CN105347311B - H2S selective oxidations generate the process of elemental sulfur - Google Patents
H2S selective oxidations generate the process of elemental sulfur Download PDFInfo
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- CN105347311B CN105347311B CN201510814964.4A CN201510814964A CN105347311B CN 105347311 B CN105347311 B CN 105347311B CN 201510814964 A CN201510814964 A CN 201510814964A CN 105347311 B CN105347311 B CN 105347311B
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- elemental sulfur
- air
- catalyst
- selective
- temperature
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 30
- 230000003647 oxidation Effects 0.000 title claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000005864 Sulphur Substances 0.000 claims abstract description 16
- 239000011229 interlayer Substances 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 7
- -1 heater Chemical compound 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 22
- 239000010410 layer Substances 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 8
- 210000000952 spleen Anatomy 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910003978 SiClx Inorganic materials 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 22
- 229910052717 sulfur Inorganic materials 0.000 description 13
- 239000011593 sulfur Substances 0.000 description 13
- 238000011084 recovery Methods 0.000 description 11
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000019635 sulfation Effects 0.000 description 2
- 238000005670 sulfation reaction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
- C01B17/0404—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by processes comprising a dry catalytic conversion of hydrogen sulfide-containing gases, e.g. the Claus process
- C01B17/0426—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by processes comprising a dry catalytic conversion of hydrogen sulfide-containing gases, e.g. the Claus process characterised by the catalytic conversion
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Treating Waste Gases (AREA)
Abstract
The present invention provides a kind of H2S selective oxidations generate the process of elemental sulfur, including heater, selective oxidation reaction device, medium temperature condenser and low-temperature condenser, Molten sulphur groove；5 12%Fe of 30 50nm of average pore diameter are loaded in reactor2O3/ silica H2S catalyst for selective oxidation, catalyst point multilayer are loaded, and interlayer respectively sets air entrance and all the way temperature-reducing coil all the way；By each reaction bed temperature of suitable control, the supplying total amount of air and the sendout in each air intake, H will be contained2H in the process gas of S 0.5 2%2S is all aoxidized, except generating≤200 mg/m3SO2, remaining is completely converted into elemental sulfur, so that there may be more stringent discharge standard for industry where reaching or area.Present invention process is more brief, SO2Concentration of emission is relatively low, process runs well.
Description
Technical field
The present invention relates to a kind of recovery technology of sulfur method, and in particular to a kind of H2S selective oxidations generation elemental sulfur
Process.
Background technology
In petrochemical industry, coal chemical industry, coal gasification course, a part of sulphur contained by raw material would generally change into H2S, through separation
Formation contains H2The sour gas of S, the sour gas are generally handled through recovery technology of sulfur, by H2S is converted into simple substance as much as possible
Sulphur.
Recovery technology of sulfur device, during operation, the tail gas through chimney emptying, its SO2Concentration is continuous monitoring item
Mesh, although the upper limit value such as 700mg/m of existing discharge standard of air pollutants GB16297-19963It is not difficult to reach, but institute
It there is likely to be more stringent discharge standard in industry or location；H2S is emission standard for odor pollutants GB14554-
One of odor pollution material included by 93, emission limit is more stringent, and the quasi- upper limit value of factory's boundary mark such as three-level is 0.45/
0.80mg/m3, 100 meters of smoke stack emission amount upper limit values are 14kg/h.
With the raising of environmental protection standard, the requirement to recovery technology of sulfur tail gas is increasingly stringent, thus, currently processed acidity
The recovery technology of sulfur of gas, its back segment often include H2The step of S selective oxidations, will come from content in preceding step Process Gas
The H of relatively low such as 0.5-2%2S, and the O of supplying2Reaction, selective oxidation generation elemental sulfur.
H2S selective oxidation reactions, purpose product are elemental sulfur, are segregated into liquid-state sulfur groove, ultimately form sulphur production
Product；Side reaction is SO2.Usually to H in tail gas2S、SO2The requirement of content, is generally to try to be free of H2S, SO2Content is as far as possible low, because
And if selective oxidation after without other processing steps for example catalysis oxidation absorption desulfurization and etc. and directly discharge, should
In H2S selective oxidations step is by H2S is converted entirely, is converted into elemental sulfur as much as possible, while reduce SO as far as possible2Selection
Property.
