EP1633458A2 - Procede de desacidification d'un flux de fluide a l'aide d'une colonne de lavage inerte et dispositif correspondant - Google Patents

Procede de desacidification d'un flux de fluide a l'aide d'une colonne de lavage inerte et dispositif correspondant

Info

Publication number
EP1633458A2
EP1633458A2 EP04739463A EP04739463A EP1633458A2 EP 1633458 A2 EP1633458 A2 EP 1633458A2 EP 04739463 A EP04739463 A EP 04739463A EP 04739463 A EP04739463 A EP 04739463A EP 1633458 A2 EP1633458 A2 EP 1633458A2
Authority
EP
European Patent Office
Prior art keywords
absorption
solutions
washing
organic substances
fluid stream
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP04739463A
Other languages
German (de)
English (en)
Inventor
Stefan Meckl
Norbert Asprion
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
BASF SE
Original Assignee
BASF SE
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE2003125358 external-priority patent/DE10325358A1/de
Priority claimed from DE2003134002 external-priority patent/DE10334002A1/de
Application filed by BASF SE filed Critical BASF SE
Publication of EP1633458A2 publication Critical patent/EP1633458A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • 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
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • 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

Definitions

  • the present invention relates to a method for deacidifying a fluid stream which contains acid gases as impurities and a device therefor.
  • fluid flows occur that contain acid gases such as CO 2 , H 2 S, SO 2 , CS 2l HCN, COS or mercaptans as impurities.
  • These fluid streams can be, for example, gas streams (such as natural gas, refinery gas, the oxidation of organic organic materials, such as organic waste coal or petroleum, or reaction gases formed in the composting of waste materials containing organic substances).
  • the removal of the acid gases is of particular importance for various reasons.
  • the content of sulfur compounds in natural gas must be reduced by suitable treatment measures directly at the natural gas source, because the sulfur compounds also form acids in the water often carried by natural gas, which have a corrosive effect.
  • predetermined limit values for the sulfur-containing impurities must therefore be observed.
  • the reaction gases generated in the oxidation of organic materials, such as organic waste, coal or petroleum, or in the composting of waste materials containing organic substances, must be removed in order to prevent the emission of gases which can damage nature or affect the climate.
  • Typical physical solvents are cyclotetramethylene sulfone (sulfolane) and its derivatives, aliphatic acid amides (acetylmorpholine, N-formylmorpholine), NMP (N-methylpyrrolidone), propylene carbonate, N-alkylated pyrrolidones and corresponding piperidones, methanol and mixtures of dialkyl ethers from polyethylene glycols ®, Union Carbide, Danbury, Conn., USA).
  • chemical solvents are used, the mode of action of which is based on chemical reactions in which, after absorption, the dissolved acid gases are present in the form of chemical compounds.
  • ions are formed from inorganic bases (eg Potash solution in the Benfield process) or organic bases (eg alkanolamines) when acid gases are dissolved.
  • the solvent can be regenerated by relaxing to a lower pressure or stripping, the ionic species reacting back to acid gases and / or being stripped off using steam. After the regeneration process, the solvent can be reused.
  • Preferred alkanolamines used to remove acid gas contaminants from hydrocarbon gas streams include monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), diethylethanolamine (DEEA), diisopropylamine (DIPA), aminoethoxyethanol (AEE) and methyldiethanolamine (MDEA).
  • MEA monoethanolamine
  • DEA diethanolamine
  • TEA triethanolamine
  • DEEA diethylethanolamine
  • DIPA diisopropylamine
  • AEE aminoethoxyethanol
  • MDEA methyldiethanolamine
  • the fluid streams are brought into contact with the washing solution in an absorption step. It is known from "Gas Purification”, Arthur Kohl, Richard Nielsen, Gulf Publishing Company, Houston, Texas, 1997, 5th edition, Chapter 3, Subchapter Amine Plant Corrosion, 187-230, to carry out this absorption step in steel washing columns. It is also described (loc. Cit) that the steel, unless expensive high-alloy steels are used, is attacked by corrosion due to the proportion of acid gases. This considerably limits the lifespan of the systems.
  • the object was therefore to provide a device for absorbing acid gases from fluid streams comprising a scrubbing column, in which the scrubbing column is largely inert to the fluid streams.
  • the fluid stream mostly a starting gas rich in acidic gas components (raw gas) is brought into contact with an absorbent in an absorption step in an internal washing column, whereby the acidic gas components are at least partially washed out.
  • the source gas is generally natural gas or a gas stream that is formed in the following ways:
