• 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:
    Method and apparatus for removing sulphur dioxide and possible hydrogen sulphide as well as nitric oxides from exhaust gases by means of sulphides in a liquid phase so that the sulphur is recovered in the form of molten elemental sulphur. The sulphur bearing gas is scrubbed in a scrubber 1 by contact with a sulphide bearing scrubbing solution whose pH is in the range 2.5 to 5 or oxidation-reduction potential is in the range -70 to -250 mV, with respect to a calomel electrode. The used scrubbing solution is passed to an autoclave 2 to generate molten elemental sulphur and a sulphate solution. …<??>The sulphate solution passes to a regeneration stage 3 where barium sulphide is supplied to produce sodium sulphide and barium sulphate. The sodium sulphide passing back to the scrubbing stage 1 and the barium sulphate being reduced 4. Gases from the barium sulphate reduction may be fed into the scrubber. …<IMAGE>…
    公开号:SU1586509A3
    申请号:SU853913606
    申请日:1985-06-26
    公开日:1990-08-15
    发明作者:Тапани Талопен Тимо；Тейе Илмари Пойярви Яакко
    申请人:Оутокумпу Ой (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for the recovery of sulfur dioxide and / or hydrogen sulfide from gases to produce elemental sulfur.
    The purpose of the invention is to reduce the loss of sulfur due to more complete processing of sulfur compounds.
    The method is based on the reaction of the interaction of sulfur dioxide with sulfide in the aqueous phase according to the equation
     + 2S02 SO- + 2S.
    (ABOUT
    In addition to this reaction, several side reactions occur in this process, as a result of which hydrosulfide, hydrosulfite, thiosulfate and tetrathionate, polygonates are formed according to the following equations:
    S- + SO + H-jO (2) 2S- 3SO 2S O - + S .; (3) 5HM SO-3- S jO -; (4)
    S .- + so2 (5)
    S, 0i + nS02 ZgOz-p GOD. (6)
    Depending on the specific metal sulfide, the relative amounts between the components of the reactions (2) - (6) may vary. When using sulphides with low solubility, in particular zinc sulphide, ferrosulphide or manganese sulphide, forms
    SP
    00
    about:
    SP
    CD

    CM
    with more sulphate and elemental sulfur than with high solubility sulphides, in particular sodium sulphide, potassium sulphide, calcium sulphide and barium sulphide. However, irrespective of sulfide, the proportion of adverse side reactions is significant, therefore only part of sulfur dioxide reacts with the formation of elemental sulfur in accordance with equation (1).
    When sulfur dioxide is introduced into an aqueous solution of sodium sulphide, it reacts first, in accordance with the equation of the reaction (2). At the same time, the pH of the solution remains above 10. After uptake of approximately 0.5 mol of sulfur dioxide to each mol of sodium sulfide, the pH quickly drops to about 8-9 and at the same time there is an intense release from the hydrogen sulfide solution. The formation of hydrogen sulfide continues until approximately one mole of sulfur dioxide is adsorbed on each mole of sodium sulfide. After this, the formation of hydrogen sulfide is stopped and the pH value quickly drops to about 2.5-3.5, i.e. after the sulfur dioxide is almost completely absorbed, noticeable hydrogen sulfide formation ceases. After this, part of the sulfur dioxide begins to slip without absorption, but subsequently the absorption rate increases again. I
    When sulfur dioxide is introduced into the sparger, the pH value or redox potential of the sulfide solution is controlled by continuously feeding fresh sodium sulfide solution into the washing solution and discharging the treated washing solution as a flow, resulting in a pH value of 2.5-5, the value redox potential remains in the range from -70 to -260 MB (if measured between standard calrmele and platinum electrodes), the absorption of sulfur dioxide is almost complete. and the amount of simultaneously infusing hydrogen sulfide is insignificant.
    In another experiment, a gas containing sulfur dioxide and hydrogen sulfide is fed into the sulfide solution. The flow parameters of the original sulfide regulate
    similar to the experiment described. In this case, both sulfur dioxide and hydrogen sulfide are almost completely absorbed.
    Similar experiments were also carried out using other sulphides, in particular manganese sulphide, calcium sulphide, barium sulphide and potassium sulphide. The results obtained are similar to those using sodium sulfide.
