Catalyst for liquid phase hydrogenation of chloronitrobenzene and preparation method thereof
A technology of nitrobenzene liquid and catalyst, which is applied in the direction of catalyst activation/preparation, preparation of amino compounds, chemical instruments and methods, etc. It can solve the problems of increased catalyst consumption, backward production process of chlorinated aromatic amines, and increased secondary pollution, etc. , to achieve the effect of simple preparation method, conducive to large-scale production, and reduce catalyst cost
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Embodiment 1
[0020] Embodiment 1: take nickel sulfate hexahydrate 1g and add 50ml deionized water to be mixed with nickel sulfate solution, add 5ml ammoniacal liquor in the solution, stir 1 hour; Under ultrasonic action, 0.4g sodium borohydride is added into 10ml deionized water; The sodium borohydride solution was added dropwise to the nickel-containing solution at room temperature, the reaction proceeded immediately and hydrogen gas was released, after the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.
[0021] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 70°C, pressure 1.0MPa, using a 100ml reactor, adding 0.4g black precipitate NiB as catalyst and 1.0g chlorobenzene, 40ml of absolute ethanol, the rotation speed is 700rpm, and the reaction time is 1 hour; the final result is tha...
Embodiment 2
[0022] Embodiment 2: take nickel chloride 1g and add 50ml deionized water to be mixed with nickel nickel chloride solution, add 10ml ammoniacal liquor in the solution, stir 1 hour; 0.6g potassium borohydride is joined in 10ml deionized water; Potassium borohydride solution was added dropwise to the nickel-containing solution, the reaction proceeded immediately and hydrogen gas was emitted. After the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.
[0023] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 75°C, pressure 0.9MPa, using a 200ml reactor, adding 0.8g black precipitate NiB as catalyst and 2.0g chlorobenzene, 80ml of absolute ethanol, the rotating speed is 800rpm, and the reaction time is 1.5 hours; the final