WO2020160842A1 - Procédé et appareil de traitement de gaz comprenant un processus oxydatif pour traiter un mélange de gaz acides à l'aide de gaz provenant d'un processus de séparation d'air - Google Patents

Procédé et appareil de traitement de gaz comprenant un processus oxydatif pour traiter un mélange de gaz acides à l'aide de gaz provenant d'un processus de séparation d'air Download PDF

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WO2020160842A1
WO2020160842A1 PCT/EP2020/025040 EP2020025040W WO2020160842A1 WO 2020160842 A1 WO2020160842 A1 WO 2020160842A1 EP 2020025040 W EP2020025040 W EP 2020025040W WO 2020160842 A1 WO2020160842 A1 WO 2020160842A1
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Prior art keywords
steam
time period
amount
air separation
air
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Oliver Neuhaus
Dimitri GOLUBEV
Marcus Guzmann
Jolien PIRARD
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Linde GmbH
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Linde GmbH
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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
    • C01B17/0452—Process control; Start-up or cooling-down procedures of the Claus process
    • 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
    • B01D53/14—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 by absorption
    • B01D53/1456—Removing acid components
    • B01D53/1468—Removing hydrogen sulfide
    • 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
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B01D53/8612—Hydrogen sulfide
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/04018—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of main feed air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • F25J3/04115—Arrangements of compressors and /or their drivers characterised by the type of prime driver, e.g. hot gas expander
    • F25J3/04121—Steam turbine as the prime mechanical driver
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04612—Heat exchange integration with process streams, e.g. from the air gas consuming unit
    • F25J3/04618—Heat exchange integration with process streams, e.g. from the air gas consuming unit for cooling an air stream fed to the air fractionation unit
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04812—Different modes, i.e. "runs" of operation
    • F25J3/04818—Start-up of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/10—Oxidants
    • B01D2251/102—Oxygen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/10—Oxidants
    • B01D2251/11—Air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/204—Amines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/24—Hydrocarbons
    • B01D2256/245—Methane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/102—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/04—Compressor cooling arrangement, e.g. inter- or after-stage cooling or condensate removal
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/06—Adiabatic compressor, i.e. without interstage cooling
    • 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

Definitions

  • Gas treatment method and apparatus including an oxidative process for treating a sour gas mixture using gas from an air separation process
  • the present invention relates to a gas treatment method including an oxidative process for the desulphurisation of a sour gas mixture, the oxidative process utilising gas from an air separation process, and to corresponding apparatus according to the
  • US 4,684,514 A discloses a method of recovering sulphur from a hydrogen sulphide- containing gas stream which removes water concurrently with the condensation of sulphur and which can be operated at high pressure.
  • US 2013/0071308 A1 relates to a method and to a plant for recovering sulphur from a sour gas containing hydrogen sulphide and carbon dioxide. Carbon dioxide is compressed and at least a part thereof is injected into an oil well.
  • the Claus process originally only mixed hydrogen sulphide or a corresponding sour gas mixture with oxygen and passed the mixture across a pre-heated catalyst bed. It was later modified to include a free-flame oxidation upstream the catalyst bed in a so- called Claus furnace.
  • Most of the sulphur recovery units (SRU) in use today operate on the basis of a correspondingly modified process. If, in the following, therefore, shorthand reference is made to a“Claus process” or to a corresponding apparatus, this is intended to refer to a free-flame modified Claus process as just described.
  • So-called oxygen enrichment is a well-known economic and reliable method of debottlenecking existing Claus sulphur recovery units with minimal capital investment.
  • Oxygen enrichment is, however, as described in detail below, not limited to retrofitting existing Claus sulphur recovery units but can likewise be advantageous in newly designed plants.
  • The“term oxygen enrichment” shall, in the following, refer to any method wherein, in a Claus sulphur recovery unit or in a corresponding method, at least a part of the air introduced into the Claus furnace is substituted by oxygen or a by gas mixture which is, as compared to ambient air, enriched in oxygen or, more generally, has a higher oxygen content than ambient air.
  • Oxygen or oxygen enriched gas mixtures for Claus sulphur recovery units can be, in general, provided by cryogenic air separation methods and corresponding air separation units (ASU) as known from the prior art, see e.g. Haering, H.-W.,“Industrial Gases Processing,” Wiley-VCH, 2008, especially chapter 2.2.5,“Cryogenic
  • Cryogenic air separation units typically comprise a so-called warm section configured for compression, pre-cooling, drying and pre-purification of feed air, and a so-called cold section configured for heat exchange and rectification.
  • US 2004/211183 A1 discloses a method for driving at least a compression machine of an air distillation unit which supplies oxygen and/or nitrogen and/or argon to an industrial plant producing water vapour.
  • the compression machine is driven at least partly by a steam turbine fed with said water vapour, which is input at an input port of the turbine.
  • the turbine has two input ports which correspond to different intake pressures.
  • the turbine is partly supplied with water vapour from an auxiliary water vapour source and input at the turbine other input port.
  • cryogenic air separation While the present invention is, in the following, described with a focus on cryogenic air separation, it can likewise be used with advantage with non-cryogenic air separation methods and units, e.g. based on pressure swing adsorption (PSA), particularly with desorption pressure levels below atmospheric pressure (Vacuum PSA, VPSA). Usage of the present invention is particularly advantageous if such methods or units operate using ratable equipment driven or drivable by using steam, particularly a steam turbine.
  • An air separation process is part of the method according to the present invention described hereinbelow and an air separation unit is part of a corresponding plant.
  • the present invention is also not limited to the Claus process but can equally be used in other gas treatment methods including an oxidative process for desulphurisation of a sour gas mixture, provided that in such methods also oxygen, e.g. pure oxygen or oxygen contained in a component mixture which is enriched in oxygen, is at least temporarily provided by an air separation unit.
  • oxygen e.g. pure oxygen or oxygen contained in a component mixture which is enriched in oxygen
  • An object of the present invention is to provide improved methods of this kind, particularly in view of reducing capital and operating expenses.
  • the present invention provides a gas treatment method including an oxidative process for the desulphurisation of a sour gas mixture, the oxidative process utilising gas from an air separation process, and to a corresponding apparatus including the features of the independent claims, respectively.
  • the sour gas mixture may, in the present invention, particularly be obtained from a gas mixture containing hydrogen sulphide and optionally carbon dioxide and other sour gases, especially in a chemical and/or physical absorption step using an absorption liquid, particularly in a so-called amine unit. Obtaining a sour gas mixture can also form part of the invention.
  • the oxidative process which is, according to the present invention, used for the desulphurisation of the sour gas mixture, is particularly a Claus process or a variant thereof.
  • the term“desulphurisation” as used herein shall refer to any process including conversion of a first sulphur compound comprising sulphur at a lower oxidation stage, which is contained in a sour gas mixture, to a second sulphur compound comprising sulphur at a higher oxidation stage in a first reaction step, and particularly further including forming elementary sulphur from the second sulphur compound in a second reaction step, the elementary sulphur particularly being obtained in liquid state.
  • the first sulphur compound may be hydrogen sulphide and the second sulphur compound may be sulphur dioxide.
  • the first reaction step may particularly include combusting the first sulphur compound and the second reaction step may particularly include using a suitable catalysis reaction as generally known for the Claus process.
  • a mixture of components may be rich or poor in one or more components, where the term“rich” may stand for a content of more than 75%, 80%, 85%, 90%, 95%, 99%, 99.5% or 99.9% and the term“poor” for a content of less than 25%, 20%, 15%, 10%, 5%, 1 %, 0.5% or 0.1 %, on a molar, weight or volume basis.
  • a sour gas mixture with a hydrogen sulphide content of more than 80% is generally referred to as“rich” while a sour gas mixture containing less hydrogen sulphide is generally referred to as“lean.”
