• 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:
    Fluoroxy-halo-compounds are prepared by direct reaction between fluorine and organic compounds having a molecular structure in which at least one oxygen atom is directly bound to a carbon atom in the carbonylic form, in the presence of a fluorination catalyst, in a gaseous phase, at an absolute pressure of between 50 and 800 kPa and at a temperature higher than -50°C and up to 250°C, under conditions of continuous feeding of the reactants and a continuous removal of the reaction product.
    公开号:SU1470176A3
    申请号:SU864027172
    申请日:1986-03-10
    公开日:1989-03-30
    发明作者:Гуглиельмо Джорджио；Конте Лино；Мария Карлина Филиппо
    申请人:Аусимонт С.П.А. (Фирма)；
    IPC主号:
    专利说明:

    one
    but
    one
    This invention relates to a process for the preparation of a fluoro-oxyhalo compound of the general formula
    (Yu „with (p) approx.
    where R is alkyl having 1 or 2 carbon atoms, fully halogenated by fluorine or. fluorine and chlorine, or R is a perfluorinated alkoxyalkyl having 5 carbon atoms i p is an integer equal to 1 or 2J
    m is an integer equal to 3-p, used as oxidizing agents in bleaching and fluorine-organic synthesis intermediates.
    The purpose of the invention is to increase the selectivity of the process and output.
    s
    The method is carried out as follows.
    Example 1. In a brass reactor | a, with a diameter of 50 mm and a usable capacity of 500 cm, completely filled with 300 g of cesium fluoride, used as a catalyst {) a „drain coke, used as a floor, is dried at 250 ° For 4 hours, the nitrogen flow is transferred and sieved in a drying cabinet to obtain a powder with an equivalent of 250 µm, 00 µm, continuously flowing a gaseous mixture of hydrogen fluoride syngole-O, purified from hydrogen fluoride, water and a system or secondary alcohol, which can:) by hydrolysis of the original carbonyl compound, in molar co-ratio, is 3.75: 1: 1, with a total volumetric flow rate of 23 nl / h C6 10: mol / 1 g of catalyst for each reactant) and an absolute pressure of 110 kPa. The temperature inside the reactor is controlled by external cooling.
    The gaseous mixture continuously exiting the reactor is subjected to spectrophotometric, infrared and spectrometric analyzes for
    | nitrogen N: CFjCE ,, C {0) F 1 molar ratio of Zs75: 1 at a 00% conversion and a yield of perfluoro toxy fluoride | ; After 400 hours of operation, the degree of Yonversion of the reactants and the yield remained unshakable. The time of impacting the reactants in the reactor is 1, 5 minutes,
    After increasing the temperature inside the reactor to + 20 ° C or absolute pressure up to 500 kPa at a temperature of –0 ° C pressure of 110 kPa, the degree of conversion of 1 "AI and output remained unchanged at 100%. Retention time in the reactor in the first case 1 , 3 m; in, in the second - 6.8 min.
    Example 2. In the reactor described in example 1, the following gas-purified N: P mixture is continuously fed as in 1 in a molar ratio of 1: 1: 1 at a total volumetric flow rate of 12 nl / h (6 10 mol / h k; a 1 g of catalyst for peatant) and an absolute pressure of 110 kPa. The temperature inside the reactor is kept at + 20 ° C by
    ten
    15 0 5
    0
    five
    0

    .
    0
    thermostatically controlled bath. Retention time 2.6 min
    The gaseous mixture leaving the reactor is subjected to infrared, spectrophotometric and iodometric analyzes in order to prove the presence of nitrogen N,:, (CO) F in a molar ratio of P 1 pr and 100% conversion and yield.
    Even after several weeks of work, no changes were found in the steps of conversion and output. Example 3 Into the reactor described in example f, the gaseous mixture N: F; CC1F COF in a molar ratio of 3.75: 1: 1 was continuously purified as in example 1 at a total volumetric flow rate of 23 nl / h (6 to 10 mol / h per 1 g of catalyst for each reactant) and an absolute pressure of 11 O kPa. Retention time 1.3 min.
    Inside the reactor can withstand a temperature of 4-20 ° C. The gaseous mixture, coming out of the reactor, is subjected to infrared, spectrophotometric and iodometric analyzes to prove nitrogen and CC1F – CF, OF in a molar ratio of 3j75: 1 at 1001 conversion and yield of 2-chloro-tetrafluoroethoxy-fluoride. After a few weeks, the output and conversion rate of ocTasajmcb are constant.