H2In the reaction of S selective oxidations generation elemental sulfur, accessory substance SO is reduced2The method of selectivity, except suitable control
O2Amount of allocating and reaction temperature, also to use the larger Fe in the relatively low catalyst such as aperture of Crouse's activity2O3/ silica is urged
Agent, but ensureing H2While S is converted entirely, the prior art is not easily achieved SO2Content is less than 200mg/m3Or even 100mg/m3、
50mg/m3Level, thus there may be more stringent discharge standard for industry where being not easy to reach or area.
The content of the invention
To overcome above-mentioned technological deficiency, the present invention provides a kind of H2S selective oxidations generate the process of elemental sulfur, use
Contain H in processing2The process gas of S 0.5-2%, is ensureing H2While S is converted entirely, make SO2Content is less than 200mg/m3Or even
100mg/m3、50mg/m3, so that there may be more stringent discharge standard for industry where reaching or area.
The technical scheme is that：A kind of H2The process of S selective oxidations generation elemental sulfur, including heater,
Selective oxidation reaction device, medium temperature condenser and low-temperature condenser, Molten sulphur groove；Average pore diameter 30- is loaded in reactor
The 5-12%Fe of 50nm2O3/ silica H2S catalyst for selective oxidation, catalyst point multilayer are loaded, and interlayer respectively sets air all the way
Entrance and all the way temperature-reducing coil；Enter by each reaction bed temperature of suitable control, the supplying total amount of air and in each air
The sendout of mouth, by the H in Process Gas2S is all aoxidized, except generation≤200mg/m3SO2, remaining is completely converted into simple substance
Sulphur；
Containing H2The unstripped gas of S volume contents 0.5-2%, and the air mixing of metering supplying, heated device is preheating to 180~
After 210 DEG C, selective oxidation reaction device is entered by top, entrance sprays into the air measured between catalyst layer；Adjust each bed
Air capacity and coil pipe cooling degree, control 180-220 DEG C of middle and upper part bed temperature, 220-240 DEG C of lower part bed temperature, makes outlet
H is free of in gas2S, SO2Volume content≤200mg/m3；Work off one's feeling vent one's spleen and enter medium temperature condenser, be cooled to 140-160 DEG C, generation
Elemental sulfur be segregated into Molten sulphur groove, medium temperature condenser overhead is worked off one's feeling vent one's spleen, then is cooled to 40-60 DEG C through low-temperature condenser and is removed
After removing remaining micro elemental sulfur, emptied through chimney.
H of the present invention2In the process of S selective oxidations generation elemental sulfur, it is preferable that urged in selective oxidation reaction device
Agent divides 4-10 layers of filling, and interlayer sets 3-9 roads air intake, together with the air intake that unstripped gas is incorporated before heater, sets 4- altogether
10 road air intakes.
H of the present invention2In the process of S selective oxidations generation elemental sulfur, it is preferable that urged in selective oxidation reaction device
Air entrance set by agent interlayer, has high speed spout, and supersonic speed spout is more preferable, more preferably has per road air intake more
A branch mouth, to enable sprayed into air and Process Gas more preferably to mix faster, the high speed spout, supersonic speed spout have
The jet size to match with air straying quatity.
H of the present invention2S selective oxidations generate the process of elemental sulfur, have the following advantages：
1) technique is more brief, SO2Concentration of emission is relatively low
The 5-12%Fe of average pore diameter 30-50nm is loaded in reactor2O3/ silica H2S catalyst for selective oxidation,
And catalyst point multilayer is loaded, interlayer respectively sets air entrance and all the way temperature-reducing coil all the way；Respectively it is catalyzed by suitable control
Agent bed temperature, the supplying total amount of air and the sendout in each air intake, make reaction temperature relatively low, make O in reacting gas2
Concentration it is relatively low so that by Process Gas H2S all aoxidize while, realize relatively low SO2Yield, remaining whole
Elemental sulfur is converted into, empties SO in tail gas2Content is less than 200mg/m3Or even 100mg/m3、50mg/m3, without other sulfide,
So that there may be more stringent discharge standard for industry where reaching or area；Fe used2O3/ silicon oxide catalyst have compared with
Low Crouse's activity, is a key；
2) process runs well
Fe is loaded in reactor2O3/ silicon oxide catalyst, can give play to selective oxygen in longer operational process
Change H2S generates the stability of elemental sulfur, and reason is the stability of its silica support, the average hole of catalyst 30-50nm
Diameter and the low O of low temperature2Under the conditions of Fe2O3It is not susceptible to the property of sulfation：Silica support acid resistance, water resistance are preferable,
From H under the conditions of 180~240 DEG C of reaction temperatures2S、SO2Erosion；Catalyst has the average pore diameter of 30-50nm, makes
The liquid sulfur formed in internal gutter is less, and the blocking formed is less；In the low O of the low temperature of this process2Under the conditions of, catalysis
The Fe of agent2O3Active component can in the operation of several years less generation sulfation.
