• 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:
    Ethylene glycol is purified, particularly for fiber- grade applications, by removal of the residual ethylene carbonate from which the glycol was derived, by distilling the effluent from a reactor in which ethylene carbonate is hydrolyzed to ethylene glycol to produce a lower-boiling fraction comprising ethylene glycol and water and a higher-boiling fraction comprising ethylene glycol, higher glycols, and concentrated hydrolysis catalyst, and recirculating the higher-boiling fraction to reflux against the lower-boiling product, thereby reducing the ethylene carbonate content of the ethylene glycol.
    公开号:SU1604153A3
    申请号:SU853896549
    申请日:1985-05-08
    公开日:1990-10-30
    发明作者:Бекер Митчелл；М.Закс Говард
    申请人:Сайентифик Дизайн Компани, Инк (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to an improved method for purifying ethylene glycol obtained by hydrolysis of ethylene carbonate in the presence of a catalyst from residual ethylene carbonate to the content of the latter in ethylene glycol suitable for producing a fiber-grade product.
    The purpose of the invention is to increase the quality of the target product due to a decrease in the ethylene carbonate content.
    Example 1 of Simple Instant
    evaporation.
    The stream leaving the hydrolysis reactor contained 70.3 wt.% Ethylene glycol (EG), 3 wt.% Ethylene carbonate (EC), 0.7 wt.% Methyltriphenylphosphonium iodide (catalyst), 24 wt.% Water and 2 wt.% of higher glycols (VG) in amounts of 290 g / h (100 May / h) are subjected to simple instant evaporation at 170 ° C and a pressure of 25.0 mm Hg. Art. in a 200 ml container. The resulting steam in the amount of 96.3 May / h contains 74.7% by weight of EG and VG, 0.3 May,% EC and 25% by weight of water.
    The liquid obtained in the amount of 3.7 wt / h contains 61 wt.% EG, 0.04 wt.% EC, 20 wt.% VG and 19 wt.% Catalyst. It can be recycled.
    05 Oh
    sd
    with

    with
    in the hydrolife reactor for reuse after purification from VG. The level of EC content is still undesirably high to produce polymer.
    Example 2: Recycle catalyst solution.
    An Oldershaw column is installed above the instant evaporation chamber used in Example 1, containing twenty mesh plates with a diameter of 3 inches (approximately 76 mm). Instead of returning the instantly evaporated liquid containing the catalyst to the hydrolysis reactor, the liquid is fed to: the upper plate of the column. The liquid then flows down during countercurrent contact with the steam formed during the instantaneous evaporation of the supplied liquid. When recirculating 3.3 hours of the high-boiling fraction (ICF), each part of the hydrolyzate is given an EG containing 0.08% by weight of EC, and by recycling 8.2 hours, an EG containing 0.14% by weight, EC, In this mode of operation, recirculation reduces the EC content in the target product, although there is an optimal recirculation rate.
    Primerz, Recycling + hydrolyzate fractionation.
    Using the setup of Example 2, the hydrolyzate feed site is changed, directing it to the midpoint of the fractionation column, i.e. on the 10th plate of 20, instead of feeding instantaneous evaporation into the chamber located below the plate under conditions of examples 1 and 2, the rate of recirculation to plate 20 is changed and the EC content in ethylene glycol is measured, obtaining the results presented in the table.
    Comparing the results obtained with, with example 2, one can see that if the hydrolyzate enters the tenth plate, and not into the instant evaporation chamber, then the high recirculation rates do not increase the EC content in the EG.
    :
    A further improvement in the quality of the EG is achieved by increasing the temperature of flash evaporation to 190 ° C so that, with sufficient recirculation, the EC content in the EG is lower than 300 hours per million (i.e., when the EC is no longer detectable).
    The drawing shows the implementation of the proposed method.
