CN106395756B - It is a kind of to handle containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carry out the novel process of sulphur recovery - Google Patents

It is a kind of to handle containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carry out the novel process of sulphur recovery Download PDF

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Publication number
CN106395756B
CN106395756B CN201610792752.5A CN201610792752A CN106395756B CN 106395756 B CN106395756 B CN 106395756B CN 201610792752 A CN201610792752 A CN 201610792752A CN 106395756 B CN106395756 B CN 106395756B
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sulphur
sulfur
sour gas
gas
hydrogen sulfide
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CN106395756A (en
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王向新
周丹黎
唐建业
张翔
尚剑
赵中
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Hualu Engineering and Technology Co Ltd
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Hualu Engineering and Technology Co Ltd
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    • 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
    • C01B17/0408—Pretreatment of the hydrogen sulfide containing gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/38—Removing components of undefined structure
    • B01D53/40—Acidic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/308—Carbonoxysulfide COS
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/406—Ammonia
    • 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
    • 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
    • Y02P20/50—Improvements relating to the production of bulk chemicals

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)

Abstract

The invention discloses a kind of processing containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carries out the novel process of sulphur recovery.Using washing except ammonia, Crouse's burning, hydrolysis, claus reaction, hydrogenation reaction, absorption oxidation reaction and the refined technique being combined of sulphur, it can be formed according to sour gas, flexibly select technological process, recycle the heat of sour gas, energy-saving and emission-reduction.This technique is applicable to the purification of various different composition sour gas, the direct qualified discharge of tail gas energy after processing, and can recycle and obtain high-quality sulphur, and sulfur recovery rate is more than 99.95%.