Brief description of the drawings
Attached drawing 1 is H of the present invention2The brief flow of the process of S selective oxidations generation elemental sulfur, wherein device numbering
It is followed successively by 1 heater, 2 selective oxidation reaction devices, 3 medium temperature condensers, 4 low-temperature condensers, 5 Molten sulphur grooves, 6 chimneys.
Embodiment
Embodiment 1
A set of sulfur recovery facility, including heater, selective oxidation reaction device, medium temperature condenser and low-temperature condenser,
Molten sulphur groove；Selective oxidation reaction device loads Fe2O3/ silica H2S catalyst for selective oxidation 60m3, 6 layers of catalyst point
Each dress 10m3, interlayer respectively sets air intake all the way and temperature-reducing coil, has 5 high speed spouts per road air；The Fe2O3/ oxygen
SiClx catalyst Fe2O3Content 5%, average pore diameter 50nm, shape are the column-shape strip of Ф 3x5-10mm；The basic behaviour of the device
It is as condition:
Unstripped gas 20000m3/ hr, H2S volume contents 0.5%, remaining is mainly N2、CO2, COS≤20mg/m3, without other
Sulfide, supplying air total amount 250m3/ hr or so reacts；Unstripped gas is incorporated 70m3The air of/hr or so, after being preheating to 210 DEG C
Selective oxidation reaction device, remaining 180m are entered by top3The air of/hr or so distributes between catalyst layer between 5 road entrances, meter
Amount sprays into；The air capacity and coil pipe cooling degree of each bed are adjusted, controls 3 210-220 DEG C of bed temperatures of top half, lower half
230-240 DEG C of the bed temperature in part 3, makes to be free of H in working off one's feeling vent one's spleen2S, SO2Volume content≤100mg/m3, without other sulphur
Compound；Work off one's feeling vent one's spleen and enter medium temperature condenser, be cooled to 150 DEG C, the elemental sulfur of generation is segregated into Molten sulphur groove；Medium temperature condenses
Device top exit gas, is cooled to 40 DEG C through low-temperature condenser and removes remaining micro elemental sulfur, emptied through chimney.
The sulfur recovery facility, in 1 year of operation, the sulfur recovery facility smooth running, is free of in air-discharging
H2S, SO2Volume content≤100mg/m3, the wherein most time≤50mg/m3, without other sulfide.
Embodiment 2
A set of sulfur recovery facility, including heater, selective oxidation reaction device, medium temperature condenser and low-temperature condenser,
Molten sulphur groove；Selective oxidation reaction device loads Fe2O3/ silica H2S catalyst for selective oxidation 50m3, 8 layers of catalyst point
Each dress 6.25m3, interlayer respectively sets air intake all the way and temperature-reducing coil, has 5 high speed spouts per road air；The Fe2O3/
Silicon oxide catalyst Fe2O3Content 12%, average pore diameter 30nm, shape are the column-shape strip of Ф 3x5-10mm；The device it is basic
Operating condition is:
Unstripped gas 10000m3/ hr, H2S volume contents 1.8%, remaining is mainly N2、CO2, COS≤20mg/m3, without other
Sulfide, supplying air total amount 450m3/ hr or so reacts；Unstripped gas is incorporated 100m3The air of/hr or so, after being preheating to 180 DEG C
Selective oxidation reaction device, remaining 350m are entered by top3The air of/hr or so distributes between catalyst layer between 7 road entrances, meter
Amount sprays into；The air capacity and coil pipe cooling degree of each bed are adjusted, controls 200-220 DEG C of the bed temperature in middle and upper part 5, lower part 3
A 230-240 DEG C of bed temperature, makes to be free of H in working off one's feeling vent one's spleen2S, SO2Volume content≤100mg/m3, without other sulfide；
Work off one's feeling vent one's spleen and enter medium temperature condenser, be cooled to 150 DEG C, the elemental sulfur of generation is segregated into Molten sulphur groove；Medium temperature condenser top
Portion works off one's feeling vent one's spleen, and being cooled to 60 DEG C through low-temperature condenser removes remaining micro elemental sulfur, is emptied through chimney.