  • a mixture may also be, in the language as used herein, enriched or depleted in one or more components, especially when compared to another mixture, where“enriched” may stand for at least 1 , 5 times, 2 times, 3 times, 5 times, 10 times or 100 times of the content in the other mixture and“depleted” for at most 0.75 times, 0.5 times, 0.25 times, 0.1 times, or 0.01 times of the content in the other mixture.
  • sour gas mixture refers, in the language as used herein, to a gas mixture containing at least hydrogen sulphide and optionally carbon dioxide and other known sour gases in an amount of at least 50%, 75%, 80% or 90% by volume, this numbers relating to the content of one of these compounds or to a common content of several ones. Further components besides sour gases may be present in a sour gas mixture as well, particularly water, hydrocarbons, benzene, toluene and xylenes (BTX), carbon monoxide, hydrogen, ammonia and mercaptans.
  • BTX benzene, toluene and xylenes
  • pressure level and“temperature level” are used herein in order to express that no exact pressures but pressure ranges must be used in order to realise the present invention and advantageous embodiments thereof.
  • Different pressure and temperature levels may lie in distinctive ranges or in ranges overlapping each other. They also cover expected and unexpected, particularly unintentional, pressure or temperature changes, e.g. inevitable pressure or temperature losses.
  • Values expressed for pressure levels in bar units are absolute pressure values.
  • the air to be treated is compressed, cleaned and cooled before it is subjected to separation, e.g. before it is fed into a distillation column system in a cryogenic method.
  • Compressors for use in air separation units can be it of the cryogenic or the non-cryogenic type, can be designed as turbo or positive displacement machines, the two types differing in their operational behaviour. With turbo machines, the amount of
  • Turbo compressors are by far the most frequently used machines in cryogenic air separation. Turbo compressors can be of the radial or the axial type. They differ from each other in the direction by which the compressed gas leaves the impeller.
  • a radial turbo compressor is typically made up of several stages which are arranged on one or more shafts. These shafts are driven via a gear either by an electric motor or a steam turbine.
  • the compression of the air is at least in part an adiabatic process.
  • the compression work carried out during compression thus increases the internal energy of the air so that its temperature rises.
  • the latter is also referred to as compression heat.
  • Air compressed in a main air compressor (MAC), e.g. of the turbo type, of an air separation unit is heated by the compression typically to about 100 °C and is therefore, in conventional processes as known from the prior art, prior to being cooled via a heat exchange with air separation products, pre-cooled with water.
  • MAC main air compressor
  • main air compressor compressor(s) of a cryogenic or non-cryogenic air separation unit which compress(es) all the air to be separated to a certain pressure level.
  • a main air compressor may be followed by a so-called booster air compressor (BAC) or several so-called boosters driven by turbines.
  • booster air compressor BAC
  • booster air compressor boosters driven by turbines.
  • BAC booster air compressor
  • BAC booster air compressor
  • a main air compressor and a booster air compressor are to be understood as machines entirely or at least partially driven by external energy, the term“external energy” referring to energy which was not obtained by expanding process streams formed in the air separation unit itself using e.g. turboexpanders.
  • a sour gas mixture used as a feed for a Claus sulphur recovery unit usually originates from a sour gas sweetening plant, e.g for sweetening natural gas or a gas from a petrochemical or oil refinery plant.
  • the sour gas mixture containing varying amounts of hydrogen sulphide and carbon dioxide, is saturated with water and frequently also contains small amounts of hydrocarbons and other impurities in addition to the principal components.
  • the sour gas mixture enters a typical Claus sulphur recovery unit at about 0.5 to 1.0 barg or about 0.8 to 1.3 barg and 50 °C.
  • combustion air is compressed to an equivalent pressure by centrifugal blowers. Both inlet streams then flow to a burner which fires into the Claus furnace, the burner being fed with a further fuel.
  • the gas mixture from the Claus furnace at a temperature of typically 900 °C and up to 1 ,450 °C, is typically cooled while generating high-pressure steam in a waste heat boiler and further cooled while producing low-pressure steam in a separate heat exchanger.
  • This cools the hot gases to approximately 160 °C, condensing most of the sulphur which has already formed up to this point.
  • the resultant liquid sulphur is removed in a separator section of the condenser and flows by gravity to a sulphur storage tank. Here it is kept molten, at approximately 140 °C, by steam coils. Sulphur accumulated in this reservoir is pumped to trucks or rail cars for shipment.
  • a typical Claus sulphur recovery unit comprises one free-flame reaction stage, i.e. one furnace, and three catalytic reaction stages. Each reaction step converts a smaller fraction of the remaining sulphur gases to sulphur vapour.
  • TGTU tail gas treatment unit
  • Wet scrubbing processes such as the BSR/amine process of WorleyParsons include a front-end section to convert all of the sulphur compounds still contained in the tail gas back into hydrogen sulphide.
  • the hydrogen sulphide-containing tail gas is contacted with a solvent to remove the hydrogen sulphide, much like in a conventional gas treating plant. The solvent is then regenerated to strip out the hydrogen sulphide, which is then recycled to the upstream Claus sulphur removal unit for subsequent conversion and recovery.
  • So-called oxygen enrichment is, as mentioned, a well-known economic and reliable method of debottlenecking existing Claus sulphur recovery units with minimal capital investment. It can also eliminate the need for fuel gas co-firing in the reaction furnace, required to maintain the correct temperature for contaminant destruction, for example for destruction of benzene, toluene and xylenes (BTX) in the sour gas mixture.
  • BTX xylenes
  • the concept of oxygen enrichment entails replacing part or all of the air fed to the Claus furnace by oxygen-enriched air or pure oxygen.
  • the volumetric flow through the Claus sulphur recovery unit decreases, allowing more of the sour gas mixture to be fed to the system. This results in an increased sulphur production capacity without the need for significant modifications to existing equipment or major changes to the process plant pressure profile.
  • oxygen enrichment is not limited to retrofitting or debottlenecking existing Claus sulphur recovery units, but can also have advantages in newly designed plants where the acid gas mixtures obtained are lean and contain benzene, toluene and xylenes.
  • Such plants classically require feed gas and/or combustion air preheating and the use of fuel gas co-firing and have not, historically, been considered for oxygen enriched operation.
  • the use of oxygen enriched technology results in a reduction in the physical size of all major equipment items and an associated, significant reduction in capital cost.
  • a large reduction in fuel requirements in co-firing in the Claus furnace and other units can be achieved and therefore more fuel, e.g. natural gas, can be used for other purposes or provided as a product of the whole plant.
  • a particular advantage of oxygen enrichment is, furthermore, that the tail gas downstream a tail gas treatment unit is less“diluted” with nitrogen from the combustion air classically used. If little or no additional nitrogen is introduced into the process, the main component of the sour gas mixture after desulphurisation, i.e. carbon dioxide, and other components like hydrogen can be recovered in a simpler and more cost-effective way, e.g. by cryogenic technology alone and without energy-intensive wet technology.
  • Air separation units irrespective whether they are based on cryogenic processes or adsorption processes, require compressors in order to process the air being used as feedstock.
  • Claus sulphur removal units conventionally are operated by introducing ambient air through blowers into the Claus furnace in order to introduce the oxygen contained in ambient air as reaction component.
  • an oxygen enriched operation at least a part of ambient air is exchanged for pure oxygen or a gas mixture which has a higher oxygen content than that of ambient air.
  • pure oxygen or an oxygen enriched gas mixture can be mixed into an air flow blown into the Claus furnace by a blower, and the amount of air is reduced correspondingly, in order to maintain a defined mass flow.
  • a blower is no longer used for introducing air to the Claus furnace and only oxygen or an oxygen enriched gas mixture can be used in order to provide oxygen for burning.
