• 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:
    1. Process for making and purifying 1,2-dichloroethane by reacting ethylene and chlorine in a reaction zone having a liquid medium containing chlorinated C2 -hydrocarbons circulated therein, at a temperature lower than the evaporation temperature of said medium under the pressure prevailing inside the reaction zone, in the presence of a customary chlorination-inducing catalyst and optionally an inhibitor reducing the formation of by-products, with the resultant formation of crude 1,2-dichloroethane, removing the crude dichloroethane from the reaction zone and purifying it in a separate fractionating zone placed downstream thereof, which comprises : a) introducing approximately equimolar proportions of ethylene and chlorine into the circulated liquid medium ; intensively mixing the whole in a mixing zone and then reacting the mixture in a reaction zone at a temperature of about 75-200 degrees C under a pressure of about 1-15 bars, the mean sojourn time of the reaction mixture in the mixing and reaction zone being about 1-15 hours ; b) removing a portion of the liquid reaction mixture from the reaction zone and subdividing said portion into two partial streams, of which one is passed through a heat exchanger to give off calorific energy, and recycled at lower temperature to the mixing and reaction zone ; whilst the second partial stream is introduced into an expansion vessel in which a quantity adequate to the reaction product formed in the reaction zone and optionally also a proportion of 1,2-dichloroethane originating from a third source and introduced into the reaction zone is evaporated from said second partial stream ; resulting vaporous matter is introduced into a fractionating column whilst unevaporated liquid matter of the second partial stream is recycled into the mixing and reaction zone of the circulated liquid medium ; and c) separating distillatively 1,2-dichloroethane from the vaporous matter introduced into the fractionating column with the use of a portion of the heat energy transferred inside the heat exchanger and removing the 1,2-dichloroethane overhead, higher chlorinated products being obtained in the column base portion from which they are removed and worked up separately.
    公开号:SU1396960A3
    申请号:SU823494114
    申请日:1982-09-20
    公开日:1988-05-15
    发明作者:Хундек Йоахим；Шольц Харальд；Хеннен Ханс；Куксдорф Бернхард；Пюше Херберт；Фомберг Хайнц；Линк Герхард
    申请人:Хехст Аг (Фирма )；
    IPC主号:
    专利说明:

    The invention relates to improved methods for producing 1,2-dichloroethane, widely used as an intermediate in the production of vinyl chloride and as a solvent,
    The object of the invention is to increase the yield of the desired product.
    Example 1. In a 25 m reactor, 20,000 l of 1,2-dichloroethane (DCE) is charged and iron chloride is added in an amount of 300 mg per 1 kg of DCE. At 2.5 atm and 105-10, 2277 kg / h of ethylene and 5737 kg / h of chlorine containing 4% by volume of inert gases and 20 air are introduced into the reactor.
    The liquid stream (446,384) leaving the reactor is divided into two streams in the ratio
    j
    969602
    3.0 atm and. 5.1 t / h DCE are obtained. In addition, an additional 12.4 t / h of DCE is fed to the reaction zone, independently obtained by oxylazing ethylene having a temperature and containing 0.4 wt.% Of high boiling impurities. 201.5 t / h of the reaction mass is withdrawn from the reactor, which is divided into two streams in the ratio 1: 9. The first stream is sent to the heat exchanger, the second to the pressure relief apparatus, where 17.5 t / h of crude DCE are evaporated. Crude DCE is sent to a distillation column.
    The temperature at the bottom of the column is 82, at the top is 68. The pressure in the upper part of the column is 0.6 atm, the ratio of pressures in the reactor and the column10
    1: 0.275., First sent to heat 2O not 5.
    Ethylene purity
    25
    A mannik where it gives off heat is sent to the reactor through a circulation pipe. The second is sent to the pressure relief apparatus. In the pressure relief apparatus, 6.384 (8000 kg / h) of crude dichloroethane is evaporated, which is sent to a distillation column. The liquid in the reaction state 90 is returned to the reactor. zo
    Dichloroethane contains 0.1 May. 1,1,2-trichloroethane (TCE) 0.01 wt.% Ethyl chloride and 1,1-dichloroethane. The enrichment of the circulating reaction medium TCE for a long period of reactor operation does not occur.