  • Organic substances which are subjected to oxidation are usually fossil fuels such as coal, natural gas or petroleum or waste materials containing organic substances.
  • Waste materials containing organic substances which are subjected to oxidation, composting or storage are primarily household waste, plastic waste or packaging waste.
  • the organic substances are mostly oxidized with air in conventional combustion plants.
  • composting and storage of waste materials containing organic substances is generally carried out in landfills.
  • Bacterial decomposition takes place e.g. in common biogas plants.
  • these gas streams contain less than 50 mg / m 3 sulfur dioxide under normal conditions.
  • the starting gases can either have the pressure which corresponds approximately to the pressure of the ambient air, for example normal pressure or a pressure which deviates from normal pressure by up to 0.2 bar. Furthermore, the starting gases can have a pressure higher than 0.2 bar than normal pressure, a pressure up to 20 bar.
  • Source gases with a higher pressure than are considered by compressing the source gases with the pressure which is close to the pressure of the ambient air or by producing the source gas at a higher pressure, for example by oxidation of organic substances with compressed air. The resulting volume flow of the gas is thereby reduced and the partial pressure of the acid gases to be separated, which is advantageous for absorption and the need for regeneration.
  • the compression effort investment and operating costs
  • the possibly higher investment costs due to the use of printing devices are disadvantageous, so that there is an optimum cost here.
  • Preferred absorbents are e.g. chemical solvents selected from the group consisting of
  • Solutions consisting mainly of aliphatic or cycloaliphatic amines with 4 to 12 carbon atoms, alkanolamines with 4 to 12 carbon atoms, cyclic amines in which 1 or 2 nitrogen atoms together with 1 or 2 alkanediyl groups form 5-, 6- or 7-membered rings, mixtures of the above Solutions, aqueous solutions of the above mixtures and
  • aqueous solutions containing salts of amino acids aqueous potash solutions, which may contain piperazine or methylethanolamine, aqueous NaOH or lime milk.
  • Solutions consisting mainly of monoethanolamine (MEA), diethanolamine (DEA), triethanolamine (TEA), diethylethanolamine (DEEA), diisopropylamine (DI PA) and aminoethoxyethanol are particularly preferred as the chemical solvent
  • AEE methyldiethanolamine
  • MDEA methyldiethanolamine
  • the absorbent described in US Pat. No. 4,336,233 has proven particularly useful. It is an aqueous solution of methyldiethanolamine (MDEA) and piperazine as an absorption accelerator or activator (aMDEA®, BASF AG, Ludwigshafen).
  • MDEA methyldiethanolamine
  • aMDEA® piperazine as an absorption accelerator or activator
  • the washing liquid described there contains 1.5 to 4.5 mol / l methyldiethanolamine (MDEA) and 0.05 to 0.8 mol / l, preferably up to 0.4 mol / l piperazine.
  • Physical solvents selected from the group consisting of cyclotetramethylene sulfone (sulfolane) and its deri- vate, aliphatic acid amides (acetylmorpholine, N-formylmorpholine), NMP (N-methylpyrrolidone), propylene carbonate, N-alkylated pyrrolidones and corresponding piperidones, methanol and mixtures of dialkyl ethers of polyethylene glycols.
  • aliphatic acid amides acetylmorpholine, N-formylmorpholine
  • NMP N-methylpyrrolidone
  • propylene carbonate N-alkylated pyrrolidones and corresponding piperidones
  • methanol and mixtures of dialkyl ethers of polyethylene glycols methanol and mixtures of dialkyl ethers of polyethylene glycols.
  • the inert wash columns used in the process according to the invention consist essentially of plastics, selected from the group consisting of polyvinyl chloride, polyethylene, polypropylene, polyvinylidene fluoride, ethylene chlorotrifluoroethylene copolymers (Halar® from Allied Chemical Comp.), Polyfluoroethylene propylene, perfluoroalkoxy polymers, copolymers of Tetrafluoroethylene and perfluoro vinyl ether, polytetrafluoroethylene. These plastics are preferably glass fiber reinforced. Also suitable are washing columns made of steel, the interior of which is coated with plastic or rubber.
  • Suitable inert wash columns are, for example, packing, packing and plate columns. Only inert wash columns are preferably used as absorbers, but it is also possible to use them in combination with other known absorbers such as membrane contactors, radial flow washers, jet washers, Venturi washers and rotary spray washers or washing columns made of steel.
  • the treatment of the fluid stream with the absorbent is preferably carried out in an inert wash column in countercurrent. The fluid is generally fed into the lower region and the absorbent into the upper region of the column.
  • the temperature of the absorbent in the absorption step is generally about 40 to 100 ° C, when using a column, for example 40 to 70 ° C at the top of the column and 50 to 100 ° C at the bottom of the column.