    When flushing a gas containing sulfur dioxide with a sulfide solution, the rate of excretion of elemental sulfur in accordance with reaction (1) is low, even extremely low, despite the use of some high solubility sulfides. However, reaction (1) can be completed by absorbing sulfur dioxide with a molar sulfide solution at a ratio of 1.8-2.1 with a subsequent solution in a closed autoclave at a high temperature. In this case, sulfur dioxide must be absorbed by sulfide in roughly the stoichiometric ratio indicated by reaction equation (1).
    If the amount of sulfur dioxide adsorbed is less than that which is required in accordance with the indicated stoichiometric ratio, products corresponding to reaction (1) are formed only in a small amount and products are formed in the arm as a result of side reactions, especially thiosulfate, which remain in solution .
    In another experiment, only a water solution of sodium thiosulfate was introduced into the autoclave, where it was kept for 3 hours. As a result of this experiment, only 7% of the thio sulfate undergoes decomposition.
    It has also been established that any excess sulfur dioxide, which is absorbed by the sulfide solution in addition to the stoichiometric amount specified in reaction equation (1), reacts to form sulfuric acid in the autoclave.
    The method is carried out as follows.
    Gases containing sulfur dioxide or sulfur dioxide, together with hydrogen sulfide, are brought into contact with a washing solution or with a suspension of metal sulfide. Fresh powders of sulfide are introduced into the solution or suspension. Wash
    The ability of the solution or suspension is controlled by feeding fresh portions of sulfide.
    The flow rate of the original sulfide is controlled in accordance with the pH value and / or the magnitude of the redox potential measured in the solution, so that the pH value remains in the range of 2.5-5 or the magnitude of the redox potential remains in the range from - 70 to -260 MB, which allows the molar ratio between the absorbed sulfur dioxide and sulfide to be adjusted, taking into account that it corresponds to the stoichiometric ratio indicated in reaction equation (1).
    The used washing solution containing the products according to reactions (2) - (6) is sent to an autoclave. In it, the temperature of the solution is increased to 130–200 ° C, as a result of which reactions proceed to the final result, which corresponds to the equation of reaction (1). The extraction from elemental sulfur falls into the sediment to the bottom of the autoclave, from where it is removed in the molten state. A sulfate solution or suspension is withdrawn from the top of the autoclave.
    The method of regenerating the washing solution depends on the sulfide used. There are two different ways to separate soluble sulphate from the solution, which is available in an autoclave. The sulfate can be crystallized from a solution either by evaporation, and then by crystallizing the sulfate with cooling, or by evaporation of all the liquid in the solution.
    The sulphate recovered by crystallization or evaporation is reduced with carbon, hydrocarbon, carbon monoxide, hydrogen or another reducing agent in the usual way to obtain sulphide, which, after the procedure described, is used to regulate the leaching capacity of the solution.
    The solution that is discharged from the autoclave can also be regenerated by removing sulfate through barium sulfide calcium. In the case of using poorly soluble sulfide, the sulfide and sulfate can be separated.
    15
    20
    25 30
    35
    40
    45 0
    five
    pour, for example, by flotation and / or hydrocyclone.
    The precipitated barium or calcium sulphate is reduced by known technology using carbon, hydrocarbon, carbon monoxide, hydrogen or other reducing agent in a kiln or in a fluidized bed furnace to sulfide, which is reused to regenerate the solution coming from the autoclave.
    A particularly advantageous embodiment of this method is to use sodium sulfate to regulate the leaching capacity of the solution and barium sulfide to regenerate the solution removed from the autoclave. In this case, the washing chemical agent is completely soluble, and there is no any risk of blockage of the washing equipment due to either solid matter deposition or deposition at the bottom of the supply tank. Since there are no solid materials inside the autoclave, unreacted sulphide and precipitated sulphate, elemental sulfur falls to the bottom of the autoclave in almost pure form.
    Potassium sulphide can also be used instead of sodium sulphide. This embodiment of the invention is shown in the drawing.