  • the main blower conventionally providing air to the Claus furnace can be dispensed of.
  • the much smaller air blowers for a reducing gas generator and a tail gas incinerator (if present, respectively) can be further reduced in size.
  • an air blower is not at all required during normal operation of the Claus furnace. Also in the former case, however, during normal operation less air has to be introduced into the Claus furnace, resulting in a smaller capacity demand for the blower. However, during start-up of the Claus sulphur removal process, a blower may still technically be required because the process is started up with ambient air and then gradually boosted by oxygen enrichment up to the desired level, e.g. up to 100% or at least 100% oxygen. Particularly, a corresponding plant must be warmed up before the main burner is ignited, in order to avoid thermal shock.
  • fuel gas will be burned with air (introduced with a blower) in the Claus furnace at start-up.
  • the introduced air, fuel gas and/or sour gas could be pre-heated using heat exchangers applying steam, which can also be done according to the invention.
  • a compressor of the air separation unit instead of the blower a compressor of the air separation unit can be used.
  • the air separation unit used in the present invention is preferably dedicated to supply the oxygen to the Claus sulphur removal unit with the objective to operate the Claus sulphur removal unit on an oxygen enriched air or 100% oxygen basis.
  • no oxygen is required because, as mentioned, the oxygen content of the feed into the Claus sulphur removal unit will be gradually increased.
  • the main air compressor being required for the air separation unit can be used, according to a preferred embodiment of the present invention, to provide the air flow into the Claus unit.
  • the required air pressure level for the feed into the Claus sulphur removal unit here referred to as feed pressure level, is between 0.5 to 3.5 barg (bar gauge pressure), which matches the air pressure providable by the main air compressor.
  • the air separation can be turned off at this stage of Claus sulphur removal unit start-up or could be run in a turndown mode in this preferred embodiment of the present invention. While the oxygen enrichment level into the Claus sulphur removal unit is gradually increased, the air volume required by the Claus sulphur removal unit may accordingly be reduced gradually and can be substituted by products of the air separation performed in the air separation unit. Therefore, the main air compressor can provide a gradually increasing air volume to the air separation process which in turn can provide gradually increasing amounts of air separation products. In contrast, a decreasing air volume is provided to the Claus sulphur removal unit until this is completely substituted by a product of air separation in the air separation unit. Usage of the main air compressor of the air separation as described means, however, that this main air compressor must be operated from some point during start-up of the plant.
  • an“air separation product” refers, in the language used herein, to any fluid which can be obtained by cryogenic or non-cryogenic air separation and which contains one or more components of ambient air in a higher or lower content than ambient air, i.e. which is enriched or depleted in the meaning above.
  • an air separation product as used in the context of the present invention is an oxygen rich or oxygen enriched air separation product or (essentially) pure oxygen.
  • The“oxygen- containing gas” referred to hereinbelow is such an air separation product.
  • the present invention is of particular advantage in connection with sour gas desulphurisation involving the Claus process, but equally suitable for other processes of sour gas desulphurisation.
  • the present invention provides an advantageous integration of air separation and sour gas desulphurisation.
  • the present invention is based on the finding that a concerted activation of the different components used in a corresponding method allows for a particularly advantageous operation when a (main air) compressor which is operated by a steam turbine is used in the air separation process. If, in the following, general reference is made to a“compressor” used in an air separation process or plant, this is particularly intended to refer to the main air compressor.
  • a central aspect of the present invention is to recover compression heat of air which is compressed for subsequent separation in the air separation process and to use this heat in generating the steam used for operating the compressor.
  • the compression heat can be used, due to its heat level, to preheat boiler feed water which is converted into the steam in a steam generator.
  • steam generator shall, in the language as used herein, refer to equipment for converting liquid water to steam and may include boilers, boiler feed water preheaters, steam heaters and superheaters and the like. All these components can be embodied as heat exchangers as known in the prior art or can be or at least include such heat exchangers.
  • a particularly important aspect of the present invention is the way in which a heat deficit which results from lacking compression heat during start-up of a corresponding method is compensated.
  • the compression heat is particularly not available during start-up, at least during the beginning of a start-up sequence, because an air separation process is, as mentioned, only gradually started and because the compressor is only gradually powered up. The latter is also the result of technical constraints. In other words, while steam is required during such periods, no
  • start-up sequence a series of process states of a steady or dynamic nature shall be understood herein, the start-up sequence particularly including sequentially putting into operation several components used in the method.
  • the method utilizes the different components in a mostly steady state, this, however, not excluding changing set-points in the context of a control operation.
  • the period subsequent to such a start-up sequence corresponds to a regular operation of the method or plant.
  • a steam generation system could generally be equipped with a heater capable of providing heat sufficient for start-up when the compression heat is not present.
  • the steam volume required for the start-up of an air separation unit including a compressor driven by a steam turbine could generally be provided using an external boiler at scale that matches the required steam capacity for the main air compressor during start-up.
  • the compression heat used for steam generation according to the present invention as indicated above can also be used to generate steam, and the full potential of the steam boiler which is required for start-up is no longer utilised. Operation of the steam boiler may thus become inefficient. Also providing a steam boiler which is essentially overdesigned for most of the time represents an unwanted investment.
  • such a boiler can be designed with a smaller capacity, as explained in the following.
  • Such a boiler can, according to the invention, generally be designed with a capacity that matches, but does not exceed, the required steam capacity for the main air compressor during regular operation wherein compression heat from the compressed air is also used in steam generation, particularly for pre-heating boiler feed water.
  • the capacity gap between steam requirements for air separation during start-up and during regular operation is filled according to the present invention using an existing start-up boiler which is particularly associated to the oxidative process for
  • start-up boiler also referred to an“auxiliary” steam generator herein
  • auxiliary steam generator is particularly used for pre-heating certain equipment used in the method during start-up, but conventionally not required during later regular operation. It can already exist in a corresponding plant for pre-heating equipment or it may be specifically installed for the process steps provided according to the present invention.
  • start-up and“auxiliary” steam generator are used synonymously herein.
  • Equipment that may be heated accordingly particularly may include a pre-heating system used to pre-heat a sulfur treatment system in the oxidative process.
  • the elementary sulfur produced is obtained in liquid form. Therefore, particularly components for handling such sulfur must be pre heated in order to avoid solidification when liquid sulfur contacts the still cold surfaces in the sulfur treatment system. However, also a number of other components may be pre-heated accordingly. Such components are mentioned throughout this description.
  • a start-up boiler or auxiliary steam generator as described provides, according to the present invention, steam for preheating components in an initial part of a start-up process or sequence and later on during the start-up sequence provides steam which is in turn used in providing or generating steam for operating the compressor of the air separation unit as explained in more detail hereinbelow.
  • An advantageous operation according to the present invention can be achieved without enlarging the steam generation system in order to cope with a reduced availability of compression heat.
  • compression heat of the air compressed in an air separation process is used in a steam generation system generating steam which is also used in the inventive method.
  • the compression heat is particularly withdrawn between different compression stages of a main air compressor and/or downstream of the main air compressor or its last compression stage.
  • the compression heat is at least in part withdrawn from the air and is transferred using a heat transfer medium used in one or more cooling steps during or downstream of the (main) compression, absorbing the heat energy from the compression.
  • This heat transfer medium is then particularly used to preheat water supplied to the steam generation system, i.e. to boiler feed water. Due to the preheating of the boiler feed water, less thermal energy is required to generate steam according to the present invention. If no compression heat is available during a start-up process, heat which is contained in steam that is provided by an auxiliary steam generator is used instead.
  • the compression of air in the air separation process is performed using at least one compressor or compression stage using steam, i.e. such a compressor or compression stage is particularly driven using a steam turbine, and the steam from the steam generation system is at least in part used to operate the steam turbine.
