(C)=O GVGLGOZIDCSQPN-PVHGPHFFSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000037396 body weight Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 239000003250 coal slurry Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 235000003642 hunger Nutrition 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000037351 starvation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
-
- 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
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Abstract
The invention relates to a method for recycling sulfur from acid gases containing hydrogen sulfide, comprising the following steps: (a) air supply; (b) acid gas pretreatment; (c) mixture; (d) primary direct catalytic oxidation; (e) primary sulfur condensation; (f) process gas reheating; (g) secondary direct catalytic oxidation; (h) secondary sulfur condensation; (i) sulfur re-separation; (j) degasification in a liquid sulfur tank; and (k) tail gas burning. When the volume concentration of H2S in the acid gases in the prior art is 1-15%, the recycle rate of sulfur can reach over 99% by the method of the invention, and the emission load of H2S in the acid gases processed by the method of the invention meets the emission requirement of Integrated Emission Standard of Air Pollutants (GB16297-1996).
Description
Technical field
The present invention relates to a kind of sulfur recovery technology, particularly a kind of technology that from the sour gas that contains hydrogen sulfide, reclaims sulphur.
Background technology
According to China's energy resource structure, China is an oil starvation, weak breath, the country of relative rich coal.Verifying in the energy reserve, the 96%th, coal, petroleum resources only account for total amount about 4%.Coal is the main force of China's energy, is that raw material system methyl alcohol and synthetic ammonia project are on the increase at present with the coal, to alleviate the pressure that petroleum resources lacks.According to China " the medium-term and long-term development plan of Coal Chemical Industry industry " (exposure draft), to 2010,2015 and the year two thousand twenty, the annual production of coal system alkene was respectively 1,400,000 tons, 5,000,000 tons and 8,000,000 tons, and 1 ton of alkene can consume 3 tons of methyl alcohol.China has the advantageous resources advantage of low-cost production fuel methanol as coal resources big country.But the environmental regulation of increasingly stringent has proposed emission request to coal gasification system methyl alcohol and synthetic ammonia installation.The Chemical Manufacture that with the coal is raw material has determined that a large amount of sour gas is arranged in the crude synthesis gas, as CO
2, H
2S, COS etc., these sour gas are disadvantageous to synthetic reaction, must before entering synthesis loop it be removed.Along with the fast development of Coal Chemical Industry industry, China has dropped into a large amount of research efforts on synthesis gas acid gas removal method and technology.In recent years, the pressing gas metallization processes, as Texaco's water coal slurry pressure gasification process, Shell fine coal pressing gas metallization processes, supporting employed process for acid gas removal mainly contains polyglycol dimethyl ether process (NHD) technology of Nan Hua company exploitation and the low-temp methanol washing process that Lu Qi, Linde Co develop.Low-temperature rectisol method and the selected solvent of NHD method are to H
2S, CO
2The selectivity absorbability is strong, CO in solvent
2Solubility is big, and required solvent internal circulating load is little, and energy consumption is lower, at sulfide and CO
2The purification process of the coal gas that content is high demonstrates advantage gradually.
But what low-temperature rectisol and NHD gas purification technique adopted all is the method for Physical Absorption, contains a large amount of CO in the regenerated acidic gas behind the solvent flashing
2With a spot of H
2S (mainly is Na with traditional alkalescence
2CO
3) the method large-scale Coal Chemical Industry development need of incompatibility of material+active carrier solution absorption+regeneration, main cause is embodied in: a. product is dark sulphur, purity is low, darker in color, selling price are low; B. operating condition is relatively harsher, the operating cost height, and labour intensity is big, needs higher cost of investment; C. operating environment is relatively poor, and environmental pollution is serious.
At present, be most widely used technology in refinery gas or the natural gas purification to reclaim sulphur in the sour gas of Crouse (Claus) technology from regeneration gas, be divided into prototype Crouse and various claus process.The prototype claus process that 19th century developed is to be based upon on the basic claus reaction, that is: SO
2+ 2H
2S=3S+2H
2O, i.e. H in the system
2S and SO
2Mol ratio be 2: 1, therefore before the Claus reactor, the Claus incinerator must be arranged, so that can be section H
2S and the O that blasts
2Reaction changes into SO
2, and incinerator will be kept the high temperature more than 1000 ℃, guarantees smooth combustion, its precondition must be the H in the sour gas
2The S volumetric concentration is greater than 25%.For H
2The S volumetric concentration is lower than the processing of 25% gas, and the Claus method just is not suitable for or is uneconomical; Another problem of prototype Claus technology is the restriction that is subjected to chemical balance, and tail gas is difficult to reach the standard of environment protection emission, must set up exhaust treatment system, and the complexity that this has just increased process has reduced the economy of technology.Sulphur output is not only operated inconvenience less than the Cross unit of 10t/d, and do not have economic implications.