Description

It is a kind of to handle containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carry out the new of sulphur recovery Type technique
Technical field
The present invention relates to the field of purification of sulfide hydrogen sour gas, specially a kind of processing is containing ammonia, carbonyl sulfur, vulcanization hydracid Property gas, and carry out the novel process of sulphur recovery.
Background technology
It can all be generated in coal chemical industry process, oil and natural gas process and largely contain H2S sour gas.Such as coalification In work the H that workshop section generates is washed from low-temp methanol2The sour gas etc. that S concentrated gas, refinery come from sour water stripping (SWS) workshop section.These sour gas Middle H2S concentration has very big difference, and the impurity concentrations such as institute's cos-containing, ammonia are also different, as environmental issue becomes increasingly conspicuous, country Discharge standard is also increasingly stringenter.It carries out at this stage《Petroleum refining industry pollutant emission standard》In require SO2Especially row It puts and is limited to 100mg/m3,《Petro chemical industry pollutant emission standard》In require SO2Especially discharge is limited to 50mg/m3。
The sulfur recovery technologies such as super Claus, super excellent Crouse in presently disclosed method based on Crouse are difficult straight Existing discharge standard requirement is accessed, and Complexing Iron is used to absorb oxidation H as catalyst2The technique of S, which has, absorbs complete, tail H in gas2The features such as S contents are low, sulfur recovery rate is high, but it cannot be handled containing NH3With the sour gas of the organic sulfurs such as COS, can cause NH3It is come out in the sulfur filtration stage, and is aqueous sulphur slurry using the sulphur of Complexing Iron oxidizing process recycling, industry is not achieved Sulphur standard.
This patent offer one kind is comprehensive to be handled containing NH3With the impurity such as COS, different H2The place of the sour gas of S concentration Reason method, simultaneously can by-product high-quality sulphur in the case where exhaust emissions is up to standard.
Invention content
The purpose of this method is provided a kind of advanced to improve the shortcoming of the vulcanisation hydrogen flow of traditional sour gas Processing containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carry out the novel process of sulphur recovery, be adapted to various working and save It can emission reduction.
To achieve the above object, a kind of processing of the present invention is containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carries out sulphur recovery Novel process, the process technology scheme of use includes the following steps：
(1) H in sour gas2When S concentration is more than 15vol.%, sour gas enters Crouse's burning after removing ammonia by water scrubber Stove, the process gas for going out Crouse's combustion furnace pass through waste heat boiler, hydrolysis reactor, two-stage claus reaction device, add hydrogen anti-successively Enter after answering device and cooling down and absorb oxidation reaction chamber, tail gas direct emission up to standard, useless pot and sulfur condenser directly generate high-quality Molten sulfur.The sulphur slurry that oxidation reaction chamber generates is absorbed to produce after molten slurry tank, sulfur melting kettle, molten sulphur separator respectively after filter Raw high-quality sulphur.It is not required to maintain H in claus reaction device2S/SO2It is stringent 2/1, control system is simple.
(2) H in sour gas2When S concentration is less than or equal to 15vol.%, sour gas enters water scrubber, hydrolysis reactor and cold But enter absorption oxidation reaction chamber afterwards, absorb the sulphur that oxidation reaction chamber generates and starch and pass through molten slurry tank respectively after filter, melt High-quality sulphur is generated after sulphur kettle, sulfur melting kettle separator, absorbs oxidation reaction chamber tail gas direct emission up to standard.Hydrolysis reactor It can be used for directly removing the COS in unstripped gas, further decrease the content of sulphur-containing substance in tail gas.
Specifically, sour gas carries out water-washing pre-treatment in the water scrubber equipped with structured packing removes ammonia, ammonia can be effectively prevented It is dispersed into gas phase in sulphur slurry filter element.
Further, waste heat boiler can generate the saturated vapor of 0.5MPag and be directly used in sulfur melting kettle, it is enabled measure it is reasonable It utilizes.
Further, it is hydrolysis reactor and two-stage claus reaction device, water after pot as an improvement, Crouse's combustion furnace gives up It solves and adds titanium-based hydrolyst in reactor, can remove the COS and CS generated in Crouse's combustion furnace2。
Further, Ti-base catalyst is loaded in hydrolysis reactor, the process gas after hydrolysis reactor need to be cooled to 40 ~60 DEG C, to reach the optimum temperature of Complexing Iron catalysis oxidation.
Further, it needs that complexing iron catalyst, fungicide, surfactant, defoaming is added in absorbing oxidation reaction chamber Agent and lye.
Further, it is passed through air in absorbing oxidation reaction chamber, the direct qualified discharge of tail gas after absorbing and aoxidizing.
Further, it absorbs the sulphur slurry feeding filter that oxidation reaction chamber generates to be filtered, filtrate sends reactor back to, filter Cake sulphur is sent to sulphur slurry tank and prepares sulphur slurry.
Further, addition water is starched to prepare sulphur in sulphur slurry tank, and sulphur concentration preferably 5%~15% in sulphur slurry, sulphur slurry is sent Enter sulfur melting kettle.
