• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a process for the desulfurization of a gas mixture containing H 2 S and CO 2 by means of selective absorption of the H 2 S into a basic absorption medium and subsequent oxidation of the absorbed H 2 S with an oxidizing agent which is characterized in that i) a H 2 and / or gas mixture to be desulphurised or CH4-containing, combustible biogas is used; ii) after the absorption step, a phase separating step for separating the liquid phase in the form of the sulfide-enriched absorbent from the gas phase containing the combustible gas components is performed; and iii) contacting the thus degassed liquid phase with an oxidizing agent to oxidize the sulfide to elemental sulfur and / or higher oxidation states of the sulfur.
    公开号:AT514460A1
    申请号:T505/2013
    申请日:2013-06-20
    公开日:2015-01-15
    发明作者:Michael Dr Harasek；Aleksander Dr Makaruk
    申请人:Tech Universität Wien；
    IPC主号:
    专利说明:

    The present invention relates to a method and an apparatus for the desulphurisation of gas mixtures, more particularly mixtures containing a combustible gas component, e.g. Methane, hydrogen, carbon monoxide or hydrocarbons.
    Such combustible components are - apart from gaseous fossil fuels such as natural gas or shale gas - for example in gas mixtures resulting from the anaerobic fermentation (biogas) or the thermal gasification of biomass. As the latter become increasingly important, the term "biogas" for combustible component-containing gas mixtures to be desulphurised will generally be referred to as "biogas". second hand.
    In such gas mixtures, H2S is frequently included as a corrosive, environmentally harmful and toxic component which may be subject to further treatment or use of the gas, such as e.g. catalytic synthesis, grid injection or power production, must be removed from it. For gas desulfurization many different processes are known, which can be differentiated according to the respective inward separation principle: adsorption (eg on activated carbon or metal oxides), absorption (eg in alkaline solutions), catalytic conversion (eg in the Claus process), microbiological / bacterial degradation processes as well as membrane separations.
    The present invention relates to desulfurization processes based on a combination of absorption and oxidation (to elemental sulfur or higher oxidation states thereof).
    The desulphurization of gas mixtures containing CO2 usually seeks to remove H2S as selectively as possible in relation to CO2, as parasitic CO 2 removal causes an increased demand for equipment and plant capacity. In the case of absorptive removal, which generally involves absorption of H 2 S into aqueous alkaline solutions (eg NaOH, KOH) to form sulfides or hydrogen sulfides (eg Na 2 S, NaHS), the carbonate formed upon co-absorption of CO 2 (eg Na 2 CO 3 ) are subsequently reacted with H2S to the desired sulfide, but for the time being larger amounts of absorbent (caustic) are required to bind the same amount of H2S.
    As a solution to the problem, contact times between the gas mixture to be desulphurized and the absorbent have been made very short, e.g. in the hundredth of a second range, since then H2S is preferably absorbed; see, e.g. CA 547,215A. This preferred absorption can be achieved by the addition of metal chelates to the absorbent, e.g. in CA 1 304 913 C, and / or applying high pressures, as described in EP 370.145 A1.
    Alternatively, several absorbents of different pH (see, e.g., U.S. 4,585,630) or one and the same multi-gas absorbent may be used sequentially (US 4,395,385). In between, separation of the desulphurised gas stream from the H2S-enriched absorbent (phase separation) can take place.
    The absorbent is preferably regenerated in all cases and recycled to the absorption stage. Regeneration may be accomplished, for example, by desorbing and expelling the absorbed gases (H2S, CO2) by steam steaming (" steam stripping ") and / or increasing the temperature (see, for example, US Pat. No. 2,886,405 and EP 004,043 A1) and / or US Pat the absorption is carried out at an elevated pressure which is released in the subsequent regeneration of the absorbent, whereby an (additional) part of the absorbed gas escapes, see for example EP 046.061 A1. In the latter document, the utility of the thus obtained H2S-containing gas stream in the Claus process, i. Oxidation to elemental sulfur, mentioned.