  • the total pressure in the absorption step is generally about 0.5 to 20 bar, preferably about 0.7 to 12 bar, particularly preferably 0.7 to 6.
  • the pressure is particularly preferably at normal pressure or a pressure which is from normal pressure to deviates to 0.2 bar.
  • a low in acidic gas components i.e. received a product gas depleted in these components (Beigas) and an absorbent loaded with acid gas components.
  • plastic absorption columns are only used up to a pressure of 5 bar for design reasons.
  • the use of plastic absorption columns is in principle also possible at higher pressures, but in such cases, because of the generally lower strength of the plastic compared to steel, comparatively high wall thicknesses are required.
  • steel absorption columns, the interior of which is coated with plastic or rubber, are therefore preferred.
  • the method according to the invention can comprise one or more, in particular two, successive absorption steps.
  • the absorption can be carried out in several successive substeps, the raw gas containing the acidic gas components being brought into contact with a substream of the absorbent in each of the substeps.
  • the absorbent with which the raw gas is brought into contact can already be partially loaded with acidic gases, ie it can be, for example, an absorbent that was returned from a subsequent absorption step to the first absorption step, or partially regenerated absorbent.
  • the absorbent with which the raw gas is brought into contact can already be partially loaded with acidic gases, ie it can be, for example, an absorbent that was returned from a subsequent absorption step to the first absorption step, or partially regenerated absorbent.
  • the method according to the invention is carried out in such a way that the fluid containing the acid gases is first treated in a first absorption step with the absorbent at a temperature of 40 to 100 ° C., preferably 50 to 90 ° C. and in particular 60 to 90 ° C. becomes.
  • the fluid depleted in acidic gases is then treated in a second absorption step with the absorption medium at a temperature of 30 to 90 ° C., preferably 40 to 80 ° C. and in particular 50 to 80 ° C.
  • the temperature is 5 to 20 ° C lower than in the first absorption stage.
  • the acidic gas components can be released in a conventional manner (analogously to the publications cited below) from the absorbent loaded with the acidic gas components in a regeneration step, a regenerated absorbent being obtained.
  • the regeneration step the loading of the absorbent is reduced and the regenerated absorbent obtained is preferably subsequently returned to the absorption step.
  • the regeneration step includes at least relieving the pressure of the loaded absorbent from a high pressure, as prevails when the absorption step is carried out, to a lower pressure.
  • the pressure relief can take place, for example, by means of a throttle valve and / or an expansion turbine.
  • the regeneration with a relaxation stage is described, for example, in the publications US 4,537,753 and US 4,553,984.
  • the acidic gas constituents can be released in the regeneration step, for example, in an expansion column, for example a vertically or horizontally installed flash tank or a countercurrent column with internals.
  • an expansion column for example a vertically or horizontally installed flash tank or a countercurrent column with internals.
  • Several relaxation columns can be connected in series, in which different pressures is regenerated. For example, in a pre-expansion column at high pressure, which is typically approx. 1.5 bar above the partial pressure of the acidic gas constituents in the absorption step, and in a main expansion column at low pressure, for example 1 to 2 bar absolute, regeneration can be carried out.
  • the last relaxation stage can also be carried out under vacuum, which is generated, for example, by means of a water vapor emitter, optionally in combination with a mechanical vacuum generator, as described in EP-A 0 159 495, EP-A 0202 600, EP-A 0 190 434 and EP-A 0 121 109 (US 4,551,158).
  • the absorbent according to the invention has a high loading capacity with acid gases, which can also be easily desorbed again. As a result, energy consumption and solvent circulation can be significantly reduced in the method according to the invention.
  • FIG. 1 schematically shows a device in which the absorption stage is carried out in one stage and the relaxation stage in two stages.
  • the starting gas (hereinafter also referred to as feed gas) is fed via line 1 into the lower region of the absorber 2.
  • the absorber 2 is a column which is packed with packing elements in order to effect the mass and heat exchange.
  • the absorbent which is regenerated absorbent with a low residual acid gas content, is fed via line 3 to the top of the absorber 2 in countercurrent to the feed gas.
  • the gas depleted in acidic gases leaves the absorber 2 overhead (line 4).
  • the absorbent enriched with acidic gases leaves the absorber 2 at the bottom via line 5 and is introduced into the upper region of the high-pressure expansion column 6, which is generally operated at a pressure which is above the CO 2 partial pressure of the absorber Raw gas lies.