In order to solve the problem that prototype Claus technology is difficult to handle light concentration gas and can not reaches environmental requirement, some claus process have been produced again.Wherein representative is listed below: low temperature selective oxidation process, rope company of Denmark Top that solution absorption-desorb enrichment adds the Clinsulf-DO technology of Crouse's SCOT technology, German Linde Co, the Selectox technology of Ba Ersen company, Dutch Comprimo Corporation's Super claus technology, French Elf Aquitaine company are the WSA technology of product with sulfuric acid.Wherein the Clinsulf-DO technology of Linde Co belongs to direct catalytic oxidation technology.Different with the prototype claus process is: claus reaction belongs to balanced reaction, and its equilibrium constant is subjected to the restriction of reaction temperature, but directly catalytic oxidation is that direct oxidation of hydrogen sulfide is the reaction of elementary sulfur and water, belongs to unidirectional response.Can in the beds of direct oxidation reactor, mend and go into air, on a kind of special catalyst with H
2S is oxidized to elemental sulfur, and this technology has been set up commercial plant, is applied to reclaim sulphur from the very high regeneration acid gas of carbon dioxide content.The Clinsulf-DO technology requires all to compare harshness, the H in sour gas to operating condition and equipment
2The S volumetric concentration was at 1%～15% o'clock, and the sulfur conversion rate of the Recovered sulphur device of the hydrogen sulfide that the Engineering Projects of domestic introduction such as Huaihe River Group Co.,Ltd remove in the NHD process for purifying gas of 180,000 tons of synthetic ammonia installations of operation in 2000 and the long celebrating gas field first gas production factory first purification plant's sulfur recovery facility is all about 90%.
Summary of the invention
Technical problem to be solved by this invention is: at the H in the sour gas in the prior art
2The S volumetric concentration was used the lower technical problem of Clinsulf-DO technology sulfur conversion rate at 1%～15% o'clock; Provide a kind of sulfur conversion rate the higher method that from the sour gas that contains hydrogen sulfide, reclaims sulphur.
The present invention is achieved through the following technical solutions: a kind of method that reclaims sulphur from the sour gas that contains hydrogen sulfide comprises the steps:
(a) air is supplied with: utilize air-blaster that air is introduced air preheater from the external world, be preheating to 240 ℃ through described air preheater and form preheated air;
(b) sour gas preliminary treatment: sour gas is introduced the sour gas separator, isolates the drop that sour gas carries, and the sour gas after separating that comes out from described sour gas separator enters the sour gas preheater, is heated to 240 ℃ through middle pressure steam;
(c) mix: according to the ratio of the amount of substance of hydrogen sulfide and the amount of substance of oxygen is that 2: 1 ratio is calculated, and respectively the sour gas that is preheating to 240 ℃ in preheated air in the described air preheater and the described sour gas preheater is fed fully to mix the back in the static mixer and form process gas;
(d) the direct catalytic oxidation of one-level: will be passed into from the process gas of static mixer in the main reactor, and be filled with Ti-base catalyst in the described main reactor, the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating first steamdrum that is connected with main reactor makes described main reactor Outlet Gas Temperature be not less than 290 ℃, avoid elemental sulfur in the condensation of the exit of described main reactor, stop up the mouth of pipe, the bottom of described main reactor is provided with the coil pipe heat-obtaining, and the temperature of control reaction makes reaction more help the generation of sulphur;
(e) one-level sulphur condensation: the process gas of coming out from described main reactor enters the one-level sulfur condenser carries out product and separates, and separates the liquid sulfur that obtains and enters the molten sulfur pond through the first molten sulfur lock hopper;
(f) process gas heats again: the process gas of coming out from described one-level sulfur condenser enters reheater, and described reheater is gas one a gas heat exchanger, will be heated to 240 ℃ from the process gas that described one-level sulfur condenser comes out;