    No. 6,365,099 B1 discloses a process in which absorption and oxidation of H 2 S in gas mixtures are carried out simultaneously by injecting a mixture of absorbent (aqueous base) and oxidizing agent (hydrogen peroxide, H 2 O 2) into the gas. In DE 101 19 991 A1, by contrast, H 2 O 2 as oxidizing agent is added to the absorbent enriched with H 2 S or at the same time to the gas passed through a column in order to oxidize sulphide to sulphate. The latter can be used in the sequence to absorptively remove ammonia from the gas mixture to be purified. According to WO 2008/000388 A1, the H2O2 is directly linked to the absorption stage, i. in the absorbent in the absorption column, added to produce again sulfate and subsequently ammonium sulfate, which is used for example as a fertilizer application.
    Finally, according to WO 2009/067333 A1, the gas mixture to be desulphurized in the column is brought into contact only with a solution of the oxidizing agent, which is preferably adjusted to a pH between 3 and 8. As an oxidizing agent, preferably Η202 is again used for cost reasons in order to oxidise H2S to elemental sulfur, which is separated from the solution.
    In the course of their research, the inventors have now found that the processes described in the latter documents sometimes entail a high risk potential, since H202 in aqueous solution is known to decompose into H 2 O and O 2. This decomposition is effected by metal surfaces or ions as well as other ions, e.g. OH ", catalyzed, thus also in alkaline solution. Since the resulting oxygen can also contribute to the usually intended oxidation of the H2S to elemental sulfur or sulfate, such decomposition according to the prior art is often not disturbing, but sometimes even desirable.
    However, in the desulfurization of " biogas ", that is, gas mixtures containing combustible components, highly explosive gas mixtures may be produced when the oxygen desorbs from the liquid to the gas phase, so that some of the above-described methods for biogas treatment are not or only with elaborate safety precautions are applicable.
    The aim of the invention was therefore the development of an improved method for ab-sorptive desulfurization of biogas and other combustible components contained border gas mixtures, and a corresponding device for its implementation.
    DISCLOSURE OF THE INVENTION
    This object is achieved in a first aspect of the present invention by providing a process for the desulfurization of a gas mixture containing H2S and CO2 by selective absorption of the H2S into a basic absorbent and subsequent oxidation of the absorbed H2S with an oxidizing agent which is characterized in that: i) as combustible biogas containing H2 and / or CH4 is used as the gas mixture to be desulfurized; ii) after the absorption step, a phase separating step for separating the liquid phase in the form of the sulfide-enriched absorbent from the gas phase containing the combustible gas components; and iii) contacting the thus degassed liquid phase with an oxidizing agent to oxidize the sulfide to elemental sulfur and / or higher oxidation states of the sulfur.
    In this way it is ensured that substantially no combustible gas components come into contact with the oxidizing agent, so that even with the use of H 2 O 2, the generally preferred oxidizing agent, there is no danger that explosive gas mixtures could form. In addition, even when using H 2 O 2, neither acidic pH of the absorbent need be adjusted, which would reduce the rate of absorption, nor avoid the presence of metal surfaces or heavy metal ions to inhibit decomposition.
    Thus, also in the present invention, for cost and availability reasons, H 2 O 2 is the preferred oxidizing agent and an aqueous solution of an alkali metal hydroxide such as e.g. NaOH or KOH, a preferred absorbent although neither the absorption nor the oxidizing agent is specifically limited. Thus, for example, solutions of metal carbonates, preferably alkali metal carbonates, metal oxides or other metal hydroxides or other basic solutions, such as e.g. aqueous ammonium carbonate or alkanolamine.
    Further, according to the present invention, it is preferable to oxidize the sulfide only to elemental sulfur and not to higher oxidation states such as sulfite or sulfate since much smaller amounts of oxidizing agent are required. For example, comparing the oxidation reactions to elemental sulfur and to sulfate requires only a quarter of the amount of oxidant in the former case since the transition from S2 'to S ° requires the transition of two electrons, while to SO42' it is eight electrons. If restricted to the more rapid oxidation to elemental sulfur shorter residence times can be set in the oxidation reactor.
    In preferred embodiments of the invention, further, contact times between the gas mixture to be desulphurized and the absorbent of less than 0.1 s, less than 0.08 s or less than 0.05 s are set in the absorption step in a known manner in order to preferentially absorb H 2 S and reduce the absorption of Suppress C02.
