• 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:
    An improved process for the separate recovery of substantially pure ammonia and substantially pure carbon dioxide from mixtures containing ammonia and carbon dioxide, and possibly water, such as are obtained as by-products in the manufacture of melamine from urea or the synthesis of urea from ammonia and carbon dioxide. The by-product mixture is introduced into a process loop having an ammonia separation zone, a carbon dioxide separation zone and a desorption zone, the zone to which the mixture is initially fed being dependent upon its composition. An ammonia off-gas, substantially free of carbon dioxide and water, is obtained from the ammonia separation zone, and the residual liquid phase is introduced into the carbon dioxide separation zone. Diluting water is also added to the carbon dioxide separation zone in an amount of from about 0.2 to 6 times, by weight, the combined total weight of the residual liquid phase from the ammonia separation zone and the by-product mixture, if any, fed into the carbon dioxide separation zone. A carbon dioxide off-gas, substantially free of ammonia and water, is obtained from the carbon dioxide separation zone and the residual liquid phase therefrom is introduced into the desorption zone wherein substantially all of the ammonia and carbon dioxide are desorbed and separated from the liquid phase and introduced into the ammonia separation zone.
    公开号:SU869551A3
    申请号:SU772540049
    申请日:1977-11-03
    公开日:1981-09-30
    发明作者:Йоханнес Бирманс Андреас
    申请人:Стамикарбон Б.В. (Инопредприятие)；
    IPC主号:
    专利说明:

    (54) METHOD FOR ISOLATION OF AMMONIA AND CARBON ACID FROM THEIR MIXTURE The invention relates to a method for separating substantially pure N3 and CO ,. The term mixture containing NHs and COj means a mixture that can be a binary mixture of NHs / CO, a gaseous mixture of NHS, CO2 and water vapor, or an aqueous solution of NHs and COj, which can also be contained in a solution of ammonium carbamate and Ammonium carbonate. It is known to release ammonia n carbon dioxide from mixtures of ammonia, carbon dioxide and water by ottonki most of the ammonia in the first stage, then distilling carbon dioxide in the second stage with an increased pressure of a mixture of ammonia, carbon dioxide and water 11. According to this method, in the first stage, press the mixture of 1- 5 ata; carbon dioxide is separated from a mixture of ammonia, carbon dioxide and water, in which the coideitrain ammonia is very small, i.e. less than in the azeotrope of ammonia / coal spray. The resulting residues are flushed with a gas, for example, metaiom prn total pressure of 1 at. This leads to a decrease in the pressure of the mixture and the release of ammonia and some carbon dioxide; get a mixture of methane, ammonia and coal; yuty at a total pressure of 1 at. For owciKH gas mixture from traces of carbon dioxide, part of this mixture is condensed, which leads to the absorption of carbon dioxide by ammonia. The closest in technical cyvatocm and the achieved result is the way in which the gas mixture of ammonia and carbon dioxide, in which the ammonia content is higher than in the azeotrope, is absorbed by water or aqueous solution. Under atmospheric pressure, the pressure is removed from the resulting aqueous solution. Then the rest of the solution is distilled by distillation at a pressure of from 5 to 20 atm and distilled to remove carbon dioxide 2. The known methods are based on the principle of changing the pressure of a mixture of ammonia, acid, and carbon dioxide. at higher. Between pressure, mixing, i.e. the sum of the ammonia, flow acids and water fractional pressures in the ammonia removal stage and the pressure of the mixture in the carbon dioxide removal stage should be from 1: 5 to 1:20 in the mix process if the separation goes smoothly. However, these methods have the disadvantage that if the mixture being processed is obtained at a pressure of more than 1 atm, then its pressure must first be reduced to 1 at. Moreover, gaseous ammonia is released at a maximum pressure of 1 atm, with the possible presence of a large amount of another gas. If ammonia is further processed, for example, in the synthesis of urea, its pressure must be increased again. This requires a significant energy consumption for compression, in addition, the concentration of carbon dioxide in ammonia must be low to prevent the formation of solid ammonium carbamate in the compressor, and high pressure lines. It is also possible to squeeze gaseous ammonia in a deep cold, with a subsequent increase in the pressure of ammonia to the desired value. But it also