  • the steam which is used to drive the steam turbine is thus, in other words, at least in part (and at least during certain time periods) produced using heat from the air which is compressed using the steam turbine or, more precisely, a compressor or a compression stage driven thereby.
  • the main air compressor of an air separation plant used in the air separation process can be operated entirely using a steam turbine.
  • the compression heat is not the only heat source for steam generation but contributes to the total heat required therefor, e.g. in the context of preheating boiler feed water.
  • the method according to the present invention includes a start-up sequence as explained in detail hereinbelow.
  • a corresponding plant is not yet fully operational, as several components not yet operate or do at least not yet operate at full capacity.
  • start-up of a corresponding plant entails subsequently activating or starting several plant components or parts.
  • the present invention can, in an illustrative example, be used in connection with an air separation unit with a production capacity of 106,000 Nm 3 /h (normal cubic metres per hour) at 2 bara (bars absolute pressure) with which no substantial amounts of other gaseous or liquid products are provided.
  • the air separation process is optimised to minimise energy consumption and includes supply of the process air at two pressure levels.
  • the main air compressor may be of the axial-radial type with a high isentropic efficiency in its axial stage.
  • the steam demand of the main air compressor aspiring ambient air at e.g. 35 °C may be 150 t/h at 25 bara at a temperature of 450 °C.
  • This required steam massflow rate to drive the main air compressor corresponds to a similar feed water volume with a feed condensate temperature of 40.3 °C.
  • the condensate exit temperature level is e.g. at about 165 °C.
  • the exemplified method involves heating boiler feed water from 40.3 to 165 °C by utilising compression heat and allows to save around 15% of natural gas required for boiler operation (in the considered case with partial heat integration and a separate steam generator serving mainly the air separation unit).
  • the sulphur recovery unit used in this example may produce superheated high-pressure steam at 25 bara and 450 °C with a mass flow of about 900 t/h, saturated at 42 bara and 370 °C. Due to the heat integration between the air separation unit and the sulphur recovery unit according to the present invention, the sulphur recovery unit may produce an increased volume of high-pressure steam.
  • the gain in steam mass flow in the present example could be up to 30 t/h and as such quite significant with reference to a steam flow required to operate the air separation unit. This steam can be at 25 bara and 450 °C.
  • the combination of both the high-pressure steam produced by sulphur recovery as well as high-pressure steam from the auxiliary steam generator can be also used to drive the main air compressor of the air separation unit.
  • the auxiliary steam generator not necessarily is used for pre-heating boiler feed water but can also be used to generate steam at a matching pressure and temperature level which is combined with or admixed to the steam from the main steam generator.
  • steam which is provided can also be fed into a steam grid which is present on-site, particularly by the auxiliary steam generator.
  • Gas processing plants and methods processing are rather complex and typically utilise various processing units such as e.g. acid gas removal units (e.g. so-called amine units in which an amine scrubbing is performed, as explained below), natural gas processing facilities (e.g. for so-called dewpointing or dehydration), sulphur removal units and tail gas treatment units as explained above.
  • acid gas removal units e.g. so-called amine units in which an amine scrubbing is performed, as explained below
  • natural gas processing facilities e.g. for so-called dewpointing or dehydration
  • sulphur removal units e.g. for so-called tail gas treatment units as explained above.
  • air separation units can be used not only to provide oxygen for the purposes as explained above but also to provide nitrogen for purging and blanketing.
  • Processes applied in such integrated processing plants and methods comprise sequential start-ups of the various processing units.
  • steam can be generated as a by-product, and this steam can be applied in another integrated units, i.e. in steam consumers.
  • a sulphur removal unit operating on the basis of the Claus process can be considered as steam exporter (in e.g. a refinery or gas processing plant) and this serves other processing units with steam during normal operation.
  • steam exporter in e.g. a refinery or gas processing plant
  • steam exporter serves other processing units with steam during normal operation.
  • steam is not yet available during start-up of the Claus process or a corresponding unit.
  • a typical amine gas treating process includes an absorber unit and a regenerator unit as well as accessory equipment.
  • a downflowing amine solution absorbs hydrogen sulphide and carbon dioxide from an upflowing gas mixture to produce a“sweetened” gas stream as a product and an amine solution rich in the absorbed acid gases.
  • the resultant“rich” amine is then routed into the regenerator unit representing a stripper with a reboiler to produce regenerated or“lean” amine that is recycled for reuse in the absorber unit.
  • An amine unit is typically used to sweeten natural gas and to provide sweetened natural gas (i.e. natural gas free of hydrogen sulphide and carbon dioxide).
  • the stripped gas mixture from the regenerator unit of this amine unit is enriched or rich in hydrogen sulphide and carbon dioxide. It represents the sour gas mixture which can be treated (desulphurised) in the Claus process.
  • residues of sour gases or intermediate products which were not fully converted to the target products, e.g. to elementary sulphur may be removed in a further amine unit.
  • the amine unit integrated in the tail gas treatment unit can be operated independently from the amine unit to which the natural gas is initially supplied.
  • the reboiler of the regenerator unit of the amine unit can be operated with steam produced using waste heat of the Claus process.
  • an amine unit producing a sour gas which is to be treated in the Claus process, and thus supplying the gas to be treated to the Claus process, must be started up before the Claus process.
  • no waste heat from the Claus process is yet available.
  • This problem is also present if other units in a corresponding integrated plant or method require steam, e.g. for heating purposes, which is not yet available at start-up.
  • a tail gas treatment unit can thus generally be considered to represent a steam consumer, wherein particularly during pre-heating and during start-up steam is required. Typically, by using waste heat from the Claus process, high and low pressure steam are produced. The tail gas treatment unit typically imports low pressure steam. Therefore, further steam can be produced and used for other purposes. In the
  • steam can be used to heat the tail gas to reaction temperature before it is introduced into the hydrogenation reactor. (The latter can, however, also be achieved by burning fuel gas in a“reducing gas generator”, RGG).
  • a dedicated steam plant including a steam boiler which is typically fired by gas or oil is used which temporarily is producing steam to serve the consumers during the start-up phase of the plant, if no waste heat is yet available.
  • This steam boiler may be the auxiliary steam generator as described herein.
  • the present invention may use, according to a preferred embodiment and during the start-up sequence, instead of steam from a dedicated steam plant or boiler, steam which is provided in a further steam plant or boiler which is used for driving one or more compressors, particularly the main air compressor, in an air separation unit which is also part of the integrated plant or method.
  • the air separation unit may, as mentioned in the outset, be a cryogenic or non- cryogenic air separation unit comprising a corresponding compressor.
  • the steam plant or boiler associated with the air separation unit may, according to the invention, be started up first to supply other gas processing units like the amine unit temporarily with steam during their start up, while no waste heat is yet available from e.g. the Claus process.
  • the steam boiler will start to serve steam to start up and later continuous operations of the air separation unit instead.
  • the present invention provides a gas treatment method including an oxidative process for desulphurisation of a sour gas mixture, and including an air separation process supplying an oxygen-containing gas to the oxidative process, wherein air is compressed in the air separation process by means of a compressor operated using steam.
  • the method comprises a start-up sequence used to sequentially put into operation the oxidative process and the air separation process as described above.
  • the start-up sequence (at least) includes a first, a second and a third time period. Further time periods can be included as well and may include further operation modes, as explained hereinbelow.
  • the first, second and third time period are non-overlapping time periods in the sequence as expressed by their enumeration, but in between these time periods further time periods may be present.
  • a first amount of steam is provided and the first amount of steam is used to preheat equipment used in the process.
  • the equipment which is pre-heated in the first time period is particularly used in the oxidative method, e.g. a Claus process.
