• 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 separation of substantially pure NH3 and substantially pure CO2 from a mixture containing NH3, CO2 and water is disclosed. In this process NH3 is separated by rectification in an NHa-separation zone (3), the remaining liquid phase is fed to a CO2-separation zone (18) where gaseous CO2 is separated by rectification, and the resulting liquid phase is fed from the bottom of this zone to a desorption zone (10), where virtually all NH3 and CO2 still contained in this liquid phase are separated as a gaseous mixture. To improve the efficiency of the separation and to decrease the sensitivity of the process to fluctuations in the feed to the NH3-separation zone (3), the process is characterized in that so much gaseous CO2 or a gaseous mixture containing CO2 is fed to the bottom of the NH3-separation zone (3) that the composition of the liquid phase released in the bottom of the NHa-separation zone (3) is not on the side of the boundary line rich in NH3. Preferably also an amount of inert gas is introduced together with the CO2.
    公开号:SU1058503A3
    申请号:SU802901346
    申请日:1980-04-03
    公开日:1983-11-30
    发明作者:Йоханнес Петрус Мария Горден Йосефус
    申请人:Стамикарбон Б.В (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for separating pure HH and pure COj from a mixture containing NH, COg and A known method for separating HNi CO2 from a mixture of KIH g COj / and HjO by distilling most of the ammonia in the first stage at a pressure of 1-5 abs.atm . and distilling off carbon dioxide gas in the second stage, the remaining liquid is desorbed, for example, with methanol at a pressure of 1 abs.atm. This leads to a decrease in the pressure of the system and the release of ammonia and some carbon dioxide from it, so that a mixture of methane, ammonia and carbon dioxide is obtained at a total pressure of 1 abs.atm. In order to remove traces of carbon dioxide contained in the gas mixture, a part of the mixture is condensed, providing conditions under which carbon dioxide is absorbed with liquid ammonia ij "h. A method is known in which the ammonia and carbon dioxide gas mixture in which the ammonia content is higher than in azeotrope, absorbed with water or aqueous solution. At atmospheric pressure, ammonia is distilled off from the resulting aqueous solution. The remainder of the solution is then subjected to fractional distillation under ata pressure and heating to distill off acid 2J. The closest method proposed is the separation of ammonia AND carbon dioxide from mixtures containing ammonia, carbon dioxide and water, including the ammonia separation by ammonia distillation in the zone of ammonia aka with the removal of the remaining liquid phase from the ammonia separation zone to the carbon dioxide separation zone, with the release of carbon dioxide in this zone by distillation and feeding the remaining liquid phase into the desorption zone, where ammonia and dioxide Carbon is separated in the B1 gas mixture. The disadvantage of the known methods is the high energy intensity of the process. The purpose of the invention is to reduce energy costs. The goal is achieved in that, according to the method of ammonia and carbon dioxide emission from a mixture containing ammonia, carbon dioxide and water, including the separation of ammonia by distillation in the ammonia separation zone, the remaining liquid phase is removed from the ammonia separation zone to the carbon dioxide separation zone. A zone of gaseous carbon dioxide by distillation and sweeping the remaining liquid phase into the desorption zone, where ammonia and carbon dioxide are separated in the form of a gaseous mixture, gas is fed to the bottom of the ammonia separation zone. ase carbon dioxide in an amount of 1-20% by kolig1estva remaining liquid phase is discharged from the ammonia separation zone., on the bottom of the ammonia separation zone fed additionally an inert gas in an amount of 43-233% by weight of gaseous carbon dioxide. Figures 1 and 2 show embodiments of the proposed method. A mixture of ammonia, carbon dioxide and water is fed through line 1 by pump 2 to ammonia-distillation. The ammonia is discharged from the head of column 3 via line 4. This ammonia can be condensed by cooling, if necessary deep, in condenser 5. An uncondensed gaseous mixture of ammonia with an inert gas is removed from the condenser. This inert gas comes from the air introduced into the passage systems of the MG1 material from which the tank equipment and pipelines are made in order to reduce corrosion to an acceptable level. For this purpose, oxygen or an oxygen-carrying substance can be used instead of air. According to one of the embodiments of the proposed cno-i soba, the amount of injected air is substantially greater than the excess required to keep materials in a passivated state. According to the proposed method, air contributes to the improvement of the separation efficiency. Part of the air is sent to the slurry distillation column 3 via compressor 6 via pipelines 7 and 8, and another part through pipeline 9 to desorber 10. The gaseous mixture from condenser b is fed through line 11 to scrubber 12, which is released from aivOvmaKa by washing with water supplied through conduit 13. Most of the heat released during absorption is removed by cooling a portion of the resulting aqueous ammonia removed by pump 14 to the recycle fridge 15 and returned to scrubber 12 via conduit 16. The valve is returned to the ammonia distillation column 3 via conduit 17. An inert gas is withdrawn through conduit 18 and fed to the bottoms of the carbon dioxide distillation column 19 via line 20, it can be discharged completely or partially through conduit 21. Part of ammonia liquefied in condenser 5, outlet t back through line 22 to eiM. The fractional distillation column for | use as oroshak tsey
    phlegm liquids). The remainder is discharged through conduit 23. A solution of ammonia and carbon dioxide in water is withdrawn from the bottom of the ammonia distillation flask 3 via conduit 22. Gaseous carbon dioxide is sent to conduit 3 via conduit 24. The condensers 3 can be heated by means of a coil heater 25.