    Example 4, Hydrolyzate from a hydrolysis reactor, containing, by weight, 70.3 EG, 3 EC, 24 water, 2 BG and 0.7 catalyst, in an amount of 100 May / h at 170 C and under pressure sufficient to maintain it in the liquid phase, is heated to the heat exchanger (1) and subjected to flash evaporation at a pressure of 680 mm Hg. when the hydrolyzate enters the tenth plate in a 20-plate distillation column (2), EC, cataln.ator and a certain amount of EG moves down to meet with the recirculating fluid going down from the dislocated plates. The liquid at the bottom of the column contains 61 wt. % EG, 0.04 wt.% EC, 20 wt.% VG and 19 wt.% Catalyst. The evaporator (3) provides steam for contact with the liquid passing down the plates for 4.5 May. h of liquid for each mass fraction of hydrolyzate (450 w / h is cooled in heat exchanger (5) and recirculated through line (4) to the tenth plate to bring into contact with the EG and water vapor rising along the column, and complete the EC hydrolysis The remainder of the liquid at the bottom of the column (3.7 w / w) is removed without returning to the head reactor.
    The steam passed through the top along the line (6) is cooled in the heat exchanger (7) and then subjected to further distillation (not shown), obtaining 96.3 w / w EG fiber grade containing 0.02 wt,% EC; 73 wt.% EG; 26 wt.% Water and 2. mas,% VG.
      /
     The proposed method allows to improve the quality of ethylene glycol by reducing the content of ethylene carbonate in it to 0.02-0.08 wt.%.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method of purification of ethylene glycol, obtained by hydrolysis of ethylene carbonate in the presence of a catalyst, o, tl, is the fact that, in order to improve the quality of the target product due to a decrease in the content of ethylene carbonate, a hydrolyzate containing 70 wt.% Ethylene glycol, 3 wt.% ethylene carbonate, 0.7 wt.% methyltriphenylphosphonium iodide, 24 mW of water and higher glycols, is subjected to distillation in a vapor-liquid contact column at a temperature of 170 to 190 s and a pressure of 250 to 680 mm Hg. Art. and a stream containing ethylene glycol and water, you 51604
    water in the form of a low boiling fraction, and a liquid stream containing 0.1% by weight ethylene glycol, 0.04% by weight,% ethyl acetate, 20% by weight of higher glycols and 19% by weight of methyltriphenylphosphonium iodide fractions recycle from 2.8 to 7.4 parts of the high-boiling fraction for each part of the hyd53
    through the contact column in a countercurrent to the low boiling fraction to reduce the ethylene carbonate content in the specified lower boiling fraction to values below 0.05 wt%, and return the rest of the high boiling fraction to the ethylene carbonate hydrolysis step.
    The results of the experiments for example
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    同族专利:
    公开号 | 公开日
    DE3574369D1|1989-12-28|
    YU45715B|1992-07-20|
    US4519875A|1985-05-28|
    RO91716A|1987-05-15|
    YU76385A|1987-12-31|
    ES8607895A1|1986-06-01|
    DD232483A5|1986-01-29|
    BR8502190A|1986-01-07|
    CA1241347A|1988-08-30|
    ES542970A0|1986-06-01|
    KR850008656A|1985-12-21|
    BG51039A3|1993-01-15|
    IN163264B|1988-08-27|
    EP0161111B1|1989-11-23|
    KR920003774B1|1992-05-14|
    AU570108B2|1988-03-03|
    ZA853523B|1986-12-30|
    JPS60239429A|1985-11-28|
    EP0161111A3|1987-04-01|
    AU4172285A|1985-11-14|
    EP0161111A2|1985-11-13|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2594159C2|2012-01-10|2016-08-10|Чайна Петролеум Энд Кемикал Корпорейшн|Method of separating ethylene glycol and 1,2-butanediol|US3629343A|1968-10-11|1971-12-21|Vnii Neftekhim Protsessov|Process for the production of alkylene glycols|