requires energy. The purpose of the invention is energy consumption and simplification of the method. The goal is achieved by the fact that in the method of release of ammonia and carbon dioxide from their mixture by fractional disintegration, when heated in the zone of release of ammonia and in the zone of release of carbon dioxide, the release of carbon dioxide is carried out in the presence of 0.2-6 times the amount of water added mixtures in carbon dioxide release. According to the invention, a method is proposed for separating practically pure ammonia and practically pure carbon dioxide from mixtures of ammonia and carbon dioxide, and this separation is carried out in the zone of ammonia released by heating and in the zone of carbon dioxide by heating; This method is different in that the release of carbon dioxide is carried out in the presence of water in an amount of from 0.2 to 6 times the weight of the feed mixture to the release of carbon dioxide, the optimum value is 0.5 to 45 times the amount below the split limit. it becomes more laborious, it requires an increase in circulation quantities and the separation is extremely small. With more than 2.5-fold amounts, the temperature of the emitted carbon dioxide increases, which leads to increased corrosion, and with 6-fold amounts of energy required for years the added water becomes unacceptably large. It should be noted that the amount of water added to the zone of carbon dioxide lithium is in excess of that contained in the initial mixture supplied to the zone of carbon dioxide lane, since it may contain ammonia, carbon dioxide and water in this mixture. The proposed method is applied for ISOKD1 & X-1 mixtures enriched in ammonia or 8 14 carbon dioxide. The term ammonia-rich mixture means that the ammonia / methyl acid ratio in the initial mixture is such that ammonia is released predominantly when heated, and the term carbon-rich mixture means that the ammonia / carbonic acid ratio in the initial mixture is such that when it heats up, carbon dioxide is preferentially released . One of the embodiments of the present invention proposes a method in which the initial mixture is an ammonia-rich mixture, it consists in: passing the said mixture to an ammonia release zone, where gaseous ammonia is obtained in the form of an upper peony, and as a residue is obtained a constantly boiling ammonia and carbon dioxide solution; passing the residue in the form of an initial mixture to a carbon dioxide ejection zone in the presence of water, where carbon dioxide is obtained as an overhead stream, and a constantly boiling solution of ammonia and carbon dioxide is obtained as a residue. According to another embodiment of the invention, a method is proposed in which the mixture is a mixture enriched with carbon dioxide, it consists in: supplying said mixture to a zone of carbon dioxide liberation in the presence of water, where carbon dioxide is released as overhead, and in view of the remainder Schy water solution of ammonia and carbon dioxide; feeding the residue to a desorption zone, where almost all of the ammonia and carbon dioxide is removed, as a gas mixture with water vapor; and supplying this gas mixture to an ammonia excretion zone, where ammonia gas is obtained as an overhead stream, and as a residue, a constantly boiling aqueous solution of ammonia and carbon dioxide is obtained. Water can be supplied to the carbon dioxide release zone at one or several points of this zone and / or it can be supplied partially in front of this zone to the mixture loaded into this zone. The added water may be a dilute solution of ammonia and carbon dioxide, for example, containing at least 90% by weight of water. However, this content depends on the pressure in the system, at lower pressures a greater amount of water is required. Preferably, in the ammonia excretion zone, the temperature of the bottom is 60-170 ° C and the top temperature is from -35 to + 66 ° C, and in the excretion zone of carbon dioxide, the temperature of the bottom is 75-200 ° C and the top temperature is O-100 ° C, and the temperature {} and the top of these zones should always be lower than the bottom temperature. 