    The solution in conduit 22 is fed to a carbon dioxide rectifier in a psadion column 19, which operates essentially at the same CciMOM pressure as the ammonia distillation column 3. A certain amount of dilution water is sent to column 19 via line 26. The bottom product of desorber 10 is removed by a pump 27 through conduit 28 and 29. In order to achieve a better heat distribution, this water used for desorption is first released from part of the heat contained in it in the bottom part of the carbon dioxide distillation column 19. The remaining heat , required for rectification, is supplied here by means of heating coils 30, heating x, for example steam, the liquid stream entering through conduit 29 is discharged, although it is possible to use part of it as a diluent Water. Additional wash water is fed to column 19 via conduit 31 to separate ammonia from carbon dioxide as fully as possible. The gas mixture, consisting of carbon dioxide and inert gases, essentially free of ammonia (if any), leaves the head of column 19 via conduit 32. The bottom product or residual liquid phase after column 19 is a dilute aqueous ammonia solution. and carbon dioxide, is passed through conduit 33 to desorber 10. Virtually all of the ammonia and all carbon dioxide is removed in desorber 10 by heating with coil heaters 34, for example, by steam. The water obtained, practically free of ammonia and carbon dioxide, after desorption is discharged through conduit 29. The gaseous mixture of ammonia, carbon dioxide and water obtained in desorber 10 is fed to the ammonia distillation column 3 via conduit 35. a mixture of ammonia, carbon dioxide and water, having a high. ammonia content. If the composition of this initial mixture is poor With respect to ammonia, then the initial
    the stream would have been fed first to the carbon dioxide distillation column 19.
    The carbon dioxide rectification of FIG. 2) is carried out under a higher
    pressure than the rectification of s1miaka. Compressor A and pump B, respectively, are installed on pipelines 1X 20 and 22 in order to increase the pressure of the gas and liquid flows, respectively. In addition, the pipeline 35 has a reduction valve-fan B, by means of which the pressure of a part of the gaseous mixture withdrawn from desorber 10 is reduced.
    In this case, the desorption column 10 operates at virtually the same pressure in the system as is the case during the rectification of carbon dioxide. Pipeline 8
    It contains a reduction valve B, which is used to reduce the pressure of a part of the air supplied through it.
    When implementing the method based on the pressure difference (Fig. 2, the pressure at which the separation of GOj occurs is two to five times higher than the pressure at which the separation of NH-j occurs.
    the need to add a diluent to the CO separation zone, as is done using the dilution method.
    Example 1. Actually pure MNZ and actually pure CO
    are separated from a mixture containing NIL, COg and H2O in an installation whose structure is similar to that shown in FIG.