    The distillation column is heated by the heat given off in the heat exchanger by the first stream of DCE. The temperature in its lower part, the pressure in the upper part is 0.7 atm, the ratio of pressures in the reactor and the column is 3.5.
    Reaction products with a boiling point lower than that of DCE
    35
    40
    The product yield is 99.5% based on ethylene and 99.6% based on chlorine, purity 99.99%.
    Pressure in the pressure relief apparatus - 1., 4 atm.
    Simultaneously with the production of DCE, further purification of 12.4 t / h is achieved, independently obtained DCE.
    Process number 3. The process is carried out according to Example 2, but the distillation column operates at a pressure of 1 atm, the flow ratio is I to 0.33, the temperature in the lower part of the column is 95, and in the top is 84 seconds. The yield of 1,2-dichloroethane is 99.6, purity is 99.99%. The pressure in the pressure relief apparatus is 1.8 atm.
    Example4. A 15 l reactor is charged with 17.35 kg of DCE containing 9 g of ferric chloride. The pressure in the reactor is 1.1 atm. 110 l / h of ethylene and chlorine and 10 l / h of air are introduced into the reactor. The temperature in the reaction zone is 80-83 s.
    The process is conducted according to example 1, but
    water from the top of the reaction 45 flow of DCE coming out of the heat exchanger is sent to the cooler where the DCE carried away with them condenses, which is returned to the reaction zone. 102 uncondensed gases containing 2.5 vol.% Of DCE and 3 vol.% Each of ethyl chloride and ethylene are sent to the incinerator.
    In a distillation column, 7972 kg / h of DCE was separated with a basic substance content of 99.99%. The output of chlorine 99,57%.
    IT p and m e r 2. The process of obtaining EDC will follow in Example 1, but with
    no 5.
    The product yield is 99.5% based on ethylene and 99.6% based on chlorine, purity 99.99%.
    Pressure in the pressure relief apparatus - 1., 4 atm.
    Simultaneously with the production of DCE, further purification of 12.4 t / h is achieved, independently obtained DCE.
    Process number 3. The process is carried out according to Example 2, but the distillation column operates at a pressure of 1 atm, the flow ratio is I to 0.33, the temperature in the lower part of the column is 95, and in the top is 84 seconds. The yield of 1,2-dichloroethane is 99.6, purity is 99.99%. The pressure in the pressure relief apparatus is 1.8 atm.
    Example4. A 15 l reactor is charged with 17.35 kg of DCE containing 9 g of ferric chloride. The pressure in the reactor is 1.1 atm. 110 l / h of ethylene and chlorine and 10 l / h of air are introduced into the reactor. The temperature in the reaction zone is 80-83 s.
    The process is conducted according to example 1, but
     the flow of DCE leaving heat exchange0
    five
    Nick, an additional 0.95 kg / h of crude DCE, obtained independently by another method and containing 0.38% TCE and 0.05% of other impurities, is introduced. I.
    The pressure in the distillation column 0.55 ATM, the ratio of the pressures in the reactor and column 2.
    The yield of DCE is 99.4% for ethylene and 99.6% for chlorine, purity 99.99%.
    PRI me R 5. The process is carried out in an industrial unit with a capacity of 100,000 tons of DCE per year in accordance with Example 1, but the ratio
    1: 2 streams. The pressure in the reactor is 5 atm, and reduced chlorine is used. The temperature in the reaction zone .14-14-14b. .
    In addition to the heat exchanger, ensuring the rectification of DCE, two more heat exchangers are installed, in which 7 t / h of water vapor with a temperature of 136 ° and a pressure of 3.4 atm and 0.65 t / h of steam with a temperature of 120 ° and pressure 2.0 atm.
    The pressure in the distillation column 0.5 ATM, the ratio of the pressures in the reactor and column 10.
    The yield of DCE 99.4%, purity 99.99%.