    In a second aspect, the present invention provides an apparatus for carrying out the method according to the invention, more particularly a device for desulfurizing a gas mixture containing H2S and CO2 by means of selective absorption and subsequent oxidation comprising at least one " absorption reactor " said first reactor for the chemisorption of the gas mixture to be desulphurised into the absorbent and at least one " oxidation reactor " for the reaction of the H2S-enriched absorbent with oxidizing agent, characterized in that: for the desulphurisation of combustible components, e.g. I) between the at least one absorption reactor and the at least one oxidation reactor, at least one separator for phase separation of a mixture of liquid phase and gaseous phase formed in the at least one absorption reactor is interposed between the gas mixtures containing H2 and / or CH4; and ii) from the at least one separator opens a gas-tight line for transferring the liquid phase to the (the) oxidation reactor (s).
    With such a device according to the present invention, analogously to the process according to the invention, it is ensured that substantially no combustible gas components come into contact with oxidizing agents or decomposition products thereof, whereby the process according to the first aspect of the invention also using H2O2 as oxidizing agent in the device of the Invention is feasible.
    The reactors, that is to say both the absorption reactor (s) and the oxidation reactor (s), are preferably selected from stirred reactors, static mixers and tubular reactors in order to provide a cost-effective device in comparison with the prior art desulfurization systems to provide low space requirements. At present, static mixers are particularly preferred which, in addition to the above advantages, ensure good mixing at a high throughput.
    As the separator, it is preferable to use a contact separator, e.g. Lamella separators, and centrifugal separators, e.g. Cyclones, selected droplet separator for use, although for example, baffles or demisters made of wire mesh come into question.
    The gas-tight conduit between the separator and the oxidation reactor may comprise, for example, check valves or flaps and / or float-controlled or electronically level-controlled arresters (e.g., level switch controlled condensate pumps) to prevent backcombination of the degassed H2S laden absorbent with combustible gas components. At appropriate levels of pressure in the absorption and oxidation stages, the conduit can become the same
    Purpose also simply include a siphon, which is a cost effective solution.
    For the transport of the gas and liquid streams involved in the process, some of the required inlets and outlets to or from the reactors, the arrangement and operation of which are familiar to the average person skilled in the art, can be pressurized, comprise single or two-fluid nozzles, or even simple tube inlets, optionally in combination with venturi nozzles. Preferably, pressurization may be directly with recycled desulfurized product gas (e.g., methane) obtained in the process of this invention, for example at a pressure of 5 bar. Gas compressors or fluid pumps required for smooth operation should be provided at appropriate locations, as will be understood by those skilled in the art, as well as the provision of additional components of the device, such as those shown in Figs. Storage tanks for substances involved in the process and mixtures of substances, pH probes for measuring the pH of the process streams, or preferably electronic control devices for pumps and / or valves and the like.
    The aqueous base used as absorbent, e.g. NaOH may further be prepared in preferred embodiments immediately prior to use in the method of the invention, e.g. by dissolving solid NaOH or diluting a concentrated NaOH solution in the required amount of water. For example, it can be assumed that commercially available 50% NaOH, which is diluted to the desired concentration.
    BRIEF DESCRIPTION OF THE DRAWING
    For purposes of illustration, and not by way of limitation, a preferred embodiment of the present invention will be described more fully hereinafter with reference to the accompanying drawing, Fig. 1, which is a flow diagram of a preferred embodiment of the invention.
    DETAILED DESCRIPTION OF THE INVENTION
    In the flow chart of Fig. 1 sources or reservoirs of the starting materials are indicated on the left, i. for at least one combustible gas containing sulfur-containing gas mixture SG, water W, absorbent A and oxidant O.
    Absorbent A in this example is aqueous NaOH, e.g. a cost-effective commercially available 50% solution, which is conveyed from a tank 10 by means of a pump 11 to the mixing point 9, where it is combined with fresh water W, which is also passed via a control valve (or a pump) 7 to the mixing point 9, in turn, a simple tube entry, a T or Y-piece or the like, but also a mixing unit, such as a static mixer may be, which may be provided in addition to or instead of the subsequent mixer 12. In the water supply a flow meter 8 is shown, based on which the water flow is adjustable.