    The sulfur-containing gases are directed to gas absorption stage I, where any water-soluble sulfide, in particular sodium or potassium sulfide, is also sent. At the stage of absorption of gas, for example, one or two scrubbing reactors may be provided, the pH or the redox potential of the npoNSbiBHoro solution is adjusted so that gas does not contain from the last scrubber reactor relative to the direction of gas flow. neither sulfur dioxide nor hydrogen sulfide. The wash solution containing sodium (or potassium) sulfur compounds is sent to aBTOj inaB 2, in which various sulfur-containing compounds react at elevated pressures and temperatures, with the result that the final product is partially molten sulfur. sodium sulfate solution. The sodium sulfate solution is directed to step 3 of the Yi regeneration, which is also fed sulfide (5ari, barium sulfide, and sodium sulfate and enter into the usual reaction to form sodium sulfide and sulfate (5ari. The sodium sulfide is returned to absorption phydium 1, Barium sulphate is fed to stage 4, reduced, where it is reduced to barium sulfide, for example, by means of carbon: or hydrocarbon. Reducer: e gases from the reduction stage can be sent to the subsequent afterburning 5 and further to stage 1 absorbed together with the solubility of sulphate obtained in an autoclave can be controlled by means of temperature. The choice of sufficiently high temperature ensures crystallization of sulphate. The separation of elemental sulfur and sulphate crystals occurs already in the autoclave as Sulfate crystals are separated from the solution, which is at temperature and pressure, which are formed inside the autoclave, in order to prevent even dissolution, for example, by means of a hydrocyclone or centrifuge. The liberated mass of sulphate crystals is subjected to an immediate reduction of “iy.
    Using poorly soluble sulphides to wash the gases, regenerating the solution that is discharged from the autoclave. Can be produced as described using barium sulfide or Calcium. However, in this case, it is necessary to separate the metal sulfides used for washing from barium or calcium sulfate.
    However, the reduction of zinc sulphate, manganese sulphate or ferrosulphate to sulphides is not as beneficial. In order to ensure the maximum possible absorption of sulfur dioxide and at the same time to ensure the maximum possible release of hydrogen sulfide, the molar ratio, sulfur dioxide and sulfide in the washing solution directed to the washing is maintained below 2, which is optimal for autoclaving. .
    Sufficiently complete absorption of sulfur dioxide and an ideal value.
    0
    five
    0
    five
    0
    five
    0
    five
    0
    five
    The molar ratio between sulfur dioxide and sulphide, required for autoclave treatment, is about 2, cannot be achieved at the same time at the same stage. However, both of these goals can be achieved by carrying out the absorption in two or more stages, and in these cases the scrubber reactors can operate both on the counter-current principle and on the principle of the pr-motor. It is advantageous to regulate the ratio between the molar flows of sulfur dioxide and sulfide, based on pH values or. the redox potential of the latter reactor in the direction of the flow of the solution directly by introducing fresh sulphide portions. At the same time, the pH value of the last reactor in the direction of the gas flow is regulated at the level of 3-5, or the value of the redox potential in the range from -100 to -260 MB by feeding sulfide.
    In a preferred embodiment of this method, the VO-containing gas is passed through 3 scrubber reactors. Fresh washing solution is fed to the 2nd reactor, and then sent from it to the 1st reactor. In the 2nd reactor, the pH value or the redox potential of the solution is adjusted so that in order to effectively remove sulfur dioxide, the pH value is in the range 3 -5 or the magnitude of the redox potential ranged from -100 to -260 MB. Any insignificant amount of hydrogen sulfide that is released in the 2nd reactor is removed in the 3rd reactor by feeding some amount of solution into it. th reactor together with the specified gas. The pH value in the 1st or 3rd reactor is regulated in the range of 2.5-3.5, the magnitude of the redox potential is in the range from -70 to -150 mV, which allows you to adjust the mol. the ratio between the total amount of absorbed sulfur dioxide and the amount of sulphide injected in the range of 1.8-2.1 required for autoclave treatment by feeding a stream of sulphide to the 1st reactor „
    The adjustment of the pH or redox potential of the first reactor in the direction of the outflow of gas at a very precise level is usually made by directly introducing relatively small portions of fresh sulphide into the first reactor, but in some cases such adjustment can also be carried out by feeding the amount of sulfide required for fine adjustment, JQ for example, in the subsequent reactor in relation to the direction of flow.
    When the content of free oxygen in a gas with SOj is absorbed, it is absorbed by the solution, increasing the redox potential due to the oxidation of sulfide. In order to maintain the solubility of the sulphate solution, it is possible to dissolve the crystallization of ferrosulphate.
    When manganese sulfate is crystallized, the required temperature to achieve the appropriate degree of separation is approximately.
