• 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 the production of aliphatic alcohols, in particular C-C alcohols, used in organic synthesis. The process is carried out by the reaction of the corresponding olefin with BQ-doy on a strongly acidic cation exchanger (QD) under heating and pressure. Then the mass is separated into aqueous and organic phases. The aqueous phase contains f 12% isopropanol and 0.1% diisopropyl ether (IPE). The organic phase contains, in wt%: propane and propane. 60; IPE 19.7; O hexanes, 2; From these phases, the target alcohol is distilled, and the IPE is recycled to the reactor separately from the reactants, i.e. at a location located at a distance of 6.6-29.3% of the boundary of the end of the reaction zone in terms of its total length. These conditions ensure the continuity of the process and its better performance for alcohols, i.e., an increase from 2 to 2.8-2.85 mol / l CT-h. 2 Il. i O)
    公开号:SU1417792A3
    申请号:SU853891175
    申请日:1985-05-16
    公开日:1988-08-15
    发明作者:Нейер Вильгельм；Веберс Вернер；Деттмер Михаэль；Остербург Гюнтер
    申请人:Дейче Тексако Аг (Фирма)；
    IPC主号:
    专利说明:


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     cm
    The invention relates to aliphatic alcohols, specifically to a method for continuously producing aliphatic alcohols of 3-4 carbon atoms used in organic synthevo
    The aim of the invention is to increase the productivity of the process by feeding the peiculate simple ether to the reactor separately from the reactants in a place located at a distance of 6.6-29.3 from the end of the reaction zone in terms of its total length
    Fig. 1 shows a schematic of an installation for carrying out the process with feeding the reagents to the head; Fig 2 is the same, with the supply of reagents in the cubic part.
    According to FIG. 1, in the filled acidic-2 end of the reaction zone (13.3% in
    through the pipeline 2, a mixture of an olefin and an alkane is fed through the tubular catalyst 1, and the water required for the reaction is fed through pipeline 3. In order to improve the control of the heat of reaction, water can be supplied in different places along the height of the reactor. As a result of a multiphase reaction, alcohol is formed at a high temperature and under pressure in the presence of an acid catalyst. Separated from the target product, the recycled simple effcr is fed through conduit 4. In the downstream part of the reactor, the reaction product is fed through conduit 5 to the separator 6j where it is separated into the organic phase discharged through conduit 7 and the aqueous phase withdrawn through conduit 8o. Both phases are recycled in a known manner. The exhausted olefin of the organic phase can be recycled depending on the desired degree of conversion. Separated ether is returned to the process via pipe 4.
    According to FIG. 2, the reactants are fed to the bottom part of the reactor 1, and the recycled ether is fed to its upper part. In this case, the reactor is equipped with a heating jacket 9. A quality catalyst is used to catalyze the catalyst, preferably thermostable sulphate-acid ion-exchange resins.
    A measure of the productivity of a process is the degree of conversion of olefins. on and code for volume / time.
    in terms of the total length of the reacting zone).
    The recycle diisopropyl ether stream contains 98.7 wt.% 25 diisopropyl ether, 1.1 wt.% Isomeric hexenes and 0.2 wt.% Isopropyl alcohol. The reaction pressure is 100 bar, the average reaction temperature is 142 ° C.
    The reaction product is divided into 31.2 kg / h of the organic phase of the composition, wt.%: Propane / pr. Foam 60j diisopropyl ether 20.1j isopropyl alcohol 19.7; hexenes 0.2, withdrawn 25 through line 7 for rectification, and 584 kg / h of the aqueous phase with a content of 12 wt.% isopropyl alcohol and .0.1 wt.% diisopropyl ether, withdrawn through line 8 to the rectilo ilO fication.
    With an average conversion of 78% propene, I get –76.0 kg / h of isopropyl alcohol and 7.0 kg of diisopropyl ether of the above composition. The volume / time yield is 2.18 mol / l of catalyst per hour. Recycled ether is almost quantitative. but turn into alcohol. Alcohol yield 99.9% o
    Example 2 (according to the prototype) o Carried out according to example 1 with the difference that recycled diisopropyl ether is added to the initial stream consisting of slefine and water. In this case, the conversion of propene is reduced to 69%, 54.1 kg of isopropyl alcohol is obtained and 9.5 kg / h of diisopropyl ether. The volume / time yield is 2.0 mol iso45.
    50
    55
    Example 1 (according to FIG 1). A reactor with a length of 9 m and a diameter of 280 mm, filled with 450 liters of amberlite 252 — a strongly acidic cation exchange resin (the length of the reaction zone is 7.5 m), 74.1 kg of 92% propane and 54.0 kg of demineralized water are hourly added. . The temperature of the streams is brought to the reaction temperature using a preheater, the streams are fed to the main part of the reactor. In order to control the temperature regime, part of the water is discharged before the preheater and is fed into the reaction
    torus in several places along its height. In addition, another 7.0 kg / h of recycled diisopropyl ether is fed to the reactor at a location located 1 m from the border.
    zo
    in terms of the total length of the reacting zone).