    With a pressure of 180 kPa 56489 kg / h
    of a solution of MN and CO2 in water, whose composition corresponds to%: N H 32, B / CO 18, 3 and water 48,9, is introduced into the distillation column 3, designed to separate N N, with the help of compressor 6 at a speed of 635 kg / h, of which 248 kg / h are introduced into distillation column 3, designed to separate NH-} and 387 kg / h - into desorber
    10. Through line 24, COi is introduced into distillation column 3, designed to separate KH-J, with a rate of 2000 kg / h, 27.026 kg / h of gaseous mixture containing,%: NH-j52.8; COj 14.1, - tiqp 27.7 and inert {1 gas 1.5,
    leaving desorber 10, is expanded by means of valve B and also fed to distillation column 3, intended to separate NHj, 38.180 kg / h of gaseous mixture containing,%: NH-j 98.0; H-jO 0.3
    and inert gas 1.7 is discharged from the top of column 3. A portion of this gas mixture is liquefied by cooling in a condenser 5, from which
    17.924 kg / h of liquid NHj are returned to column 3 as reflux, and 18.528 kg / h of liquid NH are removed from the system. 2.464 kg / h of a gaseous mixture containing 74.2% of 25.8% inert gas is discharged from condenser 5. This mixture is washed with water in a scrubber 12, with water being supplied at a rate of 2200 kg / h. Heat is removed from the scrubber 12 through a recirculation condenser 16. In an hour, 4029 kg of a solution consisting of 45.4% HH-j and 54-, are returned to the distillation column for the separation of HH. In the distillation column, designed to separate CO2, 635 kg / h of inert gas are passed through pipelines 18 and 20.. From the bottom of the distillation column 3, intended to separate the KH through conduit 22 and through pump B to the distillation column 19,. 69,180 kg / h of liquid, whose composition corresponds to 22.7% of 1H 3 23.4%, is passed through to separate CO2; CO2 and 53.9% H2O. Columns 19 are fed through pipelines 26 and 4 of 31 34.0.79 kg / h of water. The gaseous mixture leaving the upper part of the distillation column 19 intended for separating CO2 at a rate of 12.337 kg contains 93.2% GOi, including less 100 ppm to 90.913 kg / h of a solution containing 78.5% H2O, 17.3% NH, H 4.2% COg, are passed from the bottom of the column 19 to the desorber 10. The composition of this sludge is on the other side of the boundary line, which corresponds to a mixture rich in CO2. In the desorber, the solution is actually freed from N H and CO with steam. In total, 63.892 kg / h of liquid is removed from desorber, and this liquid can be used, for example, to adsorb NHj and CO or, partially, as diluent water in the CO2 separation zone. Example 2: Actually pure IN and practically pure CO are separated from a mixture of NH, CO and "20 in a plant having a structure similar to that shown in Figure 2, in which CO2, as well as air, is introduced into a distillation column for the separation of NH-j. The numerical designations correspond to those described in relation to FIG. 3, and the percentages correspond to the weight criteria. . At a pressure of 1800 kP, 51.972 kg / solution of CO in water, having the composition,%: hHj33.4 / COjlS a and water 48.4, is added to the distillation column 3 intended to separate the NH-). With the help of compressor b, 2.387 kg / h of air is introduced into the system, of which 2000 kg / h is fed to distillation column 3, designed to separate NN, 387 kg / h to desorber 10. Through conduit 24 to distillation column. 3, intended for the separation of BF, serves 2000 kg / h of CO2. 22.928 kg / h of gaseous mixture containing,%:, 7, CO2l6, p, H.jO 26.3 and inert hectares: from 1.5 from desorber 10 is expanded by means of valve B and also introduced into distillation column 3, designed for separation. From the top of this column, 32.415 kg / h of a gaseous mixture containing,%:, 0, 0.3, and inert gas 1.7 were removed. Part of this gaseous mixture is liquefied by cooling in condenser 5, of which 15.057 kg / h of liquid ammonia is returned to the 3 r column as reflux, and 17.358 kg / h of liquid bottom is removed from the system. From the conductor 5, 9.252 kg / h of residual non-condensed gaseous mixture, consisting of 74.2% of NH and H and 25.8% of inert gas, is released. This residual mixture is washed in the scrubber 12 through a recycle condenser 15. Within an hour, 3.829 kg of a solution containing 82.0% NH and 18% is returned to the distillation column for the separation of NH. In the distillation column 19, intended for the extraction of CO2, it is passed through a .20 pipeline and through the KONmpeccop A 635 kg / h of inert gas. From the bottom of the distillation column 3, designed to separate NHj through conduit 22 and through pump B, into the distillation column 19, intended to purify CO2, 62.042 kg / h of residual liquid phase having the composition,% NH) 22.3 CO 24.6, 53.1. . In the column 19 also serves on the pipeline 26 and through the pipeline 31 20,486 kg / h of water. From the upper part of the distillation column 19, designed to separate CO, a gaseous mixture is released at a rate of 11.4) 32 kg / h, which contains 93.2% CO and less than 100 h per million KN. 79.817 kg are passed from the bottom of the column 19 to desorber 10 / h solution, containing,%: 77.9, NHj 17.3 and caj4, S. The composition of this liquid is on that side of the boundary line, which corresponds to a mixture rich in C0j. In total, 55.889 kg / h of liquid is withdrawn from the desorber, which can be used, but not partially, as a dilution water in zone separation. In this stripper, a solution is obtained that is actually free of CO, which is provided from steam.
    In the table, yes, the relative amounts of energy that are required to separate the pure pure COjOT NHj + mixtures. The magnitude of the energy, depending on the amount of COif of the downstream separating zone,% of the residual liquid phase, is,%:
    I
    Energy
    COj The amount of CO and air, entered downstream of the separation zone NOR, was originally given as relative weight quantities. However, it was indicated that the ratio between COj and air was between 30:70 and 70:30.