  • Such equipment can particularly include a Claus furnace and catalytic reactors used for converting sulphur dioxide. It can also include components of a tail gas treatment unit as indicated above.
  • Equipment which is pre-heated in this way in the first time period can also be a steam turbine driving the compressor of the air separation unit which, after pre-heating in the first time period, is coupled to the steam turbine and gradually powered up thereafter.
  • auxiliary steam generator unit which is provided for preheating the equipment mentioned can therefore be used to provide steam for the steam turbine or can be used in order to support steam generation in a main steam generator, e.g. by means of pre-heating of boiler feed water.
  • Such steam can, however, also be fed into a steam grid from which the system can be supplied with steam. Pre-heating of boiler feed water is in later time periods performed via compression heat, and the operation of the auxiliary steam generator can be suspended.
  • a second amount of steam is provided and the second amount of steam is used to (at least partially) drive the compressor.
  • a third amount of steam is provided and the third amount of steam is used to drive (at least partially) the compressor.
  • a main steam generator is used in providing the second and the third amount of steam
  • an auxiliary steam generator is used in providing the first and the second amount of steam.
  • compression heat of the air compressed in the compressor is used in providing the third amount of steam as described before.
  • the auxiliary (or“start-up”) steam generator is used, and thereafter, if available, steam is instead produced including compression heat.
  • the auxiliary steam generator is used, in the first time period, predominantly or exclusively to preheat the equipment used in the process, and, in the second time period, predominantly or exclusively in providing steam (particularly in form of as a part of the second amount of steam) to drive the compressor in compensation for steam generated from the compression heat which is available in the third time period and is not available, or available in a lower amount, in the second time period.
  • a "predominant" use of the auxiliary steam generator shall refer to a use of at least 75%, 80% or 90% of the steam generated by the auxiliary steam generator for the purpose mentioned.
  • An “exclusive” use may particularly refer to a use of all the steam generated.
  • equipment is pre-heated, e.g. components used in the oxidative process and/or components like the compressor used in the air separation process.
  • the main steam generator is also used already. This main steam generator can be operated with waste heat of the oxidative process which now may be in operation or may start to operate, and thus represents a steam exporting unit.
  • the compressor already is driven by steam but not necessarily must supply the air separation process with compressed air yet.
  • compressed air may also be used to supply the oxidative process which is thus initially operated without oxygen enrichment.
  • the air separation process may be supplied with compressed air and may correspondingly produce increasing amounts of the oxygen-containing gas which then can gradually substitute the air which is previously provided to the oxidative process.
  • two sub periods may be included in the second time period, i.e. a first sub-period in which the air separation process is not yet producing air separation products and the oxidative process is operated in a non-enriched manner, and a second sub-period in which the air separation process is producing increasing amounts of air separation products and in which the oxidative process is operated in a gradually enriched manner.
  • the third time period when the system is essentially fully operational, the compression heat is used in steam generation.
  • the third time period may also essentially correspond to a subsequent operation mode.
  • an“amount” of steam, waste- heat, fluid, oxygen-containing gas or the like refers to an amount per a certain period of time, which is, if such amounts are compared to each other, an identical period of time for both cases. Particularly, such amounts can be expressed in standard units, i.e. related to standard conditions of pressure and temperature.
  • a steam generator or of heat“in providing” a certain amount of steam is meant to refer to any utilization of such steam conceivable.
  • a steam generator or such heat can be used as a part of the amount of steam, i.e. it can be combined with further proportion of steam, or heat of steam generated by such a steam generator can be used in a different steam generator, e.g. for pre-heating boiler feed water and/or for heating steam generated in the further steam generator.
  • the auxiliary steam generator which is used to perform pre-heating of equipment in the first time period via steam is used in providing the first and second amount of steam by using the steam generated for pre-heating boiler feed water which is used for generating the second amount of steam.
  • compression heat of the air compressed in the compressor is likewise used in providing the third amount of steam by pre-heating of boiler feed water.
  • Steam can also be supplied to a steam grid which can provide steam to different parts of the plant used according to the present invention and to different plants, as described. If steam is withdrawn from such a steam grid for a certain unit, the steam generator which supplies steam to the steam grid is used in providing this steam.
  • the gas treatment method preferably includes that boiler feed water is provided to the main steam generator in the second and third time period, wherein the boiler feed water is preheated at least in the third time period.
  • using the compression heat in providing the third amount of steam in the third time period comprises preheating the boiler feed water using the compression heat.
  • Using the auxiliary steam generator in providing the second amount of steam in the second time period may comprise preheating the boiler feed water using at least a part of the steam provided by the auxiliary steam generator, and/or combining such steam at least in part with the steam provided by the main steam generator.
  • the first, the second and the third amount of steam can be equal or different.
  • the first amount of steam may be smaller than the second and the third amount of steam.
  • the first, the second and the third amount of steam are not necessarily required to be constant, i.e. the second amount of steam can be increased over the second time period, in order to gradually power up the steam turbine and/or the compressor driven thereby, corresponding to the increasing amounts of waste heat available.
  • the present invention is particularly advantageous in connection with oxygen-enriched Claus processes because such processes are, as mentioned, typically started up with ambient air and then gradually boosted by oxygen enrichment of up to 100% oxygen up to the desired sulphur capacity level of e.g. up to 250% as compared to a non- enriched operation.
  • This staged start-up could be e.g. done to heat up the process equipment and to avoid thermal shock. Therefore, when starting up the Claus process, oxygen or oxygen enriched air from the air separation unit is not yet required in the Claus process and the compressor(s) of the air separation unit are not yet needed.
  • a steam plant or boiler for supplying steam to the compressor(s) of the air separation unit can instead be used to supply steam to further gas treatment units as mentioned.
  • waste heat is present.
  • fuel gas will be burned with air in the Claus furnace at start-up.
  • waste heat can be used in the second time period, as explained in detail before.
  • the air separation unit can be started after the units used in the Claus process have been pre-heated and the Claus process was started (and is initially operated with air). During this initial period, or during the“second” time period of the start-up sequence according to the present invention, the air separation unit can be gradually started up, wherein steam from the auxiliary steam generation unit (which, as mentioned, can be a“start-up boiler” already present in an existing plant or a dedicated steam generation unit) is also used in providing the steam for the compressor.
  • auxiliary steam generation unit which, as mentioned, can be a“start-up boiler” already present in an existing plant or a dedicated steam generation unit
  • initially steam may be used to pre-heat a steam turbine system which is used to drive the compressor, in order to uniformly warm the steam turbine rotor and casing, involving a still relatively small steam flow.
  • This may correspond to the first time period mentioned.
  • the compressor which is driven by the steam turbine e.g. the main air compressor of an air separation unit, is then coupled to the steam turbine and is gradually powered up to a minimum turndown at e.g. about 60 to 70% of the maximum speed or the regular operational speed.
  • the steam demand proportionally increases in this course.
  • This step may correspond to the second time period mentioned.
  • the air separation unit can start to provide the oxygen-containing gas to the oxidative process.
  • the oxygen content or amount used in the oxidative process is gradually increased until production and its use in the oxidative process are equal. If, in this context, the amount of oxygen-containing gas is too high, it can also be vented to the atmosphere or stored for later use. Reference is also made to the explanations regarding the first and second sub-periods of the second time period mentioned above. Subsequently, in a time period corresponding to the third time period mentioned, the oxydative process and the air separation process can be gradually further powered up until a maximum performance is reached. In the third time period, sufficient
  • compression heat is already available in order to contribute to steam generation.
  • the sour gas mixture desulfurised in the method according to the present invention may particularly be a lean sour gas mixture, i.e. a sour gas mixture containing less than 80%, less than 60% or less than 50% and more than 10%, more than 20%, more than 30% or more than 40% of hydrogen sulphide.