5 The optimum temperature for the bottom of the ammonia release zone depends on the composition of the mixture and the pressure. However, if texting is used below 60 ° C or the formation temperature of the solid reaction products of ammonia, carbon dioxide and possibly water, or the raw materials entering the carbon dioxide release zone have such a composition, then the optimum separation is not achieved. In most cases, the temperature of the lower ammonia release zone is not higher than 170 ° C, this is done with the aim that it and the temperature in the ammonia release zone (which is always slightly higher) is lower than the temperature at which undesirable corrosion occurs. For the same reason, the temperature of the bottom of the carbon dioxide release zone should not exceed. The temperature of the top of the ammonia release zone is determined mainly by the applied pressure. The temperature of the upper carbon dioxide release zone is determined by the final frequency of the carbon dioxide produced. As a rule, the ammonia content in 100 ppm is easily achieved at top temperatures of up to 100 ° C. The top temperatures of both excretion zones are determined by the amount of ammonia reflux and the amount and temperature of the diluent and wash water, respectively. It is better to keep the pressure in the carbon dioxide release zone no higher than twice the pressure in the ammonia release zone, even better if the pressures in both emission zones are almost equal. A ratio of pressures greater than 2 may be used, but this will lead to a pressure at which the release of ammonia will be less, therefore large investments will be required to reduce ammonia. It also leads to very high energy consumption. For this reason, it is preferred to operate at the indicated maximum pressure ratios. The proposed method can be carried out at equal pressure in the emission zones of ammonia and carbon dioxide. It is more profitable to use a pressure ratio characterized by a small ratio, for example, it saves heat when ammonia and carbon dioxide are released, and also reduces the required surface of the transfer. PRI me R. In the equipment shown in the drawing, almost pure ammonia is separated into almost pure carbon dioxide from a mixture of ammonia, carbon dioxide and water. At a pressure of 18 at a temperature of 73 ° C, an aqueous solution of ammonia n carbon dioxide, containing 33.4% ammonia, 18.2% carbon dioxide and 48.4% water, is fed to the lower part of the ammonia distillation column 1 at a speed of 51.972 kg / h. Compressor 2 serves 635 kg / h of air, of which 248 kg / h are fed to the ammonia rectifying column and 387 K1 / H to desorber 3.. A gas mixture of 50.4% ammonia, 17.7% yine acid and 30.9% water and up to G, 0% other gases with a temperature of 162 ° C, which was removed from the stripper, is also sent to the ammonia fractionation column at a speed of 39.304 kg / h A gas mixture of 99.2% ammonia and 0.6% other gases at a rate of 65.217 kg / h is removed from the top of the column. With the aid of cooling water, a part of this gas mixture is liquefied in the refrigerator 4. 44.630 kg / h of reflux is sent to the ammonia column in the form of a cooled mixture. 3.474 kg / h of a gas mixture containing 88.9% of ammonia and 11.1% of other gases leaves the refrigerator. It is washed in a washer with 114.496 kg / h of water. Heat from the blender 5 is removed in a circulation cooler 6. A solution containing 38.7% ammonia and 61.3% water is returned to the ammonia reagent column in an amount of 7.335 kg / h. The temperature at the top of this column is 46 ° C. Along lines 7 and 8, other gases are directed to a carbon dioxide distillation column 9 in an amount of 635 kg / h. From the lower part of the ammonia distillation column, 25.4% ammonia, 21.6 carbon dioxide and 53.6% water at 131 ° C, along line 10, were removed to the carbon dioxide distillation column 9 in the amount of 78.027 kg / h. In this column, the pressure of which is also i8 ata, diluents are also fed through the line 2573299 kg / h in the form of water containing traces of ammonia and carbon dioxide, which at the exit from the stripper has a temperature of 20 ° C. This liquid releases part of the heat in the bottom part of the carbon dioxide rectification column, the rest of the heat is removed in the refrigerator I. The liquid leaving the desorber in the amount of 108909 kg / h, containing 35610 kg / h, is removed as much as possible when cooled in the cooler 12 . This water can be used for the absorption of ammonia and carbon dioxide. 5.959 kg / h of rinsed water and the final traces of ammonia are fed up to the cisc distillation cone. With the encouragement of steam, the temperature of the bottom carbon dioxide distillation column is maintained at 58 ° C. The top temperature of this column is 5 ° C. From this column, 10.094 kg / h of a gas mixture containing 93.7% carbon dioxide n, 3% of other gases are taken, besides it contains less than 100 ppm ammonia. A solution containing 81.9% of ode, 13.4% of ammonia and 4.7% of water at a temperature of 158 ° C is taken from the bottom of the OLO1SHY and sent to the stripper at a rate of 147.826 kg / h.