Further, sulphur slurry is sent to separator after being melted in sulfur melting kettle, and lower layer obtains high-quality molten sulfur, controls molten sulfur temperature Degree maintain 130~155 DEG C between, upper aqueous layer be sent to flash tank flash distillation after be recycled back to sulphur slurry tank prepare sulphur slurry.
The present invention is that a kind of handle contains ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carries out the novel process of sulphur recovery, is adopted It is washed with water except ammonia, Crouse's burning, hydrolysis, claus reaction, hydrogenation reaction, Complexing Iron redox reaction and sulphur essence The technique being combined is made, can be formed according to sour gas, flexibly select technological process, is suitable for the net of various different composition sour gas Change；Sulfur content is low in tail gas after processing, and sulfur recovery rate is more than 99.95%, and can recycle and obtain high-quality sulphur.
Advantage of the present invention essentially consists in：
(1) environmental-friendly, sulfur content is low in emission；
(2) recyclable to obtain high-quality sulphur；
(3) raw material sour gas is applied widely, is applicable to contain NH3Processing with the sour gas of COS and sulphur recovery.
It (4) can be according to H in sour gas2The concentration of S flexibly selects technological process.
(5) using Sulfur Recovery Unit unit it is not required to accurately control H when2S and SO2Ratio be 2/1, control is simple, operation Flexibly.The low-pressure steam of waste heat boiler and sulfur condenser by-product can be used for the heating of sulfur melting kettle, and heat is made to be comprehensively utilized.
Description of the drawings
Fig. 1 is one of embodiment of the present invention process flow chart.
Fig. 2 is two process flow charts of the embodiment of the present invention.
Drawing reference numeral explanation：Water scrubber (1), Crouse's combustion furnace (2), waste heat boiler (3), hydrolysis reactor (4), level-one Condenser (5), level-one claus reaction device (6), secondary condenser (7), two level claus reaction device (8), three-level condenser (9), hydrogenation reactor (10), technique Gas Cooler (11), absorption oxidation reaction chamber (12), filter (13), molten slurry tank (14), Sulfur melting kettle (15) melts sulphur separator (16), flash tank (17).
Specific implementation mode
Embodiment 1
As shown in Figure 1, sour gas (101) enters Crouse's combustion furnace (2) after water scrubber (1) deviates from ammonia, after reaction Process gas enter waste heat boiler (3) and carry out waste heat recovery, and by-product low-pressure steam is preheated by the process gas of waste heat recovery Enter hydrolysis reactor (4) afterwards, hydrolyzes the COS and CS for reacting generation in claus oven2, go out the process gas of hydrolysis reactor successively By level-one sulfur condenser (5), level-one claus reaction device (6), two level sulfur condenser (7), two level claus reaction device (8), Three-level condenser (9), by-product low-pressure steam while molten sulfur (104) is discharged from level-one, two level, three-level sulfur condenser.Go out three-level By hydrogenation reactor (10) after the process gas of condenser is preheated, add the process gas after hydrogen cooling through technique Gas Cooler (11) Enter after to 40~60 DEG C and absorb oxidation reaction chamber (12), absorb use complex compound catalyst in oxidation reaction room by H2S turns Elemental sulfur is turned to, complexing iron catalyst is using the air reduction process being passed through, tail gas (107) qualified discharge after absorption.It generates Wet sulphur is filtered by filter (13), and filtrate (108), which returns, absorbs oxidation reaction chamber (12), and sulphur send molten slurry tank (14). Sulphur and water send sulfur melting kettle (15) after forming sulphur slurry in molten slurry tank, and separator (16) is sent to isolate the molten sulfur after high-purity after melting (104), water layer removes flash tank (17), and the water (110) after flash distillation returns to molten slurry tank and recycles.
Embodiment 2
As shown in Fig. 2, sour gas (101) preheats after water scrubber (1) removes ammonia, into hydrolysis reactor (4), hydrolysis The COS contained in raw material sour gas goes out the process gas of hydrolysis reactor after technique Gas Cooler (11) is cooled to 40~60 DEG C Into oxidation reaction chamber (12) is absorbed, absorb use complex compound catalyst in oxidation reaction room by H2S is converted into elemental sulfur, network It closes iron catalyst and uses the air reduction process being passed through, tail gas (107) qualified discharge after absorption.The wet sulphur generated is by filtering Machine (13) filters, and sulphur send molten slurry tank (14), and filtrate (108), which returns, absorbs oxidation reaction chamber (12).In molten slurry tank sulphur and Water send sulfur melting kettle (15) after forming sulphur slurry, and the sulphur (104) for sending separator (16) to isolate high-purity after melting, water layer goes to flash Tank (17), the water (110) after flash distillation return to molten slurry tank and recycle.
A real case using the present invention is as follows, sour gas (101) flow 7634Nm3/ h, H2S is a concentration of 35mol.%, COS a concentration of 0.08mol.%, NH3A concentration of 2.75%.When after the processing of this patent described device, go out to add The process gas flow 7746Nm of hydrogen reactor3/ h, H2A concentration of 1.39mol.% of S, the H in tail gas (107) after absorption2S contents ＜ 10ppm, can qualified discharge.By-product 10.82t/h pressure is in waste heat boiler, level-one, two level, three-level sulfur condenser simultaneously The saturated vapor of 0.5MPag is used for sulfur melting kettle, and device heat is made to be comprehensively utilized.