    As a percentage, this means that between 100% and CO use 43 to 233% of air.
    The relative amounts of air and the corresponding amounts of energy required for separation, in the case of using 3% CO, are:
    Air Energy
    权利要求:
    Claims (2)
    [1]
    1. METHOD FOR ISOLATING AMMONIA AND CARBON DIOXIDE From a mixture containing ammonia, carbon dioxide and water, including the separation of ammonia by distillation in the ammonia separation zone with * withdrawal of the remaining liquid phase from the ammonia separation zone to the carbon dioxide separation zone with the release of gaseous dioxide in this zone 'carbon distillation and feeding the remaining liquid phase in the desorption zone, where ammonia and carbon dioxide are separated in the form of a gaseous mixture, characterized in that, in order to reduce energy consumption, I submit to the bottom of the ammonia separation zone Gaseous carbon dioxide from the carbon dioxide separation eons in an amount of 1-20% of the remaining liquid phase withdrawn 'from the ammonia separation zone.
    [2]
    2. The method according to claim 1, with the exception that inert gas is additionally supplied to the bottom of the zone ~ of ammonia separation in an amount of 43-233% by weight of gaseous carbon dioxide.
    9ui.t
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE669314C|1934-11-22|1938-12-22|I G Farbenindustrie Akt Ges|Separation of carbonic acid and ammonia|
    GB664375A|1954-07-27|1952-01-02|
    US3112177A|1959-11-11|1963-11-26|Toyo Koatsu Ind Inc|Method of separating ammonia from hydrogen cyanide|
    NL264624A|1960-05-10|
    US3225519A|1962-12-13|1965-12-28|Hydrocarbon Research Inc|Gas absorption|
    AT261638B|1966-05-02|1968-05-10|Chemie Linz Ag|Process for processing an ammonia-carbonic acid gas mixture|
    DE1592349B1|1966-05-04|1971-08-26|Lentia Gmbh|Process for the separation of an ammonia-carbon dioxide gas mixture|
    NL143063B|1967-07-06|1974-08-15|Stamicarbon|METHOD OF PREPARING FERROMAGNETIC MATERIAL.|
    DE2229213C2|1972-06-15|1982-12-02|Metallgesellschaft Ag, 6000 Frankfurt|Process for the processing of waste water resulting from the degassing or gasification of coal|
    DE2262457A1|1972-12-20|1974-06-27|Linde Ag|PROCESS AND DEVICE FOR WASHING OUT CARBON DIOXIDE, HYDROGEN SULFUR AND, IF APPLICABLE, CARBON OXISULFIDE|
    DE2317603C3|1973-04-07|1982-03-25|Basf Ag, 6700 Ludwigshafen|Process for at least partial separation of gas mixtures containing ammonia and carbon dioxide|
    US3920419A|1974-04-10|1975-11-18|Republic Steel Corp|Method of removing ammonia from ammonia containing liquor|
    GB1533462A|1975-02-05|1978-11-22|Sterling Drug Inc|Method and apparatus for ammonia removal from wastewaters|
    DE2527985C3|1975-06-24|1981-04-16|Metallgesellschaft Ag, 6000 Frankfurt|Continuous process for the production of pure ammonia|
    DE2646804C3|1976-10-16|1982-03-11|Basf Ag, 6700 Ludwigshafen|Process for the production of pure ammonia from gas mixtures containing ammonia and carbon dioxide|
    NL168196C|1976-11-03|1982-03-16|Stamicarbon|METHOD FOR SEPARATING NH & 013 AND CO & 012 FROM A MIXTURE OF NH & 013, CO & 012 AND H & 012O.|
    NL7804668A|1978-04-29|1979-10-31|Stamicarbon|METHOD FOR SEPARATING NH3 AND CO2 FROM MIXTURES OF NH3, CO2 AND WATER.|JP4975205B2|2000-04-28|2012-07-11|日揮株式会社|Method for recovering ammonia from gaseous mixtures|
    US6706093B2|2000-05-23|2004-03-16|Rohm And Haas Company|Method and apparatus for preventing iron contamination in corrosive service|
    CN100475970C|2002-12-27|2009-04-08|味之素株式会社|Process for producing amino acid or salt thereof by column technique and production apparatus thereof|
    US8500868B2|2009-05-01|2013-08-06|Massachusetts Institute Of Technology|Systems and methods for the separation of carbon dioxide and water|
    CN102538394B|2011-12-27|2014-08-06|尤彪|Method for separating ammonia and carbon dioxide by low-temperature rectification|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US06/030,374|US4256471A|1979-04-16|1979-04-16|Process for the separation of ammonia and carbon dioxide from mixtures containing ammonia, carbon dioxide and water|
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