• 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 process is directed to recovering epsilon -caprolactam from a reaction mixture containing epsilon -caprolactum and sulfuric acid by separating the caprolactam from the sulfuric acid by an extraction. Extraction includes the steps of neutralizing a part of said sulfuric acid with ammonia, ammonium sulfate, ammonium hydrogen sulfate or mixture thereof, to form an ammonium salt of at least part of said sulfuric acid as a neutralization product, thermally decomposing a part of the ammonium salt formed to produce a gaseous mixture of ammonia and sulfur dioxide and contacting another portion of the neutralization product with said gaseous mixture to produce ammonium hydrogen sulfate, ammonium sulfate or both, and neutralizing at least a part of the sulfuric acid in the reaction mixture with said ammonium hydrogen sulfate, ammonium sulfate or both.
    公开号:SU710517A3
    申请号:SU772499152
    申请日:1977-06-22
    公开日:1980-01-15
    发明作者:Гуттс Рейер；Ламбертус Зварт Рудольф
    申请人:Стамикарбон Б.В., (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to a process for the isolation of y-caprolactam from a reactive sulfuric acid mixture, which is widely used in polyamide formulations. A method is known for isolating fe-caprolactam-from a sulfuric acid mixture by coupling sulfuric acid to an ammonium salt of a myaxial mixture consisting of ammonia and sulfur dioxide obtained by decomposing the whole ammonium salt, followed by extraction of the 6-caprolactam with an organic solvent and decomposition of the resulting salt ammonium 1. The disadvantage of this method is the complexity of the technological process, consisting in the need to decompose all the ammonium salt obtained. The aim of the invention is to simplify the process. The goal is achieved that those who decompose 45-50% from ammonium and the resulting ammonia and dvoy sulfur to return to neutralization is mixed with the remaining amount of ammonium salt. The drawing shows an installation diagram for carrying out the proposed method. In the diagram, reference numeral 1 denotes a reactor for converting cyclohexanone oxime into & -caprolactam, 2-neutralizer for partial neutralization of a mixture of lactam and sulfuric acid, 3 - a device for extracting lactam from a mixture of lactam and ammonium bisulfate formed in this neutralizer, 4 neutralizer for full or partial neutralization of ammonium bisulfate, 5 - a device for reducing the decomposition of ammonium bisulfate and 6 is a plant for sulfuric acid (oleum). The cyclohexanonexium pg pipe 7 enters the rearrangement reactor 1, for example, a reactor equipped with a stirrer, or a tank with cyclone mixing, into which the sulfuric acid or oleum contained in the installation 6 is also fed through pipeline 8 to the neutralizer 2 to which is supplied by ammonium sulphate solution through the conduit 10 from the neutralizer 4, ammonia through the conduit 11 and ammonia through the conduit 12. It is possible to completely or partially replace ammonia and water with gtkshachny water. The mixture, neutralized into ammonium bisulfate, is rearranged through conduit 13 to extractor 3, into which solvent for caprolactam passes in conduit 14, which is poorly dissolved; ; ammonium sulfate and ammonium bisulfate. This solvent includes, for example, benpol, toluene, 1-2-dichloroethane, chloroform, 1,1,2-tetrachloroethane, ethyl ether or dibutylcarbinol. Caprolactam, dissolved in the extracting agent, exits the system through conduit 15. and enters a plant (not shown) to obtain lactam. The resulting ammonium bisulfate aqueous solution is discharged through conduit 16. A portion of the ammonium bisulfate solution discharged through conduit 16 is transferred to decomposition apparatus 5 via conduit 17 and decomposed into a gas mixture containing mainly ammonia, sulfur dioxide and water vapor under reducing conditions. . The pipeline .18 This gas mixture is sent to the neutralizer 4, to which the remaining portion of the aqueous solution of ammonium bisulfate leaving the extracting device 3 through the pipeline 16 is fed through the pipeline 19. With the help of ammonia present in the gas from the pipe 18, bisulfate
    The ammonium in the neutralizer 4 is converted to ammonium sulfate. The gas mixture, containing mainly sulfur dioxide, leaves the neutralizer 4 and is sent to the unit for sulfuric acid oleum b through pipeline 20,
    the water content can be maintained at the required level by evaporation of the solution passing into the decomposition device 5 through the pipeline
    17
    From neutralizer 4 received.
    ammonium mono / bisulfate ammonium sulphate solution after purification can be transferred to neutralizer 2 through a 1p pipeline.
    Example. In accordance with the above scheme, about 100 tons of {, -caprolactam are produced daily. Neutralization of a mixture of lactam and sulfuric
    acids are produced at atmospheric
    pressure and temperature 40s. The resulting nd caprolactam is extracted with chloroform. Ammonium bisulfate, obtained by neutralization, is thermally decomposed with the help of a neutral gas according to the following equation
    КН Н50 СН М | 202- МНз4502 ЭН ,,
    The composition of the various streams of materials, expressed in k mol / h, is given in the table,
    lio to this example. nitrogen from a solution of ammonium sulfate / ammonium bisulfate in an amount up to 70% in the form of ammonia, and sulfur in the form of sulfur dioxide up to 100%,
    37.6
    I
    56
    Tb
    in terms of
    56 56
    The decomposition of 45-50% of the ammonium salt to ammonia and sulfur dioxide and mixing the resulting gas mixture to return to neutralization with the remaining amount of ammonium salt allows us to simplify the process for the recovery of α-caprolactam by reducing the complexity of the decomposition stage of the ammonium salt.