Claims (10)

1. a kind of processing carries out the novel process of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, it is characterized in that：
(1) H in sour gas2When S concentration is more than 15vol.%, sour gas enters Crouse's combustion furnace after removing ammonia by water scrubber (1) (2), the process gas for going out Crouse's combustion furnace passes through waste heat boiler (3), hydrolysis reactor (4), two-stage claus reaction device successively (6,8), hydrogenation reactor (10) simultaneously enter absorption oxidation reaction chamber (12) after technique Gas Cooler (11) is cooling, and tail gas is up to standard Direct emission, waste heat boiler (3) and three-level sulfur condenser (5,7,9), condensation and separation of high-quality molten sulfur, absorb oxidation reaction chamber (12) the sulphur slurry generated sequentially enters molten slurry tank (14), sulfur melting kettle (15), sulfur melting kettle separator after filter (13) filtering (16) high-quality sulphur is obtained afterwards；
(2) H in sour gas2When S concentration is less than or equal to 15vol.%, sour gas sequentially enters water scrubber (1), hydrolysis reactor (4) And enter after technique Gas Cooler (11) is cooling and absorb oxidation reaction chamber (12), it absorbs the sulphur slurry that oxidation reaction chamber generates and passes through After filter (13) filtering, thick sulphur content does not obtain after molten slurry tank (14), sulfur melting kettle (15), sulfur melting kettle separator (16) purification High-quality sulphur absorbs oxidation reaction chamber tail gas direct emission up to standard.
2. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：Sour gas carries out washing in the water scrubber (1) equipped with structured packing and removes ammonia, and washings send sewage disposal, Ammonia can be effectively prevented to be dispersed into air in sulphur slurry filter element.
3. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：For the control of Crouse's combustion furnace (2) temperature at 900~1300 DEG C, furnace body uses inner lining structure.
4. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：As the improvement of conventional Claus technique, Crouse's combustion furnace (2) give up after pot as hydrolysis reactor (4) and Two-stage claus reaction device (6,8) loads titanium-based hydrolyst in hydrolysis reactor, can remove raw in Crouse's combustion furnace At COS and CS2。
5. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：When acid gas concentration is less than or equal to 15vol.%, sour gas is directly entered hydrolysis reactor (4), and removal is former Expect the organic sulfur compounds such as the COS in gas, avoid and bring follow-up process into, sulfur content in tail gas is caused to increase.
6. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：(4) load Ti-base catalyst in hydrolysis reactor, and technique air cooling is into absorbing oxidation reaction chamber (12) Temperature is controlled at 40~60 DEG C, to reach the optimum temperature of Complexing Iron catalysis oxidation.
7. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：It needs that complexing iron catalyst, fungicide, surfactant, defoaming is added in absorbing oxidation reaction chamber (12) Agent and lye；It absorbs the sulphur slurry that oxidation reaction chamber generates to filter through filter (13), filtrate, which returns, absorbs oxidation reaction chamber, filtering Thick sulphur is sent to molten slurry tank (14) and prepares sulphur slurry；It is passed through air in absorbing oxidation reaction chamber (12), the tail after absorbing and aoxidizing The direct qualified discharge of gas.
8. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：Molten slurry tank (14) need to be added through the filtered thick sulphur of filter (13) and prepare sulphur slurry, sulphur is dense in sulphur slurry Degree preferably 5%~15%, sulphur slurry are sent into sulfur melting kettle (15).
9. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：The sulphur slurry of sulphur a concentration of 5%~15%, which is added after sulfur melting kettle (15) melts, enters sulfur melting kettle separator (16), cycle back dissolving slurry tank (14) prepares sulphur slurry after the water layer on sulfur melting kettle separator (16) upper layer is sent to flash tank (17) flash distillation； Lower layer obtains high-quality molten sulfur, and control molten sulfur temperature maintains between 130~155 DEG C.
10. a kind of processing as described in claim 1 carries out the novel of sulphur recovery containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas Technique, it is characterized in that：Sulfur melting kettle (15) and molten sulfur pipeline use jacket steam heat tracing.
CN201610792752.5A 2016-08-31 2016-08-31 It is a kind of to handle containing ammonia, carbonyl sulfur, hydrogen sulfide sour gas, and carry out the novel process of sulphur recovery Active CN106395756B (en)

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CN109336066B (en) * 2018-11-28 2022-05-31 宜宾海翔化工有限责任公司 Process and system for jointly preparing acid by recycling sulfur and waste gas from viscose waste gas TRS
CN113150837B (en) * 2021-04-23 2022-07-26 济南冶金化工设备有限公司 Coke oven gas desulfurization process

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