  • the present invention is particularly advantageous in this context, because lean sour gas mixtures comprise less oxidable components and therefore waste heat is produced to a smaller extent than in the case of rich sour gas mixtures. Therefore, a careful waste heat management is important, which is provided for according to an advantageous embodiment of the invention.
  • the sour gas mixture and the oxygen-containing gas are introduced into an oxidation unit.
  • the sour gas mixture is, for reference purposes only, referred to as a“first” gas mixture, i.e. the sour gas mixture is provided as this first gas mixture.
  • the sour gas mixture is desulphurised, i.e. an oxidable component in the first gas mixture is oxidised in the oxidating unit, providing waste heat.
  • a gas mixture used in providing the sour gas mixture is, for reference reasons only, also referred to as a“second” gas mixture.
  • the second gas mixture may e.g. be natural gas.
  • a gas mixture produced from at least a part of the sour gas mixture in the oxidating unit i.e. a gas mixture particularly depleted in hydrogen sulphide
  • a“third” gas mixture is referred to for reference purposes as a“third” gas mixture.
  • the sour gas, i.e. the first gas mixture, and/or the second gas mixture used in providing the first gas mixture and/or the third gas mixture produced from at least a part of the first gas mixture by using the oxidation unit is or are treated in one or more gas treatment units which are operated using further steam,“further steam” referring to an amount of steam not used as the first, second and third amount of steam referred to before or as a part thereof.
  • the“further steam” may generally also be provided in the main and/or the auxiliary steam generator referred to above which are used in providing the first, second and/or third amount of steam in the manner described.
  • At least a part of this further steam may be provided using heat other than waste heat of the oxidating unit or a sub-unit thereof, and in a regular mode of operation subsequent to the startup sequence, at least a part of this further steam may be provided using waste heat of the oxidating unit or a sub-unit thereof.
  • the oxidation unit may include a furnace, a catalytic unit subsequent thereto, or a tail gas treatment unit, particularly including a further burner. Each of these sub-units is capable of providing waste heat utilisable in the context of the present invention.
  • said operating the compressor using the steam may comprise expanding the steam in a steam turbine which is mechanically coupled to the compressor. This means that a direct transfer of rotational energy output by the steam turbine to the compressor is present, according to the present invention.
  • a mechanical coupling as used according to the present invention may include a coupling including equal speeds of a driving shaft of the steam turbine and a driven shaft of the compressor, or a coupling via a transmission or gearbox resulting in fixed or variable speed differences.
  • a mechanical coupling does not comprise, according to the present invention, an indirect coupling in which, for example, rotational energy from the steam turbine is converted to a different form of energy like electrical energy and wherein the different form of energy is converted to rotational energy in order to drive the compressor. Such an operation may, however, also be present, according to the present invention
  • a mechanical coupling which may be provided according to the present invention, eliminates energy conversion losses otherwise present.
  • operating the compressor using steam may comprise, in other words, expanding the steam in a steam turbine which is mechanically coupled to the compressor.
  • operating the compressor may also comprise using supplementary energy which is not provided in the form of steam expanded in the steam turbine.
  • generating further steam during at least a part of the start-up sequence may be done using heat other than waste heat and may be performed using a non waste heat steam generator.
  • Generating at least a part of this further steam subsequent to the start-up sequence may be done using waste heat of the oxidating unit or a sub-unit thereof and may be performed using a waste heat steam generator.
  • the non waste heat steam generator and the waste heat steam generator may be steam generators separate from the main and the auxiliary steam generator described before.
  • said generating at least a part of the further steam during at least a part of the start-up sequence, which is done using heat other than waste heat of the oxidating unit, and said generating at least a part of the further steam subsequent to the start-up sequence, which is done using waste heat of the oxidating unit or a sub-unit thereof, may also be performed using any other steam generators, a common steam generator, or a steam generation system including any of the steam generators mentioned.
  • At least a part of the further steam which is provided by the non waste heat steam generator during at least a part of the start-up sequence may be instead provided by the waste heat steam generator subsequent to the start-up sequence, and a total amount of steam smaller than the an amount of steam during at least a part of the start-up sequence, or no steam, may be provided by the non waste heat steam generator subsequent to the start-up sequence.
  • At least a part of the further steam provided by the waste heat steam generator subsequent to the start-up sequence may instead be provided by the non waste heat steam generator during at least a part of the start-up sequence, and a total amount of steam provided by the waste heat steam generator subsequent to the start-up sequence, or no steam, may be provided by the non waste heat steam generator during at least a part of the start-up sequence.
  • the waste heat steam generator may thus be operated only in cases in which waste heat is available, i.e. during start-up, or vice versa.
  • the non waste heat steam generator which may in at least a part of the start-up sequence be used in providing the further steam, may be used to operate the at least one gas treatment unit thereafter.
  • waste heat is also generated during at least a part of the start-up sequence.
  • the amount of this waste heat may be smaller than an amount of waste heat provided subsequent to the start-up sequence.
  • the oxidative process may be providing waste heat in a smaller waste heat amount during at least a part of the start-up sequence and may be providing waste heat in a larger waste heat amount thereafter, i.e. subsequent to the start-up sequence.
  • the present invention advantageously is used in connection with the Claus process and a corresponding gas treatment. Therefore, advantageously, the first gas mixture is a sour gas mixture, the oxidable component is hydrogen sulphide, the oxidative process is a Claus process, the oxidating unit is a Claus furnace, and a part of the hydrogen sulphide in the sour gas mixture is oxidised by free- flame oxidation in the Claus furnace.
  • the first gas mixture is a sour gas mixture
  • the oxidable component is hydrogen sulphide
  • the oxidative process is a Claus process
  • the oxidating unit is a Claus furnace
  • a part of the hydrogen sulphide in the sour gas mixture is oxidised by free- flame oxidation in the Claus furnace.
  • the air separation unit can provide, as also mentioned, oxygen or oxygen enriched air to the Claus process or its furnace or to another oxidative process.
  • a preferred method according to the present invention therefore includes that the oxygen-containing gas is provided as an air separation product, and the air separation product is pure oxygen or a mixture of components enriched in oxygen as compared to atmospheric air.
  • the method of the present invention may, according to a preferred embodiment, also include an operation mode in which the air separation process may not be in operation during a partial period of the start-up sequence while being in operation during a remainder of the start-up sequence. Likewise, also during later periods, the air separation process may not be in operation while it regularly is.
  • an operation mode i.e. when the air separation process is not in operation, which may also be an emergency or suspended operation mode, e.g. during a period of power loss or during maintenance, the oxidative process may be provided with unenriched air instead and the oxidative process, in this operation mode, may be operated without oxygen enrichment. This allows for situations in which the air separation process may not be available, e.g.
  • the oxidative process can be, with an impaired efficiency, however, operated continuously, eliminating the need for shutting down and later re-starting the oxidative process. As mentioned before, during start-up, also such an operation is contemplated.
  • the air separation product has an oxygen content higher than that of ambient air. It may comprise at least 30%, 40%, 50%, 60%, 70%, 80%, 90% or 95% oxygen by volume. In other words, different levels of oxygen enrichment are possible. Also, essentially pure oxygen may be used.
  • the air separation unit may also provide partly enriched oxygen products depending on the specific requirements of the Claus sulphur removal unit, and thus the energy consumption of the air separation unit can be optimised accordingly.
  • a cryogenic air separation unit including a mixing column can be used for this purpose, as e.g. described in EP 3 179 187 A1 and the references cited therein.
  • a larger amount of the air separation product is produced by the air separation unit subsequent to the start-up sequence, and a smaller amount of the air separation product or none of the air separation product is produced by the air separation unit during at least a part of the start-up sequence.
  • operation of the air separation unit can be fully or partially suspended. This is also the case for later periods in which the air separation process may not be in operation, particularly as described before.