  • the expansion of the absorption medium is generally carried out with the aid of conventional devices, for example a level control valve, a hydraulic turbine or a pump running in reverse. When relaxing, most of the dissolved non-acidic Gases and a small part of the acidic gases released. These gases are discharged via line 7 from the high-pressure expansion column 6 overhead.
  • the absorbent which is still loaded with the majority of the acid gases, leaves the high-pressure expansion column via line 8 and is heated in the heat exchanger 9, a small part of the acid gases being able to be released.
  • the heated absorption medium is introduced into the upper region of a low-pressure expansion column 10, which is equipped with a packed packing in order to achieve a large surface area and thus to release the CO 2 and establish the equilibrium.
  • a low-pressure expansion column 10 most of the CO 2 and H 2 S are released almost completely by flashing. In this way, the absorbent is regenerated and cooled at the same time.
  • a reflux condenser 11 with a collecting tank 12 is provided in order to cool the released acid gases and to condense part of the steam.
  • the majority of the acidic gas leaves the reflux condenser 11 via line 13.
  • the condensate is pumped back to the top of the low-pressure expansion column 10 by means of a pump 14.
  • the regenerated absorbent which still contains a small part of the CO2, leaves the low-pressure expansion column 10 at the bottom via line 15 and is applied to the top of the absorber 2 by means of pump 16 via line 3.
  • Fresh water can be fed in via line 17 to compensate for the water discharged with the gases.
  • FIG 2 shows schematically an apparatus for performing the method according to the invention using a two-stage absorber and a two-stage relaxation.
  • the absorber comprises the raw absorber 1 and the pure absorber 2.
  • the feed gas 20 is fed via line 3 into the lower region of the raw absorber 1 and treated in countercurrent with regenerated absorbent which is applied to the top of the raw absorber 1 via line 4 and is somewhat acidic Contains gases.
  • regenerated absorbent is added via line 5, which essentially no longer contains acid gases.
  • Both parts of the absorber contain a packing to effect the mass and heat exchange between the raw gas and the absorbent.
  • the treated gas leaves the pure absorber 2 overhead (line 6).
  • the absorption medium loaded with acid gases is discharged at the bottom of the raw absorber 1 and fed via line 7 into the upper region of the high-pressure expansion column 8.
  • the column 8 is equipped with a packing and is operated at a pressure which is between the pressure in the absorber and the subsequent low-pressure expansion column 11.
  • the expansion of the absorbent loaded with acidic gases takes place with the aid of conventional devices, for example a level control valve; a hydraulic see turbine or an inverted pump.
  • the high pressure release releases most of the dissolved non-acidic gases as well as a small part of the acidic gases. These gases are discharged from the high-pressure expansion column 8 overhead via line 9.
  • the absorbent which is still loaded with the majority of the acid gases, leaves the high-pressure expansion column 8 via line 10 and is fed into the upper region of the low-pressure expansion column 11, where most of the CO2 and H2S are released by flashing , The absorbent is regenerated in this way.
  • the low pressure expansion column 11 is equipped with a packing in order to provide a large surface for the heat and mass transfer.
  • a reflux condenser 12 with 20 condensate container 13 is provided in order to cool the acidic gases emerging overhead from the low-pressure expansion column 11 and to condense some of the steam.
  • the uncondensed gas which contains the majority of the acid gases, is discharged via line 14.
  • the condensate from the condensate tank 13 is fed via pump 15 to the top of the low-pressure expansion column 11.
  • the partially regenerated absorbent which still contains some of the acid gases, leaves the low-pressure expansion column 11 at the bottom via line 16 and is split into two partial streams.
  • the larger partial flow is fed via pump 17 and line 4 to the top of the raw absorber 1, whereas the smaller part is heated via line 18 by means of pump 19 in the heat exchanger 20.
  • the heated absorbent is then fed into the upper area of the stripper 21, which is equipped with a pack.
  • the majority of the absorbed CO 2 and H 2 S is stripped out by means of steam, which is generated in the reboiler 22 and fed into the lower region of the stripper 21.
  • the absorbent leaving the stripper 21 at the bottom via line 23 has only a low residual content of acid gases.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Gas Separation By Absorption (AREA)
  • Treating Waste Gases (AREA)
  • Processing Of Solid Wastes (AREA)
  • Treatment Of Sludge (AREA)