    PRI me R 1. The gas containing 20% sulfur dioxide and 80% nitrogen is first served at a flow rate of 1 l / min to a 2-liter bubbler that is filled with water at. The pH of the solution is adjusted by adding a solution of sodium sulfide (concentration of approximately 120 g / l sodium sulfide) using a titrator. The molar ratio is 1.8. In the course of the experiment, the settable pH value is changed in such a way that at first
     - - .4.-i jn at i i vjijbi and began with
    with respect to sulfur dioxide, the effect of 20 it was equal to 3.0 / 3.3 at 25 ° C). VTS JT П П Г ГТ Д nomir Ui Лттт. TU- .. “. V-„ ..
    oxygen should be compensated by adding fresh sulphide portions to the solution:
    In order to preserve the elemental sulfur formed in the washing stage, in the form of a finely dispersed suspension and at the same time in order to prevent clogging of the system, agents that improve wettability can be added to the washing surface of sulfur particles of the washing solution, and such agents can be used for example, natural tannins, in particular tannic extract from quebracho bark.
    Since sulfur is removed from the autoclave in the molten state, the melting point of sulfur determines the limit of the minimum temperature in the autoclave, i.e. the temperature in the autoclave should be higher than approximately lp.
    35
    The magnitude of the redox potential should be from -150 to -160 MB, if measured against a calomel electrode. During the experiment, the pH value to be adjusted is such that it is 4 / 4.2 at and 2.5 / 2 , 3 at 25 ° С and the magnitude of the redox potential was approximately 260 and -100 MB, respectively. At each pH value, the experiment was carried out for 10–12 hours. The results of the washing experiments are summarized in tab. one.
    2 liters of overflow formed during the described experiment, with a pH value of 3 (0-12 h), are sent to an autoclave at 130 ° C, which is kept for 1 h. The resulting elemental sulfur (35.6 g ) is separated from the solution by filtration. The composition of the solution before and after autoclave treatment is presented in table. 2
    The higher the temperature in the autoclave, the faster the products formed during side reactions (2) - (6) enter. in reaction with the achievement of the final result in accordance with reaction (1) о Experiments have shown that already at 130 ° C with Bbmie 90% of the products formed as a result of reactions (2) - (6) decompose in less than 0.5 h. Most optimum temperature in the autoclave 130-150 00 The temperature maintained in the autoclave also depends on the crystallization temperature of the sulfate. Thus, for example, the solubility of ferrosulphate begins to decrease at a temperature approximately higher. At temperatures above main



    A part of the sulphate solution can be separated by the crystallization of ferrosulphate.
    When manganese sulfate is crystallized, the required temperature to achieve the appropriate degree of separation is approximately.
    PRI me R 1. The gas containing 20% sulfur dioxide and 80% nitrogen is first served at a flow rate of 1 l / min to a 2-liter bubbler that is filled with water at. The pH of the solution is adjusted by adding a solution of sodium sulfide (concentration of approximately 120 g / l sodium sulfide) using a titrator. The molar ratio is 1.8. In the course of the experiment, the settable pH value is changed in such a way that at first
     .4.-i jn at ii vjijbi and began with
    it was equal to 3.0 / 3.3 at 25 ° C) ve


    table 3
    The magnitude of the redox potential should be from -150 to -160 MB, if measured against a calomel electrode. During the experiment, the pH value to be adjusted is such that it is 4 / 4.2 at and 2.5 / 2 , 3 at 25 ° С and the magnitude of the redox potential was approximately 260 and -100 MB, respectively. At each pH value, the experiment was carried out for 10–12 hours. The results of the washing experiments are summarized in tab. one.
    2 liters of overflow formed during the described experiment, with a pH value of 3 (0-12 h), are sent to an autoclave at 130 ° C, which is kept for 1 h. The resulting elemental sulfur (35.6 g ) is separated from the solution by filtration. The composition of the solution before and after autoclave treatment is presented in table. 2
    table 3
    Example 2 In the course of the experiment, the pK value is regulated by the addition of calcium sulfide spam (approximately 115 g / l, sulfur content 127 g / l), which is obtained by passing ciepoBo hydrogen through a calcium oxide hydrate slurry (calcium oxide concentration — 250 g / l) to a pH of approximately 8. The rest of example 1. The results obtained are given in
    table 3
    Example 3: 3.5 mol of ferrous sulfate heptohydrate is dissolved in water. Iron sulfide is precipitated by the addition of
    4 mol sodium sulfide. The precipitate is carefully filtered with extreme caution to prevent oxidation. The iron sulphide precipitate is settled in pure water, resulting in 2.5 l of liquid being obtained in a 3-liter bubbler, into which a gaseous compound is subsequently introduced at a flow rate of 1 l / min (0.1 l / min of sulfur dioxide JQ and 0 , 9 l / min of nitrogen) at 60 ° C. .