(g) the direct catalytic oxidation of secondary: the process gas after the reheater heating is sent into auxiliary reactor and is carried out direct catalytic oxidation, is filled with Ti-base catalyst in the described auxiliary reactor, the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating second steamdrum be connected with described auxiliary reactor makes described auxiliary reactor Outlet Gas Temperature be not less than 240 ℃, avoid elemental sulfur in the condensation of the exit of described auxiliary reactor, the obstruction mouth of pipe;
(h) secondary sulphur condensation: the process gas of coming out from described auxiliary reactor enters the secondary sulfur condenser carries out product and separates, and separates the liquid sulfur that obtains and enters the molten sulfur pond through the second molten sulfur lock hopper;
(i) sulphur separates again: will send into from the process gas that described secondary sulfur condenser comes out and carry out sulphur the sulphur separator and separate, and separate the sulphur that obtains and enter the molten sulfur pond by the 3rd molten sulfur lock hopper;
(j) outgas in described molten sulfur pond: blast air by the air bubbler in described molten sulfur pond, molten sulfur fully contacts the H that makes in the molten sulfur with air
2S is oxidized to sulphur, makes remaining H simultaneously
2S separates with molten sulfur, and makes the polysulfide in the molten sulfur resolve into H
2S and sulphur, waste gas is evacuated to incinerator by steam jet ejector;
(k) tail gas calcination: the tail gas that described sulphur separator and described molten sulfur pond are discharged is introduced in the described incinerator and in described incinerator and is imported air, carries out calcination under the situation of 700 ℃ and air excess.
The above-mentioned method that reclaims sulphur from the sour gas that contains hydrogen sulfide, described Ti-base catalyst comprises TiO
2, binding agent and co-catalyst, specific area is greater than 100m
2/ g, pore volume be more than or equal to 0.2ml/g, average crushing strength greater than 80 newton/, bulk density is 0.95～1.05Kg/L.
The method that reclaims sulphur from the sour gas that contains hydrogen sulfide of the present invention has following beneficial technical effects: (1) is at H in the prior art
2The S volumetric concentration is at 1%～15% sour gas, the method that reclaims sulphur from the sour gas that contains hydrogen sulfide of the present invention can make the rate of recovery of sulphur reach more than 99%, through the sour gas that the method that reclaims sulphur from the sour gas that contains hydrogen sulfide of the present invention is handled, H
2The discharge capacity of S reaches " discharge standard of air pollutants " emission request (GB16297-1996), and reasonable in design, easy for installation, stable.(2) technological process is simple, and is easy to operate, and the equipment structure is few, and gross investment economizes.(3) public work consumption is little, and operating cost is low.(4) the manufacturing material is durable in use, and regular maintenance is convenient.(5) by-product sulfur purity height, economic benefit is obvious.(6) the recyclable utilization of byproduct steam realizes resource circulation economy, energy-saving and emission-reduction.(7) capital equipment in the technology---the direct catalyst oxidation reactor heat exchange efficiency of two-stage height.
Description of drawings
Fig. 1 reclaims the molten sulfur pond degasification technique schematic diagram of the method for sulphur from the sour gas that contains hydrogen sulfide for the present invention;
Fig. 2 reclaims the method flow diagram of sulphur from the sour gas that contains hydrogen sulfide for the present invention.
Wherein: 1-air preheater, 2-boiler feedwater mouth, 3-sour gas separator; 4-sour gas preheater, 5-static mixer, 6-main reactor; 7-first steamdrum, 8-one-level sulfur condenser, 9-reheater; 10-sulphur separator, 11-auxiliary reactor, 12-second steamdrum; 13-secondary sulfur condenser, the 14-first molten sulfur lock hopper, 15-molten sulfur pond; the 16-second molten sulfur lock hopper; 17-the 3rd molten sulfur lock hopper, 18-incinerator, 19-steam jet ejector; the outlet of 20-low-pressure steam; 21-air supply port, 22-nitrogen supply port, 23-sour gas inlet; 24-middle pressure steam supply port; 25-extinguish steam inlet, 26-purging air inlet, 27-sulphur comminutor; the 28-liquid sulfur pump, 30-molten sulfur lock hopper.