    As an alternative to the 50% solution, it is also possible to prepare a solution of desired concentration from solid NaOH (or KOH, generally suitable bases suitable for this purpose) and water, which is not preferred due to the more complicated handling (solids addition, heat of reaction) ,
    From the mixing point 9, the mixture passes to the mixer 12, preferably a static mixer, where a homogeneous solution having the desired concentration (e.g., 10 or 20%) is formed.
    This is brought into contact with the biogas SG to be desulphurized at 6, which is preferably a Venturi nozzle in which the gas with a suitable choice of the flow parameters (pressure, viscosity, dimensions, etc.) sucks or entrains the liquid absorbent as it were. Alternatively, component 6 may also be used as a spray contact, e.g. be designed as a one- or two-fluid nozzle.
    From there, the mixture of biogas to be desulphurized and absorption medium is conducted into at least one first reactor, the absorption reactor 1. These are, as mentioned above, preferably a tubular reactor or, more preferably, a static mixer with which high flow rates, i. short residence times, and good mixing can be achieved. Short residence times lead to a preferential chemisorption of H2S towards CO2, which results in an increased accumulation of the adsorbent with H2S - compared to CO2. This also reduces the total amount of absorbed gas, so less caustic is needed to neutralize the CO2 and generally reduces the volume of process streams to be transported through the plant, which is why e.g. The downstream components of the system can be made smaller.
    From the absorption reactor 1, the resulting mixture of liquid and gas according to the present invention enters the separator 3, in which the phases are separated. This is preferably done in accordance with the present invention by means of a droplet separator which, as mentioned above, consists of contact separators, e.g. Lamella separators, and centrifugal separators, e.g. Cyclones, can be selected. Preferably, it is a demister of wire mesh or knit or a baffle separator (" coalescence separator ").
    The combustible gas thus separated from the liquid and desulfurized by absorption of the H 2 S into the liquid absorbent is conducted to the gas outlet G, while the liquid phase, i. Preferably, the H2S enriched liquid absorbent is drained and passed to the oxidation reactor 2.
    It is essential according to the present invention that no backmixing between the liquid phase and the gas phase, which contains combustible components such as methane, can take place, so that no explosive gas mixtures can occur due to the ingress of oxygen or the like.
    The liquid discharge 4 from the separator 3 is effectively sealed from the latter for this reason. The choice of means is not particularly limited and depends, inter alia, on the intended throughput of the plant and the selected pressure conditions. For example, non-return valves or flaps and / or float-controlled or electronically level-controlled arresters come into question. At suitable pressure levels before and after the separator, i. In the absorption and oxidation stages of the plant, the liquid drainage may also simply comprise a siphon, which is a preferred, inexpensive solution. Such is shown in Fig. 1 as reference numeral 5, but here is only representative of any means for sealing the line 4 relative to the separator 3.
    The conduit 4 may further comprise detectors, as also schematically illustrated in Fig. 1, for example for pH measurement (reference 15) or conductivity measurement (reference 16) for the composition of the liquid phase, especially with respect to the sulphide content to investigate and to be able to regulate the process flows accordingly - (semi) automatically or by hand.
    At mixing point 17, for the analogous applies as previously for mixing point 9, the enriched with sulfide and freed of combustible gas absorbent with oxidant O is mixed, which is funded by a pump 14 from a supply 13. Subsequently, the liquid mixture is passed into the oxidation reactor 2, where the oxidation of the sulphide to elemental sulfur or higher oxidation states thereof, e.g. Sulphite or sulphate, is completed.
    As already the absorption reactor 1, the oxidation reactor 2 is preferably selected from stirred reactors, static mixers and tubular reactors, which ensures a good mixing at high throughputs and low cost with low space requirements, especially when using static mixer.
    The oxidation reactor 2 may preferably comprise a heat exchanger 18 or other suitable means for heat removal, or these may - depending on the concentration-dependent heat of reaction in the reactor - this upstream or downstream. The dissipated heat, for example, to heat others
    Processes in the process, e.g. to adjust the gas temperature before absorption.