  • only a part of the amount of the air separation product which is produced subsequent to the start-up sequence is introduced into the Claus furnace subsequent to the start-up sequence, and a further part of the air separation product is at least temporarily stored and is at least in part introduced into the Claus furnace in during a subsequent start-up sequence.
  • oxygen or oxygen-enriched air may be supplied to the oxidative process from oxygen or oxygen-enriched air which is produced in the normal operation mode and is e.g. stored in a back-up tank.
  • particularly liquid oxygen can be used.
  • a Claus furnace temperature in the sulphur recovery unit can, according to the present invention, be further increased by using additional oxygen and as such a larger steam quantity can be exported.
  • the overall steam balance can be optimised.
  • this additional steam produced by the delta of a conventional air based Claus process and the oxygen-enriched process is not utilised by the other process units, this excess steam could be utilised to run the steam drives of the air separation unit, at least partially.
  • the air separation unit can be operated at 100%.
  • a steam boiler size could be optimised.
  • the third gas mixture produced from at least a part of the first gas mixture using the oxidating unit, which was already referred to above, can be treated in a tail gas treatment unit.
  • a tail gas treatment unit generally represents a steam consumer, but may nevertheless be providing waste-heat, e.g. if it comprises a further furnace. Therefore, the tail gas treatment unit can be operated using the further steam referred to hereinbefore, in order to heat the tail gas to reaction temperature before it is introduced into a hydrogenation reactor in the tail gas treatment unit, or a loaded amine solution can be regenerated using heat from the further steam mentioned hereinbefore, or a part thereof.
  • a loaded amine solution can be regenerated using heat from the further steam mentioned hereinbefore, or a part thereof.
  • the present invention can also be used with an amine unit as explained above in order to treat a second gas mixture used in order to produce the first gas mixture.
  • a tail gas treatment unit adapted to treat the third gas mixture mentioned, or a part thereof, can comprise an amine unit.
  • the second gas mixture used in providing the first gas mixture and/or the third gas mixture produced from at least a part of the first gas mixture is treated in the or one of the gas treatment units, wherein the second and/or the third gas mixture is a gas mixture containing hydrogen sulphide and carbon dioxide, wherein the gas treatment unit or the one of the gas treatment units comprises an amine unit (or amine wash unit), wherein in the amine unit hydrogen sulphide and carbon dioxide are at least partially eliminated from the second and/or the third gas mixture using an amine solution and forming an amine solution loaded with hydrogen sulphide and carbon dioxide, and wherein the hydrogen sulphide and the carbon dioxide are at least in part stripped from the loaded amine solution using heat from the first amount of steam or a part thereof.
  • two gas treatment units, each including an amine unit can be provided in order to treat the second or the third gas mixture, respectively.
  • the present invention also relates to an apparatus for performing a gas treatment method as set forth in the corresponding independent apparatus claim, which is not recited herein for reasons of conciseness.
  • Such an apparatus may particularly include a control unit programmed or adapted to control the units of the apparatus in order to particularly perform the start-up sequence.
  • Figure 1 schematically illustrates a gas treatment method including an oxidative process for desulphurisation of a sour gas mixture in general.
  • Figure 2A schematically illustrates a gas treatment method including an oxidative process for desulphurisation of a sour gas mixture in a first mode of operation.
  • Figure 2B schematically illustrates the gas treatment method according to Figure 2A in a second mode of operation.
  • Figure 3A schematically illustrates a gas treatment method including an oxidative process for desulphurisation of a sour gas mixture according to an embodiment of the present invention in a third time period of a start-up sequence.
  • Figure 3B schematically illustrates the gas treatment method according to Figure 3A in a second time period of a start-up sequence.
  • Figure 3C schematically illustrates the gas treatment method according to Figure 3A in a first time period of a start-up sequence.
  • Figure 1 schematically illustrates a gas treatment method including an oxidative process 4 for desulphurisation of a sour gas mixture in general.
  • the process is illustrated as using a gas from an air separation process and is further illustrated to include a Claus process as the oxidative process 4.
  • a Claus process as the oxidative process 4.
  • a sour natural gas stream a from a gas field 1 is introduced into an sour gas removal unit 2, in this particular case including an amine unit 21 as mentioned before.
  • the amine unit 21 is operated as generally known in the art, in the present example using a steam stream b which is used to heat a reboiler in the amine unit 21 (not shown).
  • a steam stream c of a lower temperature or a condensate stream c can be formed.
  • a sweetened gas stream d is withdrawn from the acid gas removal unit 2 and optionally subjected to further treatment 3, providing a further treated gas stream e which can e.g. fed into a gas pipeline.
  • a sour gas stream f is also withdrawn from the acid gas removal unit 2 and is introduced into the oxidative process 4 which is embodied as a Claus process 4, or, more specifically, into a Claus furnace 41 in the Claus process 4 which was hereinbefore also referred to as a“oxidation unit” 41 or a part thereof.
  • the Claus process 4 may include further components.
  • a part of the sour gas stream f can also be reinjected into the gas field 1 , as indicated by a dotted arrow in Figure 1.
  • a sulphur stream g is withdrawn from the Claus process 4 and is subjected to a sulphur product handling 5. From this, a sulphur product stream h is withdrawn or otherwise provided.
  • a tail gas stream i also withdrawn from the Claus process 4 is treated in a manner known per se.
  • the tail gas treatment unit 6 provides a purified stack gas stream k with little or no sulphur compounds. Components from the tail gas treatment unit 6 can also, as illustrated with a dashed arrow, be reintroduced into the Claus process 4 or its Claus furnace 41.
  • the tail gas treatment unit 6 may also comprise a unit operable by heat, e.g. an amine unit 61 , wherein the heat is provided in the form of steam.
  • a steam stream b' is provided to this unit and a steam stream c' of a lower temperature or a condensate stream c can be formed.
  • One or both of the amine unit 21 in the acid gas removal unit 2 and the unit 61 in the tail gas treatment unit 6 may be provided and/or one or both of them may be operated using steam.
  • the Claus process 4 is operated with oxygen-enrichment in a regular operation mode. Therefore, using an air separation unit 7, an oxygen-containing gas, i.e. an oxygen stream or an oxygen-enriched stream I is provided which is also introduced into the Claus process 4 or its furnace 41.
  • the air separation unit 7, which also may provide a nitrogen or nitrogen-enriched stream and other products and to which air is supplied (not shown), comprises a compressor 71 operated with a steam driven turbine 72 receiving a steam stream m.
  • the turbine 72 is mechanically coupled to the compressor 71.
  • a steam stream n of a lower temperature or a condensate stream n can be formed.
  • the steam or condensate streams c, c’ and n can be reused for steam production.
  • FIG 2A schematically illustrates a gas treatment method 100 including an oxidative process 4 for desulphurisation of a sour gas mixture in a regular mode of operation which is performed subsequent to a starting sequence.
  • a first (waste heat) steam generator 10 and a second (non waste heat) steam generator 20 are shown in Figure 2A and 2B.
  • the first steam generator 10 is shown in proximity to the Claus process 4 (but does not necessarily have to be located in proximity to the Claus process 4). It is operated using at least a part of the waste heat of the Claus process 4.
  • the second steam generator 20 is shown in proximity to the air separation unit 7 (but does not necessarily have to be located in proximity to the air separation unit 7). It is operated independently from the waste heat of the Claus process 4.
  • the second steam generator 20 can also be installed remotely from the air separation unit 7 and may be operated independently therefrom.
  • the gas treatment unit 2 or, more precisely, the amine unit 21 , and/or the tail gas treatment unit 6, or, more precisely, the unit 61 , is operated using steam in a certain amount which is provided by the first steam generator 10 operated using at least a part of the waste heat of the Claus process 4.