    权利要求:
    Claims (1)
    [1]
    1. USSR patent in application 2444805/04 with priority from
    5 03.02.76 (prototype).
    类似技术:
    公开号 | 公开日 | 专利标题
    SU710517A3|1980-01-15|Method of isolating epsilon-caprolactam
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    US3761575A|1973-09-25|Process for the cracking of ammonium sulfate
    SU712023A3|1980-01-25|Method of isolating epsilon-caprolactam
    SU656513A3|1979-04-05|Method of isolating e-caprone lactam
    US4054562A|1977-10-18|Process for the manufacture of lactams
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    US4072678A|1978-02-07|Process for producing caprolactam
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    US4029744A|1977-06-14|Process for removing the salt of a weak acid and a weak base from solution
    US4133810A|1979-01-09|Process for the recovery of ε-caprolactam from a reaction mixture of ε-caprolactam and sulfuric acid
    CS249529B2|1987-03-12|Method of urea production
    US3364202A|1968-01-16|Process for the recovery of free sulfuric acid from ammonium bisulfate
    US3859278A|1975-01-07|Process for separating lactams
    CN105143175A|2015-12-09|Steam stripping inorganic process liquid discharged from hpo extraction section and utilizing heat of condensation
    US4021422A|1977-05-03|Process for the recovery of ε-caprolactam from reaction mixture of ε-caprolactam and sulphuric acid
    US3525585A|1970-08-25|Process of preparing water-soluble phosphates
    KR100732799B1|2007-06-27|Process for treating a mixture comprising an ammonium sulfate solution phase and an aqueous lactam phase
    KR810000781B1|1981-07-06|Process for the recovery of -caprolactam from a reaction mixture of -caprolactam and sulphuric acid
    SU504761A1|1976-02-28|The method of obtaining urea and ammonium salts
    GB1595884A|1981-08-19|Process for the recovery of ammonia and sulphur dioxide from a contaminated ammonium salt of sulphuric acid
    PL81745B1|1975-08-30|Separation of lactams from a medium coating concentrated sulphuric trioxide in combination with the preparation of phosphate fertilizers[us3820972a]
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    同族专利:
    公开号 | 公开日
    IT1079706B|1985-05-13|
    AR216766A1|1980-01-31|
    BR7704190A|1978-03-21|
    US4140685A|1979-02-20|
    GB1522584A|1978-08-23|
    CH629784A5|1982-05-14|
    FR2356640A1|1978-01-27|
    DE2728606A1|1977-12-29|
    JPS532490A|1978-01-11|
    ES460035A1|1978-05-01|
    JPS6047254B2|1985-10-21|
    BE856019A|1977-12-23|
    MX4280E|1982-03-11|
    FR2356640B1|1982-07-16|
    CA1085836A|1980-09-16|
    NL7607047A|1977-12-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    NL132894C|1961-08-30|1900-01-01|
    NL164028C|1971-05-07|1980-11-17|Stamicarbon|METHOD FOR SEPARATING LACTAMS|
    CA989830A|1971-05-07|1976-05-25|Abraham H. De Rooij|Process for preparing and recovering lactams|
    DE2130037B2|1971-06-18|1977-02-10|Davy Powergas GmbH, 5000Köln|METHOD FOR PRODUCING LACTAMEN|
    DE2130036B2|1971-06-18|1977-02-10|Davy Powergas GmbH, 5000 Köln|METHOD FOR PRODUCING LACTAMEN|
    US3859278A|1972-12-11|1975-01-07|Stamicarbon|Process for separating lactams|
    BE792559A|1971-12-11|1973-06-12|Stamicarbon|PROCESS FOR THE SEPARATION OF LACTAMES|NL7700882A|1977-01-28|1978-08-01|Stamicarbon|PROCEDURE FOR GENERATING EPSILON CAPROLAC TAM FROM AN EPSILON CAPROLACTAM SULFUR ACID REACTION MIXTURE.|
    US5900482A|1995-07-20|1999-05-04|Mitsubishi Chemical Corporation|Process for the preparation of ε-caprolactam|
    US7022844B2|2002-09-21|2006-04-04|Honeywell International Inc.|Amide-based compounds, production, recovery, purification and uses thereof|
    US10967464B2|2017-03-31|2021-04-06|Senju Metal Industry Co., Ltd.|Solder alloy, solder paste, and solder joint|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    NL7607047A|NL7607047A|1976-06-28|1976-06-28|PROCEDURE FOR GENERATING EPSILON CAPROLACTAM FROM AN EPSILON CAPROLACTAM-SULFURIC ACID REACTION MIXTURE.|
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