    Thus, obtaining DCE in accordance with the invention makes it possible to increase its yield by 3.4-4.6%. Time
    stay in the mixing zones and the reaction of 2 o Pressure 0.5 to 1 atm and 78-95 C in
    for examples: 1-3.1 h; 2, 1.4 h; 2-3 h; 4 - 12.1 h; 5 - 2 hours
    权利要求:
    Claims (4)
    [1]
    1. A method of producing 172-dichloroethane by reacting equimole rye quantities of ethylene and chlorine in a circulating liquid medium containing chlorine derivatives of ethane, in the presence of iron chloride as a catalyst and, if necessary, oxygen used as an inhibitor, at a temperature 80 before, but below the boiling point of the medium at the pressure present in the reaction zone, and the starting materials are vigorously stirred in the mixing zone and sent to the reaction zone, 1,2-dichloroethane is formed is removed from the reaction zone and then purified from 1,2-dichloroethane is removed from the head of the rectification column, and products with a higher degree of chlorination from the bottom of the distillation column, which is heated in order to increase the yield, lj- 2-dichloroethane, 1,2-dichloroethane is used as a circulating medium, the process is carried out at the residence time of the reagent.
    25
    thirty
    35
    40
    45
    the lower part of the distillation colo and with the ratio of pressures in the reaction zone and in the distillation column is not 2-10: 1.
    [2]
    2. The method according to claim 1, characterized in that the
    In the reaction medium, inert gases or low-boiling chlorinated carbon hydrogens, such as ethyl chloride, are removed from the upper part of the reaction zone and transferred to a refrigerator, and 1,2-chloroethane, which is entrained with these products, is condensed and returned to the reaction zone.
    [3]
    3. Method according to paragraphs. 1 or 2, which differs in that the independently obtained crude 1,2-dichloroethane is introduced through a refrigeration unit into the reaction zone or into the reaction mass stream exiting the heat exchanger before returning it to the reaction zone.
    [4]
    4. Method according to paragraphs. 1-3, which is warm, as a result of the reaction, and is obtained for the rectification of the obtained independently 1,2-dichloroethane.
    Priority item
    09.21.81 2-4;
    07/09/82 in Clause 1.
    VNIIPI Order 2508/59
    Random polygons pr-tie, Uzhgorod, st. Project, 4
    1396960
    In the reaction and mixing zones of 1.412.1 hours and a pressure of 1.1-5 atm, the reaction mass removed from the reaction zone is divided into two streams in a ratio of 1: 0.275-1: 9, with the first stream being sent to a heat exchanger, where it gives its heat, and after passing the heat exchanger return
    to the mixing and reaction zones, while the second stream is sent to the expansion apparatus to release pressure, where it is partially evaporated at a pressure of 1.4 to 1.8 atm, and the non-evaporated liquid part is returned to the mixing and reaction zones, and 1,2-dichlorostan vapor is sent to a distillation column, where 1,2-dichloroethane is purified by rectification at
    five
    0
    five
    0
    five
    the lower part of the distillation column and at a ratio of pressures in the reaction zone and in a distillation column 2-10: 1.
    2. The method according to claim 1, characterized in that the contained
    In the reaction medium, inert gases or low-boiling chlorinated hydrocarbons, such as ethyl chloride, are withdrawn from the upper part of the reaction zone and transferred to a cooler, where 1,2-dichloroethane, carried with these products, is condensed and returned to the reaction zone.
    3. Method according to paragraphs. 1 or 2, characterized in that the obtained independently crude 1,2-dichloroethane is introduced through a cooler into the reaction zone or into the reaction mass stream exiting the heat exchanger before returning it to the reaction zone.
    4. Method according to paragraphs. 1-3, wherein the heat released from the reaction is used to rectify 1,2-dichloroethane obtained independently.
    Priority points;
    09.21.81 2-4;
    07/09/82 in Clause 1.