    US3809724A|1971-09-08|1974-05-07|Halcon International Inc|Preparation and recovery of alkylene glycols|
    US4057471A|1975-09-12|1977-11-08|Halcon International, Inc.|Recovery of alkylene glycols|
    US4021311A|1975-09-12|1977-05-03|Halcon International, Inc.|Recovery of alkylene glycols by azeotropic distillation with 1,2,3-trimethyl benzene|
    US4314945A|1977-12-22|1982-02-09|Union Carbide Corporation|Alkylene carbonate process|
    US4117250A|1977-12-22|1978-09-26|Union Carbide Corporation|Continuous process for producing alkylene glycols from alkylene carbonates|
    US4160116A|1978-08-28|1979-07-03|Showa Denko K.K.|Process for the production of alkylene glycols|
    GB2048698B|1979-05-11|1983-03-30|Eardley D|Rapid response distillation method and apparatus for use therein|
    CA1121389A|1979-05-24|1982-04-06|Hiroshi Odanaka|Processfor the production of alkyleneglycols|
    JPS5690029A|1979-12-24|1981-07-21|Nippon Shokubai Kagaku Kogyo Co Ltd|Preparation of high-purity alkylene glycol|
    JPS5692228A|1979-12-27|1981-07-25|Nippon Shokubai Kagaku Kogyo Co Ltd|Preparation of high-purity alkylene glycol|
    JPS6125693B2|1980-02-22|1986-06-17|Nippon Shokubai Kagaku Kogyo Kk|
    JPS5758328B2|1980-04-03|1982-12-09|Showa Denko Kk|
    JPS6058897B2|1980-06-30|1985-12-23|Nippon Shokubai Kagaku Kogyo Kk|
    JPS6055042B2|1981-12-25|1985-12-03|Nippon Shokubai Kagaku Kogyo Kk|
    US4400559A|1982-06-14|1983-08-23|The Halcon Sd Group, Inc.|Process for preparing ethylene glycol|
    JPH0427972B2|1982-07-14|1992-05-13|Mitsubishi Yuka Kk|US4691041A|1986-01-03|1987-09-01|Texaco Inc.|Process for production of ethylene glycol and dimethyl carbonate|
    US4830712A|1987-09-29|1989-05-16|Union Carbide Corporation|Process for refining ethylene glycol|
    US5019669A|1989-03-10|1991-05-28|Chemical Research & Licensing Company|Alkylation of organic aromatic compounds|
    US5080871A|1989-03-10|1992-01-14|Chemical Research & Licensing Company|Apparatus for alkylation of organic aromatic compounds|
    US5118872A|1989-03-10|1992-06-02|Chemical Research & Licensing Company|Process for conducting heterogeneous chemical reactions|
    US5672780A|1995-08-11|1997-09-30|Eastman Kodak Company|Purification of ethylene glycol recovered from polyester resins|
    EP1119561B1|1998-10-07|2003-04-16|Huntsman Petrochemical Corporation|Process for the preparation of alkylene carbonate|
    US6156160A|1998-10-07|2000-12-05|Huntsman Petrochemical Corporation|Alkylene carbonate process|
    US6258962B1|1999-06-14|2001-07-10|Mobil Oil Corp.|Process for producing alkylene carbonates|
    US6407279B1|1999-11-19|2002-06-18|Exxonmobil Chemical Patents Inc.|Integrated process for preparing dialkyl carbonates and diols|
    US20090221840A1|2006-03-20|2009-09-03|Masahiko Yamagishi|Process for purifying ethylene carbonate, process for producing purified ethylene carbonate, and ethylene carbonate|
    JP5282366B2|2006-03-20|2013-09-04|三菱化学株式会社|Method for purifying ethylene carbonate, method for producing purified ethylene carbonate, and ethylene carbonate|
    WO2019213029A1|2018-04-30|2019-11-07|Scientific Design Company, Inc.|Process for preparing ethylene glycol|
    TW201945328A|2018-04-30|2019-12-01|美商科學設計有限公司|Method for improving the manufacture of ethylene glycol|
    EP3788027A4|2018-04-30|2022-03-09|Scient Design Co|Recirculating process for preparing ethylene glycol|
    TW201945071A|2018-04-30|2019-12-01|美商科學設計有限公司|Epoxidation process with concentrated ethylene oxide solutions|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US06/608,639|US4519875A|1984-05-09|1984-05-09|Purification of ethylene glycol derived from ethylene carbonate|
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