    The results are presented in Table. four.
    I p and me R 4. The washing solution, J5, which was obtained according to the procedure described in Example 3, and which is withdrawn from the process of the corresponding washing with potassium sulphide, is autoclaved at 201 / C for 20 1 hour.
    The results are summarized in table. five.
    Example 10: SO-containing gas was washed with sodium sulphide solution at a molar ratio of 1.8. The wash solution is then sent to an autoclave and kept there for 1 hour at. The average values of the analysis are shown in Table. eight.
    The proposed method allows, unlike the prototype, to process serog-containing compounds that are formed as a result of side reactions during gas cleaning from 80 and, into sulfur sulfur and sulphate of the corresponding metal, reducing sulfur losses.
    权利要求:
    Claims (2)
    [1]
    1. The method of obtaining elemental sulfur from gases containing sulfur dioxide or its mixture with hydrogen sulfide, comprising washing the gas with a solution or suspension of metal sulfide with the Amount of elemental 25 obtained pH 2.5-5 to obtain a mixture of elemental sulfur, sulfate, sulfite, thiosulfate of the corresponding metal , processing of this mixture into sulfur
    sulfur was 189 g.
    II e r i me r 5. To adjust the pH, magnesium sulphide slurry (5 mol of manganese sulphide per 2 liters of water) is used, which is prepared by precipitating 30 manganese sulphate from a solution of hydrogen sulfide. The essential difference of this experiment is that the flow rate of sulfur dioxide is 100 ml / min and the flow rate of nitrogen is 900 ml / min.
    The results of the experiment with washing are summarized in table. 6
    2 l of the solution from the absorption stage at a pH value of 3 is sent to an auto-dof clav, at 150 ° C, in which it is kept for 1 hour. The resulting 41.9 g of elemental sulfur is separated from the solution by filtration. Consumption of this sulphate solution, reduction of the latter to sulphide and its recirculation to the washing stage,
    It is distinguished by the fact that in order to reduce sulfur losses due to more complete processing of sulfur compounds, at the gas washing stage, the molar ratio of sulfur dioxide to metal sulfide is 1.8-2.1, and the resulting mixture of sulfur compounds is processed at 130-200 C.
    [2]
    2. A method according to claim 1, characterized in that metal sulfide is used as the metal sulfide selected from the group containing a hydrogen sulfide gas that is washed with a sodium sulfide solution at a molar ratio of 1.8. The wash solution is then sent to an autoclave and kept there for 1 hour at. The average values of the analysis are shown in Table. eight.
    The proposed method allows, unlike the prototype, to process serog-containing compounds that are formed as a result of side reactions during gas cleaning from 80 and, into sulfur sulfur and sulphate of the corresponding metal, reducing sulfur losses.
    Invention Formula
    and sulfate, reduction of the latter to sulfide and its recycling to the washing stage,
    It is distinguished by the fact that in order to reduce sulfur losses due to more complete processing of sulfur compounds, at the gas washing stage, the molar ratio of sulfur dioxide to metal sulfide is 1.8-2.1, and the resulting mixture of sulfur compounds is processed at 130-200 C.
    2. A method according to claim 1, characterized in that as the metal sulfide use metal sulfide selected from the group containing
    Table before and after autoclave treatment is listed in Table. 7
    45 cubic potassium, sodium, barium, calcium, zinc, iron, manganese.
    Table 1
    after 60 min
    1060145
    Accumulation expense
    manganese sulphide sludge (5 mol to 2 l, water).
    Table A
    Table 5
    405
    0.05
    Less than 0.05
    Spreadsheets
    Table 7
    Table 8
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    同族专利:
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FI842578A|FI69621C|1984-06-27|1984-06-27|FOERFARANDE FOER AVLAEGSNING OCH TILLVARATAGANDE AV SVAVEL SOMGRUNDAEMNESSVAVEL FRAON SVAVELDIOXID- ELLER SVAVELDIOXID HOCSVAVELVAETEHALTIGA GASER|
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