    Example 4OB AIS1-316 type reactor with a diameter of 25 mm and a working capacity of 500 cm, completely filled with 4 mm5 Raschig copper bars. peremetanny with 300 g of cesium fluoride, treated as in precher 1, continuously serves a gaseous mixture. o4mueHHSTO k-ak in U in a molar ratio of 30; 2; 1 at a total volumetric flow rate of 16.5 nl / h. (7.4 10-ol / h CF, COF per 1 g of catalyst and 14.9 10 mol / h of fluorine per 1 g of catalyst) and absolute pressure t 10 kPa, Ud-hp 1.3 min.
    The temperature inside the reactor is maintained at 135 ° C using a thermostatic bath. The effluent gases are subjected to infrared, spectrophotometric and iodometric anapicam to prove the content of nitrogen and, CF.jC (0) F, with full conversion to.
    Example 5 In the reactor described in Example 4, continuously pour.
    gaseous mixture consisting of CjClFyfr rCF COF, purified as in example 1, at a molar ratio of 1: 1: 1 and a total volumetric flow rate of 45 nl / h (2.2--10 mol / h per .1 g of catalyst for each reactant) and absolute pressure
    Example 9. It is operated as in β-example 7 by feeding a mixture of nitrogen, fluorine, CF5-CF-CF2, -0-CF (CF,) - COF, clean 10
    110 kPa. In the reactor, withstand the puppy as indicated above. A temperature of 20 ° C is obtained by external cooling. The outgoing gas mixture is subjected to infrared, spectrophotometric and iodometric analyzes in order to prove the content is en: in a molar-cm, the corresponding is completely filled with copper wire ratio of 1: 1, at 100% conversion and output of pentafluoroethoxyfluoride . Hold time 0.7 min.
    Example 6. A gaseous mixture, purified as indicated above, COCl, in a molar ratio of 3.75: 1.5: 1 at a total volumetric flow rate of 25 nl / h (9-- 10 mol / hr of fluorine per 1 g of catalysis, torus and 6. Yu mol / h per 1 g of catalyst) and absolute pressure of .110 kPa. A temperature of 30 ° C is maintained inside the reactor with external cooling. The retention time is 1.2 minutes. :
    The outgoing gaseous mixture is subjected to infrared, spectrophotometric, iodometric ana-a. The method of obtaining the fluoro-oxohalo compounds allows to increase the yield of the target products and the conversion of the starting compound to 100%. Besides.
    CF, -CF -CF2-0-CF (CF,), the degree of conversion and the yield being 100% each. Retention time 1.3 minutes Example 10. To a reactor with a diameter of 25 mm with a usable capacity of 100 cm
    The diameter of 0.3 mm and length of 20 mm mixed with 10 g of CSF, obtained as in example 1, is continuously supplied with a mixture prepared as described in example 1, at a molar ratio of 1: 1: 1 flow rate 45 nl / h (6.7 (10 mol / h per 1 g of catalyst for each reagent) and absolute
    25 pressure 110 kPa. The temperature inside the reactor is maintained with a thermostatic bath. Retention time 0.1 min.
    The gas mixture leaving the reactor consisted of CF, CF, OF at a molar ratio of 1: 1, at 100%
    conversion and output in CF, GF, j, OF.
    Chloride lysam and titration to prove the presence of .N.2: CF3CFj, COF:: Clj in a molar ratio of 7.5: 2: 1 at 100% -HbDC conversion and pentafluoroethoxy-fluoride yield.
    And p im 7. In the reactor of Example 1, a 40 gaseous mixture, purified as above, NjiFj: (CFj) 2 CO is continuously supplied at a molar ratio of 3.75: 1: 1 and a total flow rate of 23 nl / h (6 Yu / h per 1 g of catalyst for each reactant) and an absolute pressure of 110 kPa. Inside the reactor the temperature is maintained by external cooling. Retention time 1.3 min.50
    The output gas mixture is given by,. infrared, spectrophotometry-. This method consists of (CF,) -CF-O-F at a molar cm ratio of 3.75: 1 and a 100% conversion of 55 and an output.
    Example 8. Act as in example 7, feeding a gaseous mixture of nitrogen, fluorine and purified
    The improvement of the technological process is that of replacing the periodic mode of the process with a continuous one.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method of obtaining fluoroxyhalo compounds of the general formula
    (R), C (F) OF,
    where R is alkyl having 1 or 2. Lactual atom, completely. halogenated with fluorine or fluorine and chlorine cm, or R is a perfluorinated alkoxy dial, having 5 carbon atoms; 1 or 2, an integer} 3-n ,. integer
    by reacting in the presence of a fluorine fluorination catalyst and an organic compound of the formula
     P
    m
    as indicated above. CF.-CFj-CFj-OF is obtained, the degree of conversion and the yield being 100% each. Hold time 1.3 min.
