• 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:
    Process for the preparation of a cyclic sulphate of general formula (I) by rapid reaction at a temperature of between 150 and 250 DEG C of concentrated sulphuric acid with a glycol of general formula (II). …<??>In the general formulae (I) and (II), R1, R2, R3, R4, R5 and R6, which are identical or different, denote hydrogen, halogen, alkyl, alkoxy, aryl, aryloxy or alkoxycarbonyl and n is equal to 0 or 1. …<IMAGE>…
    公开号:SU1657063A3
    申请号:SU894614050
    申请日:1989-05-15
    公开日:1991-06-15
    发明作者:Массонно Вивиан；Мюльхаузер Мишель
    申请人:Рон-Пуленк Санте (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to an improved process for the preparation of ethylene sulfate of the formula Si -QJ
    II O 0
    oh
    which finds use as an intermediate in organic synthesis, for example, in ethoxylation reactions.
    The purpose of the invention is to intensify and simplify the process.
    The goal is achieved according to the method consisting in the interaction of equimolar amounts of concentrated sulfuric acid and 1,2-ethanediol (ethylene glycol) at 200 ° C and a pressure of 0.13 KPa for 1C minutes.
    The drawing shows a diagram of the reactor in which the process is carried out.
    Example. 6.2 g of ethylene glycol (0.1 mol) is mixed with 9.8 g of 97% sulfuric acid (0.097 mol). 2.5 g of the mixture is introduced into the reactor with a syringe. The reactor is heated at 200 ° C using a heating winding. The apparatus is under reduced pressure (1 mm Hg, 0.13 kPa). The residence time of the mixture of ethylene glycol and sulfuric acid in the heated part of the reactor is 10 minutes.
    The ethylene sulfate formed is collected in a Vigro column placed in a cylinder with dry ice. At the end of the reaction, the Vigrau column is rinsed with dichloromethane. After decanting the resulting solution and evaporating dichloromethane, 0.85 g of ethylene sulfate is obtained in the form of white crystals. The yield is 45% with respect to the sulfuric acid used.
    . Reactor for supplying The method has a hole 1 for the introduction of reagents, a flushing tube 2
    yo
    Ov SL VI About OJ

    Ca
    reagents, heating winding 3, tank 4 for receiving ethylene sulfate after rinsing the Vigro column, Vigro column 5, the cooling cylinder 6. The position 7 designates the connection of the installation to reduced pressure. The advantages of the proposed method are to conduct it in a significantly short time (10 min. Against 50 h), as well as in the simplicity of the technology due to the exclusion of additional operations associated with the isolation of the desired product, for example, recovery of toxic solvent and the absence of complex distillation.
    0
    five
    权利要求:
    Claims (1)
    [1]
    The invention The method of producing ethylene sulfate of the formula Icn2 - ch2
    II
    s- °
    xx
    oh oh
    the interaction of equimolar amounts of concentrated sulfuric acid and 1,2-ethanediol with heating, characterized in that in order to intensify and simplify the process, the latter is carried out at a temperature of 200 ° C and a pressure of 0.13 KPa for 10 minutes.
    S
    Sj
    eleven
    }
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    同族专利:
    公开号 | 公开日
    GR3003629T3|1993-03-16|
    FI892327A0|1989-05-15|
    ZA893620B|1990-01-31|
    DK238289D0|1989-05-16|
    FR2631340B1|1990-07-27|
    YU46933B|1994-06-24|
    EP0343053B1|1992-01-22|
    DE68900749D1|1992-03-05|
    KR900018067A|1990-12-20|
    PT90573B|1994-08-31|
    EP0343053A1|1989-11-23|
    DK238289A|1989-11-17|
    AU618092B2|1991-12-12|
    CA1305712C|1992-07-28|
    YU99389A|1990-06-30|
    AT71943T|1992-02-15|
    JPH0217183A|1990-01-22|
    CN1037708A|1989-12-06|
    FR2631340A1|1989-11-17|
    IL90306D0|1989-12-15|
    US4924007A|1990-05-08|
    ES2028455T3|1992-07-01|
    HU201542B|1990-11-28|
    AU3479589A|1989-11-16|
    FI892327A|1989-11-17|
    PT90573A|1989-11-30|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE1049870B|1959-02-05|VEB Filmfabrik AGFA Wolfen, Wolfen |Process for the preparation of cyclic sulfuric acid esters of diprimary glycols|
    FR1171347A|1956-10-24|1959-01-23|Wolfen Filmfab Veb|Process for preparing sulphates of alkenes or olefins|
    FR2628423B1|1988-03-08|1991-09-13|Rhone Poulenc Sante|PROCESS FOR THE PREPARATION OF CYCLIC SULFATES|US5149844A|1989-10-20|1992-09-22|Air Products And Chemicals, Inc.|Heterocyclic diorganotin catalysts for use in polyurethane systems|
    FR2664274B1|1990-07-09|1992-09-11|Rhone Poulenc Sante|PROCESS FOR THE PREPARATION OF CYCLIC SULFATES.|
    US5171892A|1991-07-02|1992-12-15|E. I. Du Pont De Nemours And Company|Chiral phospholanes via chiral 1,4-diol cyclic sulfates|
    US6180799B1|2000-05-01|2001-01-30|The United States Of America As Represented By The Secretary Of The Air Force|Sulfalation of tetraol|
    US8247526B2|2010-12-20|2012-08-21|E I Du Pont De Nemours And Company|Process for the preparation of polyalkylene ether glycol|
    CN107353277B|2017-07-11|2020-01-31|湖南有色郴州氟化学有限公司|Preparation method of cyclic sulfates|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR8806523A|FR2631340B1|1988-05-16|1988-05-16|PROCESS FOR THE PREPARATION OF CYCLIC SULFATES|
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