• 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:
    A process for the simultaneous removal of H2S, SO2 and elemental sulfur from gaseous mixtures, comprises treating the gaseous mixture with a solvent. After the solvent becomes loaded with the components to be removed, it is regenerated and reused. In order to obtain savings in costs and energy, the sulfur is separated from the loaded solvent by lowering the temperature thereof. In this way, chemical regeneration of the scrubbing medium takes place within the cycle eliminating the requirement for outside regenerating apparatus.
    公开号:SU1530091A3
    申请号:SU833655349
    申请日:1983-10-25
    公开日:1989-12-15
    发明作者:Хайзель Михаэль；Ранке Герхард
    申请人:Линде Аг (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to the purification technology of industrial sulfur-containing gases, in particular, to a method for purifying gases containing hydrogen sulfide and sulfur dioxide.
    The aim of the invention is to increase the degree of purification.
    The method consists in the fact that when purifying gases containing hydrogen sulfide and sulfur dioxide, to obtain elemental sulfur, including countercurrent absorption by an organic solvent at 60–120 ° C with the supply of absorbent to the upper part of the column, the sulfur is liberated from the saturated absorbent upon indirect cooling to 20–50 ° C and the recycling of the preheated regenerated absorbent to the absorption stage, before the sulfur is released, the absorbent is kept in the bottom of the column for 3–15 minutes.
    If the source gas contains carbon dioxide, then it is hydrolyzed before absorption.
    with

    cm
    A part of the saturated absorbent in the amount of 10-50 OBL can be removed from the system to remove water accumulated in it from it.
    The absorbent can be additionally supplied to the middle part of the column.
    It is advisable to use as an absorbent toluene or ether polyethylene glycol. It is also possible to use alcohol, ketones, dimethylformamide, glycols of aromatic hydrocarbons, butyrolactone.
    Absorption can be carried out in the presence of a catalyst, for example, N-methyl-pyrrolidone, fine activated carbon or alumina (alumina).
    The method can be carried out in an installation whose scheme is shown in the drawing.
    The installation works as follows.
    Pipeline 1 supplies gas to column 2 containing hydrogen sulphide and sulfur dioxide, for example, Claus process off-gas. In column 2, countercurrent absorption of gas by an organic absorbent, such as toluene or polyethylene glycol ether, is carried out at 60-120 ° C. Before being supplied to the absorber, the absorbent can be cooled using refrigerant 4. ° s Purified ha is discharged through line 5. The absorbent is saturated with sulfur compounds and the mines are kept in the bottom of the column, after which the absorbent is discharged through line 7 to separate elemental sulfur from it alternately (their heat exchangers 8, 9, where the absorbent is cooled up to 20-50 0. When one heat exchanger is clogged with solid elemental sulfur, with the help of pump 10, the absorbent is fed through pipe 11 to another heat exchanger. Then, from the clogged heat exchanger, sulfur is withdrawn in a liquid state through pipeline 12 or 13 .. Preliminarily indirect heating of the respective heat exchanger, for example, low vapor pressure of about 10-50% of the absorbent can be withdrawn via line to the column. -
    15, in which the water collected in it is removed by distillation. From the top of the column 15 through the pipeline 1b
    five
    0
    five
    five
    0
    0
    five
    0
    five
    water vapor is removed, and a purified absorbent is obtained in the bottom of the column, which is recycled to absorption through conduit 17 and 3. The gases carried away by the column head product 15 are separated in separator 18 and added to conduit gas 19.
    Countercurrent absorption can be carried out in the presence of a catalyst, for example, P-methyl-pyrrolidone, which is added to the absorbent through conduit 20. If necessary, a portion of the absorbent can be supplied via conduit 21 to the middle part of the column 2.
    PRI me R 1., 1 kmol / h of waste gas of the Claus process of composition, o6,%: 2, k8 39.82 0, 0.33 16.71, is subjected to countercurrent absorption of 1bЗ g / h fed to the upper part of the toluene column at 70 C. From the upper part of the column, 635.9 kmol / h of purified gas of the composition,% by volume:, 63 C02, bb, 3.8i 10 ob.h / Mln. and 10 p.p./million SOj. Thus, the purification rate is about 99.9. The absorbent saturated with sulfuric compounds is kept in the bottom of the column for 5 minutes, after which elemental sulfur is isolated in the amount of 7 kmol / h by indirect cooling to the central heating station C.
    one
    EXAMPLE 1 Example 1 is repeated with the difference that countercurrent absorption is carried out at a temperature of 120 ° C for 3 minutes and sulfur is liberated by indirect cooling to 50 ° C. In addition, water is removed from the system Output 10 saturated absorbent. The degree of gas purification is 95, the amount of sulfur is 7, kmol / h.
    Froze Example 1 is repeated, with the difference that countercurrent absorption is carried out at 60 ° C for 15 minutes, and sulfur is liberated by indirect cooling to 20 ° C. In addition,% of a saturated absorbent is removed to remove water from the system. The degree of gas purification is 99.2%, the amount of sulfur is 7, kmol / h.
    PRI me R. Example 3 is repeated, with the difference that countercurrent absorption is carried out in the presence of a catalyst, I-methylpyrrolidone,
    in the amount of 0.01 by weight of the absorber, Pm, the degree of gas purification is 5 b, the amount of sulfur l, kmol / h.
    EXAMPLE 5 Example 1 is repeated with the difference that gas of the composition is used, mol.%: 35.83 CO, 29.1 kg; 29.99 1.1 H .; 2, i WITH; 0.86, O, AZ SO, -, 0.25 Ar, - 0, COS. At the same time, before being fed to countercurrent absorption, the gas is heated to l80 ° C and passed over a layer of palladium catalyst. As a result of this treatment, the carbon dioxide content is reduced to 20 vol / ppm, and the hydrogen sulfide content is increased to 8900 ob.h / million. After cooling, the gas is fed to the treatment according to example 1.
