• 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 invention relates to a process for the extraction of paraffins from mixtures obtained by the sulphoxidation of paraffins having a number of carbon atoms comprised within the range of from 12 to 18, which is characterized in that as the solvent CO2 under supercritical conditions is used.
    公开号:SU1586511A3
    申请号:SU874202320
    申请日:1987-03-26
    公开日:1990-08-15
    发明作者:Фаджиан Лучио；Маркотуллио Армандо；Платоне Эдоардо；Пиччи Эмилио
    申请人:Эниричерке С.П.А. (Фирма)；Эникем Аугуста С.П.А. (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for the extraction of paraffins from their mixtures with alkanesulfonic acids (BAC).
    The purpose of the invention is to simplify the process.
    The proposed method involves the extraction of raw material containing alkanesulfonic acids with a carbon number of 12-18, hexane-1, sulfuric acid, C-C JJ-paraffins and water, carbon dioxide under supercritical conditions, after which the extracted phase is separated, at that it contains, in addition to CO, paraffins and alcohol, and a purified phase containing alkanesulfonic acids, sulfuric acid, and water. Sulfuric acid is then neutralized or removed by known methods, whereby alkanesulfonic acids are separated.
    The conditions for performing the Extraction-1C1I step are the following: temperature in the range of 32-60 ° C, operating pressure from 85 to 350 bar, ratio (9.2-.-49): 1 .. -. .
    The proposed method can be carried out either as a continuous or as a batch process.
    The drawing shows schematically the laboratory equipment used in the process.
    The laboratory unit includes a refrigeration cycle of carbon dioxide condensation in a heat exchanger. Liquid
    cl
    00
    sd

    s
    CO2 1 is supplied by the membrane pump 2 to the heater 3 and then to the extractor i 4. The temperature in the heater and the ext-Grektor are kept constant and one I, using a water thermostat. The pressure in the extractor is kept constant by means of the regulator 5 and the operating valve 6.
    Carbon dioxide, the contents of the product: you, which are extracted from the raw material in the extractor 4, and flowing out of the valve 6, constitute the supercritical region in the separation unit 7, where the CO evaporates and the condensate
    I et in heat exchanger 8 so that
    i
    i returns to the cycle again, whereas
    I extracted phase remains inside the separation unit. The loss of carbon dioxide gas is compensated for through 9. I Separation unit 7 is equipped with i diametrically opposed I glass windows for visual level I observation. This level: keep constant by adjusting the temperature of the water coming from the second thermostat. The pressure in separation unit 7 is kept constant by means of a pressure regulator, which controls the cooling cycle. i Inside the extractor 4. there is a cylindrical vessel with end walls of porous mesh steel into which the extractable raw product can be loaded. In accordance with the preferred embodiment, the extractor is filled with stainless steel blocks. In a continuous cycle of operation, a second pump 10 is used to supply the raw product to the extractor, in which case the purified product is discharged through valve 11.
    Example 1. 126.1 g of a crude mixture of .j-paraffinsulfonic acids (secondary alkanesulfonic acids), which, in addition to sulfo and disulfonic acids, also contain May.%: 1-hexanol 17.06; C, j-Cig-α-n-paraffins 36.72; 11.22; 0.78, loaded into the vessel of the extractor 4 and extraction with supercritical CMM with carbon dioxide at 40 ° C and a pressure of 150 bar for 1 h (COj / crude BAC 14.5).
    At the end of the experiment, the products contained in the separation unit 7 (the extracted phase) and in the extractor 4 (the purified phase), respectively, discharge the valves 12 and 11 and analyze. Mass extracted
    0 Q
    5 Q
    five
    five
    paraffin relative to the initial one in raw BAC was 99.4%, K; 1-hexanol 91.9%.
    PRI mme R 2. Extraction is subjected to 125 g of the raw BAC mixture of Example 1, the extraction being carried out with supercritical CO 2 at 5 (f C and a pressure of 150 bar for 3 hours (CO2 ratio) / raw BAC 43.8) At the end of the experiment, the extracted phase and the purified phase were analyzed. It was established that the paraffin content was 99.53% by weight of the initial one in BAC, 1-hexanol, 98.8% by weight.
    Example 3. The extraction is subjected to 119.3 g of a crude mixture of paraffin sulfonic acids having the composition of Example 1. The process is carried out with supercritical carbon dioxide at pressures of 150 bar for 2 hours (CO2 ratio / raw YOU is 30.5). Analysis of the extracted and purified phases at the end of the experiment showed that the paraffin yield reached 99.87% of the 99.15% by weight contained in the original YOU, 1-hexanol.
    PRI me R 4. 120 g of a crude paraffinsulfonic acid mixture in Example 1 is subjected to extraction with CO at a pressure of 350 bar for 1 hour. The mass ratio of CO to BAC is 9.2, Analysis of the extract and the purified product at the end of the test showed that paraffins were extracted in the amount of 99.7% of the crude YOU, initially injected, and 1-hexanol was extracted in the amount of 99.0%.
    Example5. 102, 2g of the raw BAC mixture of example 1 is subjected to extrac- tal supercritical carbon dioxide at a pressure of 85 bar for 1.25 h (the ratio of CO to the raw mixture of BAC is 20.1: 1).