    The recycle diisopropyl ether stream contains 98.7 wt.% 25 diisopropyl ether, 1.1 wt.% Isomeric hexenes and 0.2 wt.% Isopropyl alcohol. The reaction pressure is 100 bar, the average reaction temperature is 142 ° C.
    The reaction product is divided into 31.2 kg / h of the organic phase of the composition, wt.%: Propane / pr. Foam 60j diisopropyl ether 20.1j isopropyl alcohol 19.7; 0.2 hexene, withdrawn by 25 via line 7 for rectification, and 584 kg / h of the aqueous phase with a content of 12% by weight of isopropyl alcohol and .0.1% by weight of diisopropyl ether, withdrawn by line 8 for rectification .
    With an average conversion of 78% propene, I get –76.0 kg / h of isopropyl alcohol and 7.0 kg of diisopropyl ether of the above composition. The volume / time yield is 2.18 mol / l of catalyst per hour. The recycled ether is almost quantitative. turn into alcohol. Alcohol yield 99.9% o
    Example 2 (according to the prototype): This is carried out according to example 1 with the difference that the recycled diisopropyl ether is added to the initial stream consisting of slefen and water. In this case, the conversion of propene is reduced to 69%, 54.1 kg / h are obtained isopropyl alcohol and 9.5 kg / h of diisopropyl ether. The volume / time yield is 2.0 mol iso5
    0
    five
    propyl alcohol per liter of catalyzate per hour, and the formation of ether - 4, A%.
    Example 3 (according to figure 2). A reactor with a length of 13.5 mi of a free cross-sectional area of 5 cm, filled with 6.75 l of amberlite 252 - strongly acidic cation-exchange resin (length of the reaction zone is 13 m), 2,000 g of water and 527 g of 98.9% n-bu In addition, at a distance of 2.5 m from the end of the reaction zone (19.2% in terms of the total length of the reaction zone), 690 g of diisobutyl ether containing 96.3 mAco% sec-diisopropyl ether, 3, 4% by weight of butane dimers and 0.3% by weight of n-butenes.
    The pressure in the reactor is 60 bar, temperature. The reaction product is separated into aqueous and organic phases.
    By pipeline. 8 hourly discharged 1830 g of an aqueous solution containing 1.1% sec-butyl alcohol.
    The organic phase is separated by continuous distillation. From the liquid phase C, 580 g / h of sec-butanol, 690 g of diisobutyl ether and 40 g of water are separated. Hourly 8,330 g of liquid gas with content is obtained. n-butenes 90%. 60 g of this gas is removed from the process due to the alkane content in the feed gas, and the remaining 8270 g is recycled to the reactor. Recycled diisobutyl ether is almost quantitatively cleaved to alcohol. The degree of conversion of n-butenes is 90%. The volume / time yield is 1.20 mol / l of catalyst per hour. The alcohol yield is 99.9%.
    Example 4. Carried out as in example 1 with the difference that the recirculated diisopropyl ether is introduced into the reactor at the location
    at a distance of 2.2 m from the end of the reaction zone (29.3% B calculated on the total length of the reaction zone). Here, the conversion of propene is 76%. The yield per volume / time is 2.8 mol / l of catalyst per hour. The yield of isopropanol is almost 100%.
    Example 5. Carried out as in example 1 with the difference that the recirculated diisopropyl ether is introduced into the reactor at a location located at a distance of 0.5 m from the end of the reaction zone (6.6% in terms of total the length of the reaction zone). Here, the conversion of propene is 77% at a volume / time of 2.85 mop / l of catalyst per hour. Output
    isopropanol is 98.2%.
    The proposed method allows to increase the productivity of the process from 2.0 to 2.8-2.85 mol of alcohol per 1 liter of catalyst per hour.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    Method for the continuous production of aliphatic alcohols with the number of atoms
    3-4 carbon by reacting the corresponding olefin with water on a strongly acidic catalyst as a primary temperature and under pressure, separating the reaction product into an organic and aqueous phase, separating the target product and recycling the ether formed as a by-product of the ether
    so that, in order to increase the productivity of the process, recirculated ether is fed to the reactor separately from the reactants in a place located at a distance of 6.6-29.3% of the border
    the end of the reaction zone is recalculated for its total length.