Embodiment
The method that reclaims sulphur from the sour gas that contains hydrogen sulfide of present embodiment comprises the steps: the supply of (a) air: utilize air-blaster that air is introduced air preheater 1 from the external world, be preheating to 240 ℃ through described air preheater 1 and form preheated airs; (b) sour gas preliminary treatment: sour gas is introduced sour gas separator 3, isolate the drop that sour gas carries, the sour gas after separating that comes out from described sour gas separator 3 enters sour gas preheater 4, is heated to 240 ℃ through middle pressure steam; (c) mix: according to the ratio of the amount of substance of hydrogen sulfide and the amount of substance of oxygen is that 2: 1 ratio is calculated, and respectively the sour gas that is preheating to 240 ℃ in preheated air in the described air preheater 1 and the described sour gas preheater 4 is fed fully to mix the back in the static mixer 5 and form process gas; The flow of air is to determine that according to the desired amount of oxygen of chemical reaction the flow size is regulated control by control valve by DCS by the sour gas body weight sulfide hydrogen amount of the flow of sour gas and assay determination; (d) the direct catalytic oxidation of one-level: will be passed into from the process gas of described static mixer 5 in the main reactor 6, and be filled with Ti-base catalyst in the described main reactor 6, the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating first steamdrum 7 that is connected with main reactor 6 makes described main reactor 6 Outlet Gas Temperatures be not less than 290 ℃, avoid elemental sulfur in the condensation of the exit of described main reactor 6, stop up the mouth of pipe, the bottom of described main reactor 6 is provided with the coil pipe heat-obtaining, and the temperature of control reaction makes reaction more help the generation of sulphur; Total chemical reaction is hydrogen sulfide and oxygen reaction generation sulphur and water in the described main reactor 6, and the heat that reaction produces improves the temperature of self and utilizes interior cold water heat exchange; Establish beds in the described main reactor 6, top is the high speed reaction zone, and the bottom adds heat production coil pipe.During reaction, reaction heat makes bed temperature rapid rising the in top add fast response, organic sulfur is transformed also can obtain higher reaction rate.Reactor lower part makes it higher conversion ratio through effectively controlling temperature after the cooling, and reactor coil pipe layout is more reasonable, has increased powerful heat exchange efficiency.In order to guarantee security, take following measure making main reactor: joint for pipe carries out except that each weld bond with argon arc welding welding back 100%X illumination penetrates, each root pipe is carried out the superpower water pressure test (design operation pressure 3 times), and it is 2 times of operating pressure that integral body is finished the back water pressure test; The temperature that temperature that can be by regulating the coil pipe feedwater and consumption are regulated described main reactor 6 internal upper part heat insulation layers and bottom isothermal layer can move reaction towards the direction that sulphur generates, and has avoided the molten sulfurs in the described main reactor 6 to generate again to greatest extent; (e) one-level sulphur condensation: the process gas of coming out from described main reactor 6 enters one-level sulfur condenser 8 carries out product and separates, and separates the liquid sulfur that obtains and enters molten sulfur pond 15 through the first molten sulfur lock hopper 14; Reaction gas enters the sulphur in described one-level sulfur condenser 8 refrigerating gases and the condensed gas, the pipe of described one-level sulfur condenser 8 produces low-pressure steam outward, the pressure of steam regulation is regulated the outlet temperature of tube side, sulphur condensation in the gas is got off, can not be lower than the freezing point of sulphur again and make line clogging; The low-pressure steam that described one-level sulfur condenser 8 produces can be recycled; (f) process gas heats again: the process gas of coming out from described one-level sulfur condenser 8 enters reheater 9, and described reheater 9 is gas one a gas heat exchanger, will be heated to 240 ℃ from the process gas that described one-level sulfur condenser 8 comes out; (g) the direct catalytic oxidation of secondary: the process gas after reheater 9 heating is sent into auxiliary reactor 11 and is carried out direct catalytic oxidation, is filled with Ti-base catalyst in the described auxiliary reactor 11, the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating second steamdrum 12 that is connected with described