    Analysis of the extract and the purified fraction at the end of the test showed that paraffin extraction amounted to 99.51% of the paraffin contained in the initially loaded raw BAC mixture, and extraction of 1-hexanol was 95.9%.
    Example 6. The extractor is filled with a ceramic packed material instead of a steel packed material. 110.9 g of the raw BAC mixture of Example 1 is subjected to extraction with supercritical carbon dioxide at 33+ and a pressure of 270 bar. Extraction
    158
    carried out for 30 minutes at a volumetric flow rate of CO of 330 g / h and a ratio of CO to the raw mixture BAC 1, A9.
    Analyzes of the extract and the purified fraction carried out at the end of the test showed that extraction amounted to 99.12% of the paraffin initially contained in the loaded YOU raw mixture, and extraction of 1-hexanol reached 98.78%.
    Thus, the proposed method is simpler known, since it eliminates the long heating stage during extraction and high energy costs.
    sixteen
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method of extraction of paraffins from. their mixtures with alkane sulfonic acids, obtained by sulfonating С j-С - paraffins and containing an aqueous mixture of paraffins, alkanesulfonic acids and sulfuric acid, in the presence of alcohol, characterized in that, to simplify the process, hexanol-T and extraction are used as alcohol carbon dioxide is carried out at a mass ratio of carbon dioxide - alkanesulfonic acid 9.2-49: 1, temperature 32-60 ° C and pressure 85-350 bar.
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    同族专利:
    公开号 | 公开日
    ZA872037B|1987-09-14|
    IN169362B|1991-10-05|
    PT84576B|1989-11-30|
    NO165919B|1991-01-21|
    ES2019368B3|1991-06-16|
    JP2540038B2|1996-10-02|
    EP0239177A1|1987-09-30|
    DD255732A5|1988-04-13|
    MX172944B|1994-01-25|
    CA1274854A|1990-10-02|
    NO871157L|1987-09-28|
    BR8701987A|1988-01-12|
    PT84576A|1987-04-01|
    GR3001176T3|1992-06-30|
    DK154787D0|1987-03-26|
    AT57686T|1990-11-15|
    DE3765667D1|1990-11-29|
    CN87103209A|1987-11-04|
    DK167115B1|1993-08-30|
    US4798915A|1989-01-17|
    NO165919C|1991-05-02|
    CN1010008B|1990-10-17|
    CS268176B2|1990-03-14|
    IT1191720B|1988-03-23|
    CS214787A2|1989-05-12|
    DK154787A|1987-09-28|
    EP0239177B1|1990-10-24|
    NO871157D0|1987-03-20|
    JPS62240630A|1987-10-21|
    IT8619893D0|1986-03-27|
    AR244781A1|1993-11-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2228598A|1938-06-30|1941-01-14|Charles L Horn|Purification of hydrocarbon-sulphur dioxide-chlorine reaction products|
    US2875257A|1954-06-15|1959-02-24|Atlantic Refining Co|Preparation of improved alkylate products using a sulfuric acid treatment|
    US3033898A|1958-08-18|1962-05-08|Bray Oil Co|Sulfonation of oils|
    US3681442A|1968-12-26|1972-08-01|Universal Oil Prod Co|Alkylaromatic sulfonate detergent process of preparation|
    IT1074825B|1977-01-11|1985-04-20|Euteco Spa|PROCESS FOR THE PURIFICATION OF ALCHYLSULPHONIC ACIDS|
    US4361520A|1979-07-26|1982-11-30|Marathon Oil Company|Refinement of sulfonated hydrocarbons|
    US4269789A|1979-12-31|1981-05-26|Phillips Petroleum Company|Petroleum sulfonation|IT1196982B|1986-07-23|1988-11-25|Eniricerche Spa|PROCEDURE FOR EXTRACTION OF PARAFFINS FROM MIXTURES CONTAINING THE SAME AND ALCAN-SULPHONE ACIDS|
    IT1196981B|1986-07-23|1988-11-25|Eniricerche Spa|PROCEDURE FOR REMOVING PARAFFINS FROM MIXTURES OF THE SAME WITH PARAFFINSOLPHONIC ACIDS|
    IT1213456B|1986-07-23|1989-12-20|Eniricerche Spa|PROCEDURE FOR THE EXTRACTION OF PARAFFINS FROM THEIR MIXTURES WITH PARAFFINSOLPHONIC ACIDS.|
    IT1230155B|1989-06-15|1991-10-14|Enichem Augusta Spa|IMPROVED PROCEDURE FOR THE PREPARATION OF PARAFFIN-SULPHONIC ACIDS|
    FI105080B|1995-10-11|2000-06-15|Rauma Ecoplanning Oy|extraction|
    DE102008032723A1|2008-07-11|2010-01-14|Clariant International Limited|Process for the isolation of paraffin sulphonic acids|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT19893/86A|IT1191720B|1986-03-27|1986-03-27|PROCEDURE FOR THE EXTRACTION OF PARAFFINS FROM MIXTURES OF THE SAME WITH ALCANSOLPHONIC ACIDS|
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