• 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:
    A highly active cathode, having utility for electrolytic reduction of 2,3,5,6-tetrachloropyridine to 2,3,5-trichloropyridine, comprises a wet, immobilized layer of aggregated silver microcrystals, formed by the electrolytic reduction of colloidal, silver oxide particles in the presence of water and hydroxyl ions.
    公开号:SU925254A3
    申请号:SU802909297
    申请日:1980-04-11
    公开日:1982-04-30
    发明作者:Кириакоу Деметриос
    申请人:Дзе Дау Кемикал Компани (Инофирма)；
    IPC主号:
    专利说明:

    () METHOD FOR PRODUCING 2,3,5-TRICHLORPYRIDINE
    one
    The invention relates to the electrosynthesis of organic compounds and can be used to obtain 2,3,5-trichloropyridine from 2,3. 5,6-tetrachloropyridine.jj
    A known method for producing 2, trichlopyridine, including the electrochemical reduction of 2,., Tetrachloropyridine in the presence of an organic solvent. The IQ process is carried out in a salt solution in an organic solvent; mercury, lead and some other metals are used as cathodes 1.
    The product yield is very small - only 15 a small amount of tetrachloropyridine is reduced f. obtaining unidentified trichloropyridine.
    The purpose of the invention is to increase the yield of the product.
    The goal is achieved by the fact that in the method of obtaining 2,3,5 trichloropyridine, including the electrochemical reduction of 2,3.5,6-25
    tetrachloropyridine on a metal cathode in the presence of an organic solvent before electrochemical reduction, the metal cathode is polarized at a potential of from -0.5 to -2.0 V relative to the normal calomel electrode in the presence of colloidal particles of silver oxide, water and hydroxyl ions.
    The increase in product yield is achieved mainly due to the fact that the outer layer of the cathode is covered with freshly precipitated silver microcrystals and at the same time maintained in a wet state. Colloidal silver oxide particles are conveniently prepared by anodic dissolution of silver and subsequently used as a cathode.
    Example. A catholyte is prepared. For this purpose, in a 100 ml solution of tetrahydrofuran in water 1: 1, 1Og of pentachloropyridine and 15 g of sodium acetate, ri (a source of hydroxyl ion ions) are mixed. In the catholyte is immersed in a lory ceramic bowl, into which anolyte is poured 50 ml of a 25% aqueous solution of NaOH in water. Anolyte is placed in a catholyte anolyte with a silver grid of cylindrical shape. A normal calomel comparison electrode is applied to the cathode. Set the temperature to 20-30 ° C. The catholyte is stirred with a magnetic stirrer until an emulsion is formed. An electric current is connected and a cathode potential of -1.5 V relative to the reference electrode is established. A solution of silver nitrate in water is added to the catholyte to form colloidal particles of silver oxide. Within 30 seconds, due to the activation of the cathode, the current increases in order to keep it constant (1 And the potential of the cathode is reduced to 1, 1 V.
    Periodic analysis of catholyte samples is performed using gas chromatography and IR spectroscopy. The results of the analyzes are shown in the table.
    The resulting product is extracted from catholyte in three portions of 20 ml of dichloromethane and the combined extracts are washed with water and evaporated, while taking precautions in order to avoid the loss of trichloroprivodic as a result of sublimation. The resulting residue is a mixture of crystalline solids and a small amount of oil. Total weight 9.5 g
    The 2,3,5 Trichloropyridine component of the crystalline phase is separated by sublimation, and the remaining 2,3,5,6-tetrachloropyridine is purified by recrystallization or used as a starting material to obtain an additional amount of trichloro derivative.
    Similar results are obtained when using graphite, stainless steel, platinum as an anode,
    nickel, and as the liquid component of the catholyte, water, benzene, and isopropanol (or glycol ether) in a volume ratio of 5.5: 2.5: 5.0.
    EXAMPLE 2 A cathode was prepared, for which a wet precipitate of silver oxide was applied to a stainless steel sieve with a working surface of 5x7.5 cm. Immerse the sieve (cathode) in a NaOH solution and cathode polarized at a potential of 1–, 5 V 15 min, with the current decreasing from j to 0.5 A.
    The electrolysis was carried out under the conditions of example 1 for 20 hours and similar results were obtained.
    The results show that the proposed method allows to increase the yield of the product in comparison with the known.
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    The method of obtaining 2,3,5-trichloropyridine, including electrochemical 5 92525 6
    The recovery of 2,3,5,6-tetrachloro-2.0 V relative to normal calapiridine on a metal cathode of a welcome electrode in the presence of organic solvent, soluble particles of silver oxide, body water, and hydroxyl ions. that, in order to increase the output of the product s Information sources, the one before the electrochemical metal cathode field -1, which was taken into account during the examination, was restored. U.S. Patent No., run at a potential of -0.5 doc, published. 1972 (prototype).
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    同族专利:
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    AR223704A1|1981-09-15|
    IN153664B|1984-08-04|
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    IL59482D0|1980-05-30|
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    AU527014B2|1983-02-10|
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    DE3064869D1|1983-10-27|
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    引用文献:
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    US3130136A|1961-05-10|1964-04-21|Hercules Powder Co Ltd|Electrolytic method for the preparation of gem-dinitrocompounds|
    US3449162A|1965-09-17|1969-06-10|Analytic Systems Co|Method of making oxygen measuring cells|
    DE1546728C3|1965-09-18|1975-07-17|Varta Batterie Ag, 3000 Hannover|Process for the production of a powdery powder containing silver! Catalyst for oxygen electrodes|
    DE1567689A1|1965-10-09|1970-06-11|Barthel Dipl Chem Guenter|Electrode for the electrolytic decomposition of hydrochloric acid and process for its manufacture|
    US3657003A|1970-02-02|1972-04-18|Western Electric Co|Method of rendering a non-wettable surface wettable|
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    DE2508853C3|1975-02-28|1980-06-26|Siemens Ag, 1000 Berlin Und 8000 Muenchen|Process for the production of thin silver cathodes for electrochemical cells|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    US06/029,600|US4242183A|1979-04-13|1979-04-13|Highly active silver cathode, preparation of same and use to make 2,3,5-trichloropyridine|
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