auxiliary reactor 11 makes described auxiliary reactor 11 Outlet Gas Temperatures be not less than 240 ℃, avoid elemental sulfur in the condensation of the exit of described auxiliary reactor 11, stop up the mouth of pipe; Total chemical reaction is hydrogen sulfide and oxygen reaction generation sulphur and water in the described auxiliary reactor 11, and the heat that reaction produces improves the temperature of self and utilizes interior cold water heat exchange; Being provided with of described auxiliary reactor 11 one is that working conditions change is played regulating action; The 2nd, share part sulfur recovery function; The 3rd, the flexibility of raising system and the system of assurance sulphur recovery efficiency; Described auxiliary reactor 11 principles, structure, use catalyst and described main reactor 6 are similar, and volume is less than described main reactor 6; (h) secondary sulphur condensation: the process gas of coming out from described auxiliary reactor 11 enters secondary sulfur condenser 13 carries out product and separates, and separates the liquid sulfur that obtains and enters molten sulfur pond 15 through the second molten sulfur lock hopper 16; Reaction gas enters the sulphur in described secondary sulfur condenser 13 refrigerating gases and the condensed gas, the pipe of described secondary sulfur condenser 13 produces low-pressure steam outward, the pressure of steam regulation is regulated the outlet temperature of tube side, sulphur condensation in the gas is got off, can not be lower than the freezing point of sulphur again and make line clogging; The low-pressure steam that described secondary sulfur condenser 13 produces can be recycled; (i) sulphur separates again: will send into from the process gas that described secondary sulfur condenser 13 comes out and carry out sulphur the sulphur separator 10 and separate, and separate the sulphur that obtains and enter molten sulfur pond 15 by the 3rd molten sulfur lock hopper 17; (j) degassing in described molten sulfur pond 15: in described molten sulfur pond 15, blast air by the air bubbler, molten sulfur fully contacts the H2S that makes in the molten sulfur with air and is oxidized to sulphur, remaining H2S is separated with molten sulfur, and making the polysulfide in the molten sulfur resolve into H2S and sulphur, waste gas is evacuated to incinerator 18 by steam jet ejector 19; (k) tail gas calcination: the tail gas that described sulphur separator (14) and described molten sulfur pond 15 discharged is introduced in the described incinerator 18 and in described incinerator 18 and is imported air, carries out calcination under the situation of 700 ℃ and air excess; The high-temperature gas that incinerator produces is taken its most of heat away with waste heat boiler earlier, takes after-heat away with steam superheater again, and the flue gas that is cooled to 300 ℃ is discharged into atmosphere by chimney.In the present embodiment, described Ti-base catalyst comprises TiO
2, binding agent and co-catalyst, specific area is greater than 100m
2/ g, pore volume be more than or equal to 0.2mL/g, average crushing strength greater than 80 newton/, bulk density is 0.95～1.05kg/L.H in sour gas
2The S volumetric concentration was greater than 6% o'clock, the adiabatic temperature rise of cooling bed can be above 400 ℃～450 ℃ in the described main reactor 6, in order to prevent corrosion and to keep Crouse's balance, can reduce H by the exit gas of described one-level sulfur condenser 8 partly being circulated to the import of described main reactor 6
2The concentration of S inlet is so that the temperature rise of limiting catalyst bed.
The method that reclaims sulphur from the sour gas that contains hydrogen sulfide of present embodiment adopts concentrates instrument, carries out centralized Control in the DCS control room, at H in the prior art
2The S volumetric concentration can make the rate of recovery of sulphur reach more than 99% at 1%～15% sour gas, through the sour gas that the method that reclaims sulphur from the sour gas that contains hydrogen sulfide of present embodiment is handled, H
2The discharge capacity of S reaches " discharge standard of air pollutants " emission request (GB16297-1996), and reasonable in design, easy for installation, stable.And technological process is simple, and is easy to operate, and the equipment structure is few, and gross investment economizes; Public work consumes little, and operating cost is low; The manufacturing material is durable in use, and regular maintenance is convenient; By-product sulfur purity height, economic benefit is obvious; The recyclable utilization of byproduct steam realizes resource circulation economy, energy-saving and emission-reduction; Capital equipment in the technology---the direct catalyst oxidation reactor heat exchange efficiency of two-stage height.