    Example 9: Act as in γ-example 7, feeding a mixture of nitrogen, fluorine, CF5-CF-CF2, -0-CF (CF,) -COF, purified as indicated above. Get
    schenna as indicated above. Get
    completely filled with copper wire
    CF, -CF -CF2-0-CF (CF,), the degree of conversion and the yield being 100% each. Retention time 1.3 minutes, Example 10. Into a reactor with a diameter of 25 mm with a usable capacity of 100 cm
     15 fully filled copper wire
    The diameter of 0.3 mm and length of 20 mm mixed with 10 g of CSF, obtained as in example 1, is continuously supplied with a mixture prepared as described in example 1, at a molar ratio of 1: 1: 1 flow rate 45 nl / h (6.7 (10 mol / h per 1 g of catalyst for each reagent) and absolute
    25 pressure 110 kPa. The temperature inside the reactor is maintained with a thermostatic bath. Retention time 0.1 min.
    The gas mixture leaving the reactor consisted of CF, CF, OF at a molar ratio of 1: 1, at 100%
    The method of obtaining fluoroxygal
    conversion and output in CF, GF, j, OF.
    The improvement of the technological process is that of replacing the periodic mode of the process with a continuous one.
    Invention Formula
    The method of obtaining fluoroxyhalo compounds of the general formula
    (R), C (F) OF,
    where R is alkyl having 1 or 2. Lactual atom, completely. halogenated with fluorine or fluorine and chlorine cm, or R is a perfluorinated alkoxy dial, having 5 carbon atoms; 1 or 2, an integer} 3-n ,. integer
    by reacting in the presence of a fluorine fluorination catalyst and an organic compound of the formula
     P
    m
    .7U701768
    (R) C (X) 0 current of the reagent (R) C (X) ,, 0,7,4-10-h m-1- 6,7-10 MOL / H per 1 g of catalyst,
    with continuous feed reacting
     L:. the value of .5- "-l. at the removal of products% l and h and yushchi and so. what, a hundred reactions so. so that the retention time of the increase in the selectivity of the pro- and reactant substances in the reactor
     Gyvyhoda. the interaction was 0.1-6.8 minutes. at tap
    St, l ".t in gazvoy phase at avsotnom-Gat GeGerGturgG
    a pressure of 110–500 kPa, a temperature of 10-use as kacheg-10–135, providing the fluorine fluorination of fluoride .1 compounds in a gaseous and copper filler,
    state at volume velocity
    类似技术:
    公开号 | 公开日 | 专利标题
    SU1470176A3|1989-03-30|Method of producing fluoroxyhalocompounds
    US4724269A|1988-02-09|Process for producing p-chlorobenzenes
    RU2166498C2|2001-05-10|Method of preparing sulfur pentafluorides
    JP4520712B2|2010-08-11|Method for producing fluorohalogen ethers
    EP1553072B1|2009-03-11|Method for producing chlorinated hydrocarbon having chlorinated tertiary carbon
    EP0433611B1|1994-01-26|Process for producing alpha-hydroxyisobutyric acid amide
    EP0384261B1|1993-05-19|Process for the preparation of fluorooxy-fluorosulfonyl compounds by direct fluorination of fluoro-beta-sultones
    US5259938A|1993-11-09|Process for omega-halo-perfluoro acid chlorides
    KR20020068517A|2002-08-27|Crystals of penicillin and process for the production thereof
    US20040146453A1|2004-07-29|Process for the synthesis of BrSF5
    EP0023014B1|1982-12-01|Process for preparing hexafluoropropene oxide
    US6750371B2|2004-06-15|Process for the oxidation of alcohols to aldehydes and ketones in the presence of nitroxyl compounds as catalysts
    US4098832A|1978-07-04|Fluorination process catalysed by molybdenum pentachloride
    US5432290A|1995-07-11|Process for the preparation of 2,2-difluoro-1,3-benzodioxole
    US4183873A|1980-01-15|Liquid phase fluorination process
    US3963751A|1976-06-15|Chlorination of butadiene sulfone to 3,3,4,4-tetrachlorotetrahydrothiophene-1,1-dioxide
    AU602162B2|1990-10-04|Process for the preparation of perhalohydrocarbon hypochlorites
    JPH0723332B2|1995-03-15|Process for producing 1,3-dichloro-2-propanol
    WO2010099922A1|2010-09-10|Chemical process for the production of haloalkenone ethers