Abstract

Procédé de désacidification d'un flux de fluide contenant des gaz acides en tant qu'impuretés, qui consiste à mettre en contact étroit le flux de fluide et un absorbant lors d'au moins une étape d'absorption à une pression de 0,5 à 11 bars, à condition que l'étape d'absorption et, dans le cas de plusieurs étapes d'absorption, qu'au moins une des étapes d'absorption soit effectuée dans une colonne de lavage inerte dont la surface interne est constituée essentiellement de plastique ou de caoutchouc.
EP04739463A 2003-06-05 2004-05-29 Procede de desacidification d'un flux de fluide a l'aide d'une colonne de lavage inerte et dispositif correspondant Withdrawn EP1633458A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE2003125358 DE10325358A1 (de) 2003-06-05 2003-06-05 Verfahren zum Entsäuern eines Fluidstroms mittels einer inerten Waschkolonne und Vorrichtung hierzu
DE2003134002 DE10334002A1 (de) 2003-07-25 2003-07-25 Verfahren zum Entsäuern eines Fluidstroms mittels einer inerten Waschkolonne und Vorrichtung hierzu
PCT/EP2004/005849 WO2004108244A2 (fr) 2003-06-05 2004-05-29 Procede de desacidification d'un flux de fluide a l'aide d'une colonne de lavage inerte et dispositif correspondant

Publications (1)

Publication Number Publication Date
EP1633458A2 true EP1633458A2 (fr) 2006-03-15

Family

ID=33512381

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04739463A Withdrawn EP1633458A2 (fr) 2003-06-05 2004-05-29 Procede de desacidification d'un flux de fluide a l'aide d'une colonne de lavage inerte et dispositif correspondant

Country Status (4)

Country Link
US (1) US20060156923A1 (fr)
EP (1) EP1633458A2 (fr)
JP (1) JP2006526496A (fr)
WO (1) WO2004108244A2 (fr)

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