Claims (2)
1. a method that reclaims sulphur from the sour gas that contains hydrogen sulfide is characterized in that, comprises the steps:
(a) air is supplied with: utilize air-blaster that air is introduced air preheater (1) from the external world, be preheating to 240 ℃ through described air preheater (1) and form preheated air;
(b) sour gas preliminary treatment: sour gas is introduced sour gas separator (3), isolate the drop that sour gas carries, the sour gas after separating that comes out from described sour gas separator (3) enters sour gas preheater (4), is heated to 240 ℃ through middle pressure steam;
(c) mix: according to the ratio of the amount of substance of hydrogen sulfide and the amount of substance of oxygen is that 2: 1 ratio is calculated, and respectively the sour gas that is preheating to 240 ℃ in preheated air in the described air preheater (1) and the described sour gas preheater (4) is fed fully to mix the back in the static mixer (5) and form process gas;
(d) the direct catalytic oxidation of one-level: will be passed into from the process gas of described static mixer (5) in the main reactor (6), described main reactor is filled with Ti-base catalyst in (6), the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating first steamdrum (7) that is connected with main reactor (6) makes described main reactor (6) Outlet Gas Temperature be not less than 290 ℃, avoid the exit condensation at described main reactor (6) of elemental sulfur, stop up the mouth of pipe, the bottom of described main reactor (6) is provided with the coil pipe heat-obtaining, and the temperature of control reaction makes reaction more help the generation of sulphur;
(e) one-level sulphur condensation: the process gas of coming out from described main reactor (6) enters one-level sulfur condenser (8) carries out product and separates, and separates the liquid sulfur that obtains and enters molten sulfur pond (15) through the first molten sulfur lock hopper (14);
(f) process gas heats again: the process gas of coming out from described one-level sulfur condenser (8) enters reheater (9), and described reheater (9) is gas one a gas heat exchanger, will be heated to 240 ℃ from the process gas that described one-level sulfur condenser (8) comes out;
(g) the direct catalytic oxidation of secondary: the process gas after reheater (9) heating is sent into auxiliary reactor (11) and is carried out direct catalytic oxidation, and described auxiliary reactor is filled with Ti-base catalyst in (11), the H in the process gas
2S and airborne O
2Carry out direct catalytic oxidation, reaction generates elemental sulfur and water, the pressure of regulating second steamdrum (12) that is connected with described auxiliary reactor (11) makes described auxiliary reactor (11) Outlet Gas Temperature be not less than 240 ℃, avoid the exit condensation at described auxiliary reactor (11) of elemental sulfur, stop up the mouth of pipe;
(h) secondary sulphur condensation: the process gas of coming out from described auxiliary reactor (11) enters secondary sulfur condenser (13) carries out product and separates, and separates the liquid sulfur that obtains and enters molten sulfur pond (15) through the second molten sulfur lock hopper (16);
(i) sulphur separates again: will send into from the process gas that described secondary sulfur condenser (13) comes out and carry out sulphur the sulphur separator (10) and separate, and separate the sulphur that obtains and enter molten sulfur pond (15) by the 3rd molten sulfur lock hopper (17);
(j) degassing in described molten sulfur pond (15): blast air by the air bubbler in described molten sulfur pond (15), molten sulfur fully contacts the H that makes in the molten sulfur with air
2S is oxidized to sulphur, makes remaining H simultaneously
2S separates with molten sulfur, and makes the polysulfide in the molten sulfur resolve into H
2S and sulphur, waste gas is evacuated to incinerator (18) by steam jet ejector (19);
(k) tail gas calcination: the tail gas that described sulphur separator (14) and described molten sulfur pond (15) are discharged is introduced in the described incinerator (18) and import air to described incinerator (18) in, carries out calcination under 700 ℃ of situations with air excess.
2. the method that reclaims sulphur from the sour gas that contains hydrogen sulfide according to claim 1 is characterized in that described Ti-base catalyst comprises TiO
2, binding agent and co-catalyst, specific area is greater than 100m
2/ g, pore volume be more than or equal to 0.2mL/g, average crushing strength greater than 80 newton/, bulk density is 0.95～1.05kg/L.
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| CN110605109B (en) * | 2018-06-14 | 2022-05-10 | 中国石油天然气股份有限公司 | Catalyst, preparation method and application process for waste gas treatment of liquid sulfur degassing process |
| US10953365B2 (en) | 2018-07-20 | 2021-03-23 | Jiangnan Environmental Protection Group Inc. | Acid gas treatment |
| US11529584B2 (en) | 2018-07-20 | 2022-12-20 | Jiangnan Environmental Protection Group Inc. | Acid gas treatment |
| US11224838B2 (en) | 2019-12-26 | 2022-01-18 | Jiangnan Environmental Protection Group Inc. | Controlling aerosol production during absorption in ammonia-based desulfurization |
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