  • the steam stream b is correspondingly provided by the first steam generator 10.
  • the compressor 71 of the air separation unit 7 is also operated using steam in the steam turbine 72 which is mechanically coupled to the compressor 71 , this steam being provided by the second steam generator 20.
  • the steam stream m is correspondingly provided by the second steam generator 20.
  • steam provided by the first steam generator 10 in the first mode of operation as shown in Figure 2B is instead provided by the second steam generator 20 (see steam stream b, wherein this is also possible for steam stream b' but not shown for reasons of clarity).
  • No steam is provided by the first steam generator 10.
  • No steam is, furthermore, provided to the steam turbine 72 mechanically coupled to the compressor 71 of the air separation unit 7 and the air separation unit 7 is not in operation in the startup sequence in this example. It is, however, likewise possible to provide stream to the steam turbine 72 by the second steam generator 20 or any other steam generator.
  • the heat recovered from the Claus process 4 is typically from two different sources.
  • the heat recovered from the Claus furnace 41 can be high pressure steam (HP steam). This can be up to 45 barg and is suitable for re-heating of the acid gas before entering the catalytic reactors and for driving turbines (it can also be superheated in the stack from the incinerator). Low pressure steam (LP steam) is generated in the sulphur condensers; this can be used to reboil the solvent in the amine unit(s) but is not suitable for driving turbines.
  • HP steam high pressure steam
  • LP steam Low pressure steam
  • Figure 3A schematically illustrates a gas treatment method including an oxidative process for desulphurisation of a sour gas mixture according to an embodiment of the present invention in a time period of a startup sequence previously referred to as the “third” time period in which compression heat is available.
  • Figure 3B schematically illustrates the gas treatment method according to Figure 3A in a mode of operation corresponding to the“second” part of the startup sequence referred to hereinbefore.
  • Figure 3C schematically illustrates the gas treatment method according to Figure 3A (and 3B) in a mode of operation corresponding to the“first” part of the startup sequence referred to hereinbefore.
  • FIG. 200 The process shown in Figures 3A, 3B and 3C is denoted 200. It may utilise all of the components as previously explained in relation to Figures 1 , 2A and 2B. Details are omitted for conciseness only, and in order to avoid repetitions. Particularly, the elements 1 to 6 are shown in a strictly simplified way, and only selected fluid streams are shown in Figures 3A, 3B and 3C.
  • the first, second and third time periods are illustrated in reversed order in Figures 3A, 3B and 3C only in order to better explain the differences therebetween, while in practice these time periods are arranged in the order of their enumeration, as mentioned.
  • the steam turbine 72 and the compressor 71 are shown in more detail in Figures 3A, 3B and 3C.
  • the compressor 71 a stream o of atmospheric air is compressed, obtaining a compressed air stream p which is cooled in one or more coolers 73, obtaining a cooled, compressed air stream q, and then subjected to an arbitrary number of further steps 74, e.g. to purification, further cooling and rectification. This is the case for the third and the second time periods shown in Figures 3A and 3B.
  • further coolers may be present which can be operated like the cooler 73.
  • the air separation unit 7 provides the oxygen or oxygen-enriched stream I which was already referred to before.
  • the cooler 73 is operated using one or more streams r of a heat transfer medium, via which compression heat is at least in part withdrawn from the air of the compressed air stream p in the third time period shown in Figure 3A.
  • the heat is transferred to a steam generation system, which may include the steam generator 10 or 20 as already described before, or a further steam generator 30.
  • the compression heat is used to feed boiler feed water in a boiler feed water heater 11 in such a steam generation system.
  • a steam generator 10, 20, 30 used accordingly is also referred to as a“main” steam generator hereinbefore.
  • the steam generation system or the steam generators 10, 20 or 30 may provide steam in form of the steam stream m to the steam turbine and/or further steam streams b, b' to any of the other components shown, as explained with reference to Figures 1 , 2A and 2B before.
  • the streams c, c' shown in Figures 1 , 2A and 2B, which are formed herein as well are omitted for conciseness.
  • several steam generators 10, 20 and 30 may operate accordingly and the block indicated with 10, 20, 30 in Figures 3A, 3B and 3C is only shown as one entity for reasons of conciseness herein.
  • the steam turbine 72 is also in operation here and sufficient steam can be provided via the operation of a further steam generator 40 in this case, which is referred to as an “auxiliary” steam generator.
  • a further steam generator 40 which may be operated by a firing, also e.g. the steam generator 20 can be used which may comprise an additional firing.
  • the steam generator to which the compression heat is transferred in the first mode of operation may be a steam generator different from the steam generator 20.
  • the steam generator 40 may also, instead of supplying steam directly to the steam turbine 72, used in order to pre-heat boiler feed water in the steam generators 10, 20 and/or 30.
  • the steam turbine 72 may not be in operation here and no air may be compressed in the compressor 71 , as also indicated by dashed lines.
  • the further steam generator 40 which may be operated like before, provides steam in order to pre-heat components of the process 200 as indicated before.

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Abstract

La présente invention concerne un procédé de traitement de gaz (200) comprenant un processus oxydatif (4) pour la désulfuration d'un mélange de gaz acides, et comprenant un processus de séparation d'air (7) alimentant au moins temporairement un gaz contenant de l'oxygène au processus d'oxydation (4). L'air est comprimé dans le processus de séparation d'air (7) à l'aide d'un compresseur (71) actionné à l'aide de vapeur. Selon la présente invention, le procédé (200) comprend une séquence de démarrage utilisée pour mettre en œuvre séquentiellement le processus oxydatif (4) et le processus de séparation d'air (7). La séquence de démarrage comprend une première, une deuxième et une troisième période de temps. Dans la première période de temps, une première quantité de vapeur est fournie et la première quantité de vapeur est utilisée pour préchauffer l'équipement utilisé dans le procédé (200); dans la seconde période de temps, une seconde quantité de vapeur est fournie et la seconde quantité de vapeur est utilisée pour entraîner le compresseur (71); dans la troisième période de temps, une troisième quantité de vapeur est fournie et la troisième quantité de vapeur est utilisée pour entraîner le compresseur (71); au moins dans la deuxième et la troisième période de temps, un générateur de vapeur principal (10, 20, 30) est utilisé pour fournir la deuxième et la troisième quantité de vapeur; au moins dans la première et la deuxième période de temps, un générateur de vapeur auxiliaire (40) est utilisé pour fournir la première et la seconde quantité de vapeur; et dans la troisième période de temps, la chaleur de compression de l'air comprimé dans le compresseur (71) est utilisée pour fournir la troisième quantité de vapeur. Le générateur de vapeur auxiliaire (40) est utilisé, dans la première période de temps, principalement ou exclusivement pour préchauffer l'équipement utilisé dans le procédé (200), et, dans la seconde période de temps, principalement ou exclusivement pour fournir de la vapeur pour entraîner le compresseur (71) en compensation de la vapeur générée à partir de la chaleur de compression qui est disponible dans la troisième période de temps et n'est pas disponible, ou disponible en quantité inférieure, dans la seconde période de temps. Un appareil correspondant est également selon la présente invention.
PCT/EP2020/025040 2019-02-07 2020-01-30 Procédé et appareil de traitement de gaz comprenant un processus oxydatif pour traiter un mélange de gaz acides à l'aide de gaz provenant d'un processus de séparation d'air Ceased WO2020160842A1 (fr)

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EP3984621A1 (fr) * 2020-10-13 2022-04-20 Linde GmbH Procédé et appareil de désulfuration d'un mélange de gaz impur
WO2022078628A1 (fr) * 2020-10-13 2022-04-21 Linde Gmbh Procédé et appareil pour la désulfuration d'un mélange gazeux acide

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