The sulfur recovery facility, in 1 year of operation, the sulfur recovery facility smooth running, is free of in air-discharging
H2S, SO2Volume content≤100mg/m3, the wherein most time≤50mg/m3, without other sulfide.
Claims (5)
- A kind of 1. H2The process of S selective oxidations generation elemental sulfur, including heater, selective oxidation reaction device, medium temperature are cold Condenser and low-temperature condenser, Molten sulphur groove；The 5-12%Fe of average pore diameter 30-50nm is loaded in reactor2O3/ silica H2S catalyst for selective oxidation, catalyst point multilayer are loaded, and interlayer respectively sets air entrance and all the way temperature-reducing coil all the way；It is logical Each reaction bed temperature of suitable control, the supplying total amount of air and the sendout in each air intake are crossed, by Process Gas H2S is all aoxidized, except generating≤200 mg/m3SO2, remaining is completely converted into elemental sulfur；Containing H2S unstripped gas is in Fe2O3/ oxygen Gas hourly space velocity in SiClx catalyst bed is 200h-1；Containing H2The unstripped gas of S volume contents 0.5-2%, and the air mixing of metering supplying, heated device are preheating to 180~210 DEG C Afterwards, selective oxidation reaction device is entered by top, entrance sprays into the air measured between catalyst layer；Adjust the air capacity of each bed With coil pipe cooling degree, 180-220 DEG C of middle and upper part bed temperature is controlled, 220-240 DEG C of lower part bed temperature, makes in working off one's feeling vent one's spleen not Containing H2S, SO2The mg/m of volume content≤2003；Work off one's feeling vent one's spleen and enter medium temperature condenser, be cooled to 140-160 DEG C, the list of generation Matter sulphur is segregated into Molten sulphur groove, and medium temperature condenser overhead is worked off one's feeling vent one's spleen, then is cooled to 40-60 DEG C of removing through low-temperature condenser and remains After remaining micro elemental sulfur, emptied through chimney.
- 2. H as claimed in claim 12S selective oxidations generate the process of elemental sulfur, it is characterised in that oxidation reactor Interior catalyst divides 4-10 layers of filling, and interlayer sets 3-9 roads air intake, common together with the air intake that unstripped gas is incorporated before heater If 4-10 roads air intake
- 3. H as claimed in claim 12S selective oxidations generate the process of elemental sulfur, it is characterised in that selective oxidation Air entrance set by catalyst in reactor interlayer, has high speed spout, and the high speed spout has and air straying quatity The jet size to match.
- 4. H as claimed in claim 32S selective oxidations generate the process of elemental sulfur, it is characterised in that the high speed spray Mouth is supersonic speed spout.
- 5. any H as described in claim 1-42S selective oxidations generate the process of elemental sulfur, it is characterised in that selection Property oxidation reactor inner catalyst layer between set every road air intake there are multiple mouths.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510814964.4A CN105347311B (en) | 2015-11-23 | 2015-11-23 | H2S selective oxidations generate the process of elemental sulfur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510814964.4A CN105347311B (en) | 2015-11-23 | 2015-11-23 | H2S selective oxidations generate the process of elemental sulfur |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105347311A CN105347311A (en) | 2016-02-24 |
| CN105347311B true CN105347311B (en) | 2018-05-08 |
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| CN201510814964.4A Active CN105347311B (en) | 2015-11-23 | 2015-11-23 | H2S selective oxidations generate the process of elemental sulfur |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL2017533B1 (en) * | 2016-09-26 | 2018-04-04 | Jacobs Nederland Bv | Improved catalyst for the selective oxidation of hydrogen sulfide |
| CN106698361B (en) * | 2016-12-14 | 2019-04-05 | 山东迅达化工集团有限公司 | The recovery technology of sulfur of sour gas |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| NL8901893A (en) * | 1989-07-21 | 1991-02-18 | Veg Gasinstituut Nv | Selective oxidn. catalyst - used to oxidise sulphur cpds. partic. hydrogen sulphide to elemental sulphur |
| US7108842B2 (en) * | 2004-01-15 | 2006-09-19 | Conocophillips Company | Process for the catalytic partial oxidation of H2S using staged addition of oxygen |
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