    US5629460A|1997-05-13|Process for the preparation of 1,1,1,3,3,3-hexafluoro-2-propanone
    EP0854128B1|2001-07-25|Process for the preparation of chloro-benzoyl chlorides
    EP0421322A1|1991-04-10|Process for preparing penta-fluorodichloropropanes
    US4046812A|1977-09-06|Process for preparing 1,1-dimethyl hydrazine
    US5648570A|1997-07-15|Process for preparing substituted chloroaromatics
    CA1233485A|1988-03-01|Process for the production of methallyl chloride
    同族专利:
    公开号 | 公开日
    EP0194862A3|1989-01-11|
    AU594326B2|1990-03-08|
    IL78104D0|1986-07-31|
    EP0194862B1|1991-09-11|
    JPH0657679B2|1994-08-03|
    IT1184149B|1987-10-22|
    CA1271778A|1990-07-17|
    AU5461586A|1986-10-16|
    IT8519847D0|1985-03-11|
    AT67176T|1991-09-15|
    JPS61257949A|1986-11-15|
    IL78104A|1990-11-05|
    UA7050A1|1995-03-31|
    US4827024A|1989-05-02|
    KR930001326B1|1993-02-26|
    ZA861809B|1986-10-29|
    DE3681309D1|1991-10-17|
    KR860007187A|1986-10-08|
    EP0194862A2|1986-09-17|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2689254A|1954-09-14|Process of preparing the compound |
    US3442927A|1964-02-03|1969-05-06|Minnesota Mining & Mfg|Fluoroxy compounds|
    NL8200023A|1981-01-30|1982-08-16|Lummus Co|METHOD FOR PREPARING TERT. ALKYL HYPOHALOGENITIES.|IT1197474B|1986-09-08|1988-11-30|Ausimont Spa|BROMOFLUROETYLIPOFLUORITE AND PROCEDURE FOR ITS PREPARATION|
    IT1197476B|1986-09-10|1988-11-30|Ausimont Spa|HYPOFLUORITES AND BIS-HYPOFLUORITES AND PROCEDURE FOR THEIR PREPARATION|
    IT1213536B|1986-11-14|1989-12-20|Ausimont Spa|2-BROMO, 1 ', 2', - DICHLORO-PERFLUORO DIETYL-ETHER AND PROCEDURE FOR LASUA PREPARATION.|
    IT1264662B1|1993-07-05|1996-10-04|Ausimont Spa|PERFLURODIOSSOLS THEIR HOMOPOLYMERS AND COPOLYMERS AND THEIR USE FOR THE COATING OF ELECTRIC CABLES|
    IT1272863B|1995-01-04|1997-07-01|Ausimont Spa|THERMOPROCESSABLE COPOLYMERS OF TETRAFLUOROETHYLENE|
    IT1272861B|1995-01-04|1997-07-01|Ausimont Spa|COPOLYMERS OF ETHYLENE WITH TETRAFLUOROETHYLENE AND / OR CHLOROTRIFLUOROETHYLENE, WITH IMPROVED MECHANICAL PROPERTIES AT HIGH TEMPERATURES|
    IT1275568B|1995-07-19|1997-08-07|Ausimont Spa|PROCESS FOR THE PREPARATION OF FLUOROSSI- OR CHLOROSSI- PERFLUOROACILFLUORURI|
    US6596128B2|2001-02-14|2003-07-22|Sun Coke Company|Coke oven flue gas sharing|
    ITMI20020198A1|2002-02-05|2003-08-05|Ausimont Spa| haloethers|
    ITMI20021782A1|2002-08-06|2004-02-07|Ausimont S P A Ora Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI.|
    ITMI20030019A1|2003-01-09|2004-07-10|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF SINGLE COMPOUNDS|
    ITMI20030018A1|2003-01-09|2004-07-10|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF SINGLE COMPOUNDS|
    ITMI20030150A1|2003-01-30|2004-07-31|Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI.|
    ITMI20030444A1|2003-03-11|2004-09-12|Solvay Solexis Spa|PROCESS TO PREPAREFLUOROALOGENOETERI.|
    ITMI20040132A1|2004-01-29|2004-04-29|Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI|
    ITMI20040133A1|2004-01-29|2004-04-29|Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI|
    ITMI20052456A1|2005-12-22|2007-06-23|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF FLUOROALOGENOETERI|
    ITMI20052455A1|2005-12-22|2007-06-23|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF FLUOROALOGENOETERI|
    US7247759B1|2006-01-04|2007-07-24|Honeywell International Inc.|Fluorination reactor|
    US9023554B2|2009-12-11|2015-05-05|Shandong Huaxia Shenzhou New Material Co., Ltd.|Perfluorinated ion exchange resin, preparation method and use thereof|
    EP2514773B1|2009-12-15|2014-12-03|Shandong Huaxia Shenzhou New Material Co., Ltd.|High exchange capacity perfluorinated ion exchange resin, preparation method and use thereof|
    WO2019110710A1|2017-12-06|2019-06-13|Solvay Specialty Polymers Italy S.P.A.|Process for preparing fluorohalogenoethers|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    IT19847/85A|IT1184149B|1985-03-11|1985-03-11|PROCESS FOR THE PREPARATION OF FLUOROSSI-ALO-COMPOSTI|
    [返回顶部]