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    类似技术:
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    US5463157A|1995-10-31|Process for preparing 3-methyl-2-pentene
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    同族专利:
    公开号 | 公开日
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    DK173271B1|2000-06-05|
    RO91490A|1987-04-30|
    FI82679C|1991-04-10|
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    RO91490B|1987-05-01|
    AU4264785A|1985-11-28|
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    CS340885A2|1989-04-14|
    JPS60260530A|1985-12-23|
    JPH0118061B2|1989-04-03|
    CS266569B2|1990-01-12|
    NO852001L|1985-11-25|
    EP0162362B1|1987-11-11|
    ES543053A0|1986-01-01|
    PL253569A1|1986-02-11|
    CA1246620A|1988-12-13|
    IN164716B|1989-05-13|
    AU576243B2|1988-08-18|
    YU84885A|1987-06-30|
    PL145417B1|1988-09-30|
    DE3560944D1|1987-12-17|
    YU43595B|1989-08-31|
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    DE3419392C1|1985-12-05|
    US4579984A|1986-04-01|
    AT30711T|1987-11-15|
    DK231785A|1985-11-25|
    ZA853297B|1985-12-24|
    FI851681A0|1985-04-29|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE1065398B|1959-09-17|
    US2533808A|1950-12-12|Manufacture of isopropyl alcohol |
    US2050445A|1932-06-20|1936-08-11|Air Reduction|Manufacture of ethyl alcohol|
    DE2233967C3|1972-07-11|1979-01-18|Deutsche Texaco Ag, 2000 Hamburg|
    DE2404329C3|1974-01-30|1981-03-19|Deutsche Texaco Ag, 2000 Hamburg|Method for filling and commissioning or restarting a fixed bed reactor designed as a trickle column|
    DE2429770C3|1974-06-21|1981-04-16|Deutsche Texaco Ag, 2000 Hamburg|Process for the production of lower alcohols by direct catalytic hydration of lower olefins|
    US4087471A|1977-05-20|1978-05-02|Petro-Tex Chemical Corporation|Fixed bed process for the production of t-butanol|
    US4182920A|1977-07-11|1980-01-08|The Dow Chemical Company|Process for hydration of olefins to produce alcohols|
    DE2759237C2|1977-12-31|1987-05-27|Huels Ag, 4370 Marl, De|
    DE3024146C2|1980-06-27|1983-07-21|Deutsche Texaco Ag, 2000 Hamburg|Process for the continuous production of alcohols having 3 to 5 carbon atoms|
    US4352945A|1981-10-30|1982-10-05|Chevron Research Company|Diisopropyl ether reversion in isopropanol production|
    US4405822A|1981-10-30|1983-09-20|Chevron Research Company|Diisopropyl ether hydration in isopropanol production|
    DE3336644A1|1983-10-08|1985-05-23|Deutsche Texaco Ag, 2000 Hamburg|METHOD FOR THE CONTINUOUS PRODUCTION OF ALCOHOLS|
    DE3512518A1|1985-04-06|1986-10-09|Deutsche Texaco Ag, 2000 Hamburg|METHOD FOR THE CONTINUOUS PRODUCTION OF LOW ALCOHOLS|DE3512518A1|1985-04-06|1986-10-09|Deutsche Texaco Ag, 2000 Hamburg|METHOD FOR THE CONTINUOUS PRODUCTION OF LOW ALCOHOLS|
    DE3628008C1|1986-08-19|1987-11-05|Deutsche Texaco Ag, 2000 Hamburg, De|
    AU598845B2|1986-08-19|1990-07-05|Rwe-Dea Aktiengesellschaft Fur Mineraloel Und Chemie|Process for the production of isopropanol and tertiary alcohols with 4 to 5 carbon atoms|
    DE3628007C1|1986-08-19|1987-11-05|Deutsche Texaco Ag, 2000 Hamburg, De|
    IN170837B|1987-11-17|1992-05-30|Council Scient Ind Res|
    US4935552A|1989-01-12|1990-06-19|Mobil Oil Corporation|Dual stage process for the production of ethers|
    AU651373B2|1990-07-25|1994-07-21|Mobil Oil Corporation|Reactor quenching for catalytic olefin hydration in ether production|
    US5162591A|1990-07-25|1992-11-10|Mobil Oil Corporation|Catalytic olefin hydration for ether production|
    US5444168A|1994-05-16|1995-08-22|Mobil Oil Corporation|Process for the production of symmetrical ethers from secondary alcohols|
    US5569789A|1994-12-01|1996-10-29|Mobil Oil Corporation|Multistage indirect propylene hydration process for the production of diisopropyl ether and isopropanol|
    CN1101799C|1999-12-13|2003-02-19|孙业茂|Multiple-section water circulation resin process of preparing para-butanol|
    US20040236158A1|2003-05-20|2004-11-25|Collin Jennifer Reichi|Methods, systems and catalysts for the hydration of olefins|
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    RU2453526C2|2010-05-04|2012-06-20|Общество с ограниченной ответственностью "Научно-производственное объединение ЕВРОХИМ"|Method of producing tertiary butyl alcohol|
    US8558036B2|2010-11-15|2013-10-15|Saudi Arabian Oil Company|Dual phase catalysts system for mixed olefin hydrations|
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    RU2462447C1|2011-08-26|2012-09-27|Общество с ограниченной ответственностью "Научно-производственное объединение ЕВРОХИМ"|Method of producing tertiary butyl alcohol|
    SG11201402373UA|2011-12-05|2014-06-27|Saudi Arabian Oil Co|Hydrophilic membrane integrated olefin hydration process|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE3419392A|DE3419392C1|1984-05-24|1984-05-24|Process for the continuous production of isopropyl alcohol or sec. Butyl alcohol|
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