    The degree of gas purification is 99.7, the amount of sulfur is 7, And kmol / h.
    EXAMPLE 6 Example 1 is repeated with the difference that 117 g / h of polyethylene glycol ether is used as the absorbent, 50% of which is fed to the upper part of the column, and the remaining 50% to the middle part of the column. In addition, the absorbent is kept in the bottom of the column for 10 minutes and 50% of the saturated absorbent is removed from the system to remove water. At the same time, 625.5 kmol / h of purified gas of composition, vol.%: 50.45 CO., 47.31%, 2.2i + HjO, 7 vol / million are withdrawn from the upper part of the column. H2.S and 6 vol. Ppm 50. The degree of gas purification is 99.9%, the amount of sulfur is 7 kmol / h.
    PRI me R 7 (comparative).
    Example 1 is repeated with the difference that the absorbent is kept in a cube for 2.5 minutes. The degree of gas purification is 80%.
    Comparison of data on the degree of gas purification, given in the prototype and in examples 3, 7, suggests that if the lower limit of the absorbent in the bottom of the column is not met, the goal is almost not achieved.
    PRI me R 8 (comparative).
    Example 3 is repeated with the difference that the absorbent is kept in the bottom of the column for 16 minutes. At the same time
    five
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    about
    5 Q 5
    five
    0
    five
    gas cleaning stump is 99%.
    Comparison of the data on the degree of purification given in the make-up units 7, 8 suggests that if the upper limit of the time for keeping the absorbent in the bottom of the column is not observed, the positive effect is not further enhanced, but rather deteriorates.
    As follows from the examples given, this method provides a high degree of purification (95-99.9%), while in the prototype the degree of purification is 6.5%.
    权利要求:
    Claims (3)
    [1]
    Invention Formula
    1. Method of purification of gases containing hydrogen sulfide and sulfur dioxide, to obtain elemental sulfur, including countercurrent absorption by an organic solvent at 60-120 С
    with the supply of absorbent to the upper part of the column, the release of sulfur from the saturated absorbent during indirect cooling to 20-50 ° C and the recirculation of the preheated regenerated absorbent to the absorption stage, which is aimed at increasing the degree of purification before the release of sulfur the absorbent is kept in the bottom of the column for 3-15 minutes.
    2. A method according to claim 1, characterized in that the source gas, when it contains carbon monoxide, is subjected to a hydrolysis before absorption.
    [2]
    3. The method according to claim 1, characterized in that a portion of the saturated absorbent in an amount of 10-50% by volume is removed from the system and the water accumulated in it is removed from it.
    [3]
    k. Method pop.1, characterized in that the absorbent is added to the middle part of
    u and, respectively, served lonny.
    5. The method according to claim 1 and with the fact that bent is used with ethylene glycol.
    6. Method POP.1, characterized in that the absorption is carried out in the presence of a catalyst.
    distinguished - that as an absorptive toluene or ether
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    同族专利:
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    CA1211614A|1986-09-23|
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2467788C1|2011-06-02|2012-11-27|Сергей Анатольевич Щелкунов|Method of cleaning waste gases from sulfur dioxide|
    RU2545273C2|2010-03-29|2015-03-27|ТюссенКрупп Уде ГмбХ|Method and device for processing acid gas enriched with carbon dioxide in claus process|GB190802719A|1907-03-06|1908-09-24|Walther Feld|Improvements in the Treatment of Sulphur-dioxide and Sulphuretted Hydrogen for the Obtainment of Sulphur therefrom.|
    NL75853C|1949-08-12|
    US2987379A|1958-12-15|1961-06-06|Universal Oil Prod Co|Production of sulfur|
    US2992076A|1959-02-24|1961-07-11|Universal Oil Prod Co|Production of sulfur|
    US3149920A|1961-07-21|1964-09-22|Universal Oil Prod Co|Production of sulfur|
    US3798315A|1970-10-27|1974-03-19|Gas Council|Treatment of gases|
    FR2358187B1|1976-07-12|1978-12-22|Raffinage Cie Francaise|
    FR2358186B2|1976-07-12|1980-12-12|Raffinage Cie Francaise|
    DE2923895C2|1979-06-13|1982-01-28|Davy McKee AG, 6000 Frankfurt|Process for removing hydrogen sulfide and sulfur dioxide from Claus exhaust gases|
    US4250151A|1979-09-04|1981-02-10|Gulf Canada Limited|Recovery of sulfur from gas streams containing sulfur and sulfur compounds in dilute concentration|US5480860A|1988-12-23|1996-01-02|Petrolite Corporation|Methods for reducing sulfides in sewage gas|
    US5851265A|1996-09-03|1998-12-22|Monsanto Company|Selective removal and recovery of sulfur dioxide from effluent gases using organic phosphorous solvents|
    FR2753396B1|1996-09-16|1998-10-30|Inst Francais Du Petrole|METHOD AND DEVICE FOR TREATING A GAS CONTAINING SULFUR HYDROGEN AND SULFUR DIOXIDE COMPRISING A SULFUR DEPLETION STAGE OF RECYCLED SOLVENT|
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    US6162282A|1999-05-10|2000-12-19|Mobil Oil Corporation|Method for determining hydrocarbon saturation of carbon filters in a gas treatment process|
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    US10119948B2|2016-01-06|2018-11-06|Saudi Arabian Oil Company|Sulfur solubility in gas measurement system|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19823239603|DE3239603A1|1982-10-26|1982-10-26|METHOD FOR REMOVING H2S, SO2AND ELEMENTAL SULFUR FROM GAS MIXTURES|
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