    As the last component before the derivation of the sulfur, sulfite and / or sulfate-containing absorbent SA, which - depending on stoichiometry - also contains more or less large amounts of oxidizing agent, Fig. 1 shows a preferred detector 19 for measuring the redox potential to the To determine the efficiency of the oxidation reactor and to be able to regulate the amount of oxidizing agent depending on it.
    It will be understood that this flow sheet shows a relatively simple, exemplary embodiment of the invention which can be easily adapted and optimized by the average person skilled in the art without undue experimentation to the respective circumstances and purposes.
    As mentioned above, in particular, both the reactors 1 and 2 can be provided in multiple design, wherein both the parallel and the serial operation of multiple reactors are possible in each case. Further, not only for these purposes may all the process streams branch in an arbitrary manner, or a process stream or a part thereof may be recycled, e.g. to increase the efficiency of a process step to pressurize or purge (Venturi) nozzles with desulfurized gas or the like.
    Furthermore, other reactors may be provided for additional processes, such as, for example, in a known manner, for ammonia washing, etc., along with corresponding storage containers, etc.
    In any case, as can be seen from the above description, the invention provides an effective method and an associated device by means of which combustible component-containing gas mixtures, in particular biogas from biomass fermentation or gasification, can be desulphurized in an efficient, reliable and economical manner.
    权利要求:
    Claims (10)
    [1]
    1. A process for the desulfurization of a hydrogen sulfide (H2S) and carbon dioxide (CO2) containing gas mixture by selective absorption of H2S in a basic absorbent and subsequent oxidation of the absorbed H2S with an oxidizing agent, characterized in that: i) as the gas mixture to be desulfurized an H2 and / or CH4-containing, combustible biogas is used; ii) after the absorption step, a phase separating step for separating the liquid phase in the form of the sulfide-enriched absorbent from the gas phase containing the combustible gas components; and iii) contacting the thus degassed liquid phase with an oxidizing agent to oxidize the sulfide to elemental sulfur and / or and / or higher oxidation states of the sulfur.
    [2]
    2. The method according to claim 1, characterized in that the oxidizing agent comprises hydrogen peroxide (H2O2).
    [3]
    3. The method according to claim 1 or 2, characterized in that an aqueous solution of an alkali metal hydroxide is used as the absorbent.
    [4]
    4. The method according to any one of claims 1 to 3, characterized in that the sulfide is oxidized to elemental sulfur.
    [5]
    5. The method according to any one of the preceding claims, characterized in that in the absorption step contact times between the desulfurizing the gas mixture and the absorbent of less than 0.1 s, be set under 0.08 s or below 0.05 s.
    [6]
    6. An apparatus for desulfurizing a gas mixture containing H 2 S and CO 2 by means of selective absorption and subsequent oxidation, comprising at least one absorption reactor (1) for the chemisorption of the gas mixture to be desulfurized in the absorbent and at least one oxidation reactor (2) for the reaction of the so with H 2 S enriched absorbent with oxidizing agent, characterized in that: for the desulfurization of combustible components, such as I) between the at least one absorption reactor (1) and the at least one oxidation reactor (2), at least one separator (3) for phase separation of a mixture of liquid phase and gas phase formed in the at least one absorption reactor (1) is; and ii) from the at least one separator (3) opens a gas-tight conduit (4) for transferring the liquid phase to the (the) oxidation reactor (s) (2).
    [7]
    7. Apparatus according to claim 6, characterized in that the reactors (1, 2) are selected from stirred reactors, tubular reactors and in particular from static mixers.
    [8]
    8. Device according to claim 6 or 7, characterized in that the separator (3) is a droplet separator selected from contact separators and centrifugal separators.
    [9]
    9. Device according to one of claims 6 to 8, characterized in that the gas-tight line (4) comprises a float-controlled arrester (5).
    [10]
    10. Device according to one of claims 6 to 9, characterized in that some of the supply and discharge lines to and from the reactors (1, 2) can be pressurized and / or comprise one or more nozzles (6). Vienna, on June 20, 2013

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    引用文献:
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