    权利要求:
    Claims (1)
    [1]
    Claim
    The method of separation of ammonia and carbon dioxide from their mixture by fractional distillation
    869551 8 when heated in the zone of ammonia and in the zone of carbon dioxide, characterized in that, in order to reduce energy consumption and simplify the method, the recovery of utle5 acid is carried out in the presence of 0.2-6 times the amount of added water to the weight of the initial mixture in the zone of selection carbon dioxide.
    类似技术:
    公开号 | 公开日 | 专利标题
    US4308385A|1981-12-29|Process for purifying urea-containing waste water and process for preparing melamine
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    SU833158A3|1981-05-23|Method of urea and ammonia synthesis
    US3155722A|1964-11-03|Recovery of residual ammonia and carbon dioxide in the synthesis of urea
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    US2046827A|1936-07-07|Production of urea and nitrogen oxides
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    US3470247A|1969-09-30|Process for the production of urea by synthesis of ammonia and carbon dioxide,with total recycling of the portion which has not been converted into urea
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    US3232983A|1966-02-01|Urea synthesis
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    US2864772A|1958-12-16|Gas processing
    US4053508A|1977-10-11|Process and installation for preparing urea from ammonia and carbon dioxide
    US3305582A|1967-02-21|Urea synthesis with recovery of excess ammonia
    US3232982A|1966-02-01|Urea synthesis
    同族专利:
    公开号 | 公开日
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    DE2748639A1|1978-05-11|
    CA1100286A|1981-05-05|
    BE860418A|1978-05-03|
    IE45824L|1978-05-03|
    NO151116C|1985-02-13|
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    FR2370247B1|1982-11-05|
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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|
    DE1067014B|1957-05-18|
    US2992703A|1958-06-05|1961-07-18|Vasan Srini|Separation of carbon dioxide from ammonia|
    US3112177A|1959-11-11|1963-11-26|Toyo Koatsu Ind Inc|Method of separating ammonia from hydrogen cyanide|
    NL264624A|1960-05-10|
    US3315442A|1964-10-05|1967-04-25|American Cyanamid Co|Quenching of crude melamine gases|
    FR1457776A|1964-10-16|1966-01-24|Allied Chem|Process for reducing corrosion in a gas scrubber during the separation of carbon dioxide and ammonia from their mixtures with water vapor|
    US3336761A|1964-12-03|1967-08-22|Universal Oil Prod Co|Plural expansion-compression refrigeration cycle with a fractionating column|
    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.|
    DE1670290A1|1967-12-01|1971-01-14|Basf Ag|Process for the separation of ammonia from the waste gases resulting from melamine synthesis|
    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|
    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|
    DE2527985C3|1975-06-24|1981-04-16|Metallgesellschaft Ag, 6000 Frankfurt|Continuous process for the production of pure ammonia|NL7804668A|1978-04-29|1979-10-31|Stamicarbon|METHOD FOR SEPARATING NH3 AND CO2 FROM MIXTURES OF NH3, CO2 AND WATER.|
    US4256471A|1979-04-16|1981-03-17|Stamicarbon, B.V.|Process for the separation of ammonia and carbon dioxide from mixtures containing ammonia, carbon dioxide and water|
    NL7903623A|1979-05-09|1980-11-11|Stamicarbon|METHOD FOR PURIFYING UREAUS WASTE WATER AND METHOD FOR PREPARING MELAMINE.|
    NL8200905A|1982-03-05|1983-10-03|Stamicarbon|METHOD FOR SEPARATING AMMONIA AND CARBON DIOXIDE FROM AMMONIA, CARBON DIOXIDE AND WATER MIXTURES|
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    CN105289210B|2015-10-28|2018-02-13|北京烨晶科技有限公司|A kind of ammonia carbon separating technology|
    CN110433517A|2019-08-23|2019-11-12|安徽广信农化股份有限公司|A kind of cyclohexyl isocyanate rectifying column|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    NLAANVRAGE7612163,A|NL168196C|1976-11-03|1976-11-03|METHOD FOR SEPARATING NH & 013 AND CO & 012 FROM A MIXTURE OF NH & 013, CO & 012 AND H & 012O.|
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