    Circulation 370 Subscription
    类似技术:
    公开号 | 公开日 | 专利标题
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    JP4859084B2|2012-01-18|Method and apparatus utilizing reaction heat generated when producing 1,2-dichloroethane
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    US4324932A|1982-04-13|Process for the manufacture of vinyl chloride by the thermal cracking of 1,2-dichloroethane
    US3634200A|1972-01-11|Ethylene dichloride purification by plural stage distillation
    CS225148B2|1984-02-13|The production of dichloroethane
    US3557229A|1971-01-19|Oxychlorination of ethane to vinyl chloride
    SU404220A1|WAY OF OBTAINING 1, 1, 1-TRICHLORETHANE
    JPH0819014B2|1996-02-28|Method for producing ethane dichloride
    US3745103A|1973-07-10|Method for making 1,1,1-trichloroethane by photochemical chlorination of 1,1-dichloroethane
    US3548014A|1970-12-15|Process for reducing the 2-chlorobutadiene-| and benzene contents of 1,2-dichloroethane recovered from 1,2-dichlororethane thermally cracked into vinyl chloride
    US2814649A|1957-11-26|Process for separation of chlorinated xylenes
    US3761361A|1973-09-25|Production and purification of vinyl chloride
    US3903183A|1975-09-02|Production of chlorinated hydrocarbons
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    US3886221A|1975-05-27|Production of chlorinated hydrocarbons
    同族专利:
    公开号 | 公开日
    AR229367A1|1983-07-29|
    EP0075742B1|1984-11-07|
    ES515671A0|1983-05-01|
    NO154879B|1986-09-29|
    EP0075742A1|1983-04-06|
    DE3261204D1|1984-12-13|
    CA1204787A|1986-05-20|
    AU8854582A|1983-03-31|
    HU191189B|1987-01-28|
    NO154879C|1987-01-07|
    NO823183L|1983-03-22|
    ES8305292A1|1983-05-01|
    MX155726A|1988-04-20|
    CS235027B2|1985-04-16|
    AU554470B2|1986-08-21|
    BR8205514A|1983-08-23|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    NL130522C|1964-04-01|
    BE725636A|1968-12-18|1969-06-18|
    US3839475A|1971-05-20|1974-10-01|Allied Chem|Process for the production of ethylene dichloride|
    GB1422303A|1973-06-11|1976-01-28|Stauffer Chemical Co|Production of ethylene dichloride|
    DE2743975B1|1977-09-30|1979-03-01|Bayer Ag|Process for the preparation of a practically vinyl chloride-free 1,2-dichloroethane|
    DE2935884A1|1979-09-05|1981-04-02|Wacker-Chemie GmbH, 8000 München|METHOD FOR PRODUCING 1,2-DICHLORETHANE|DE3445896C1|1984-12-15|1986-04-10|Dynamit Nobel Ag, 5210 Troisdorf|Process for the continuous production of 1,2-dichloroethane|
    DE3604968A1|1985-02-19|1986-08-21|Kanegafuchi Kagaku Kogyo K.K., Osaka|METHOD FOR PRODUCING DICHLORETHANE|
    DE3519161A1|1985-05-29|1986-12-04|Hoechst Ag, 6230 Frankfurt|METHOD FOR PURIFYING 1,2-DICHLORETHANE|
    EP0211151B1|1985-05-30|1992-09-09|International Business Machines Corporation|Procedure for controlling the order of editing cells in a spreadsheet|
    DE4117592A1|1991-05-29|1992-12-03|Huels Chemische Werke Ag|REACTOR FOR PHASE HETEROGENEOUS REACTIONS|
    CZ286067B6|1993-01-27|2000-01-12|Hoechst Aktiengesellschaft|Process for preparing 1,2-dichloroethane by direct chlorination and apparatus for making the same|
    DE4425872A1|1994-07-21|1996-01-25|Hoechst Ag|Process and device for producing 1,2-dichloroethane by direct chlorination with exhaust gas recirculation|
    TW442449B|1996-07-04|2001-06-23|Hoechst Ag|Process for preparing 1,2-dichloroethane by direct chlorination|
    DE19904836C1|1999-02-06|2000-08-31|Krupp Uhde Gmbh|Process for the preparation of 1,2-dichloroethane|
    DE19916753C1|1999-04-14|2000-07-06|Krupp Uhde Gmbh|Production of 1,2-dichloroethane, used in the manufacture of vinyl chloride, by reaction of chlorine and ethylene in plant including a downdraft evaporator|
    DE19953762C2|1999-11-09|2003-07-10|Uhde Gmbh|Process for the use of the resulting in 1,2-dichloroethane production in Direktchlorierungsreaktor heat|
    DE10050315C2|2000-10-10|2003-08-21|Uhde Gmbh|Process for dissolving salts in 1,2-dichloroethane by means of ultrasound and device for carrying out the process|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE19813137513|DE3137513A1|1981-09-21|1981-09-21|METHOD FOR PRODUCING 1,2-DICHLORETHANE|
    DE19823225732|DE3225732A1|1982-07-09|1982-07-09|Process for the preparation and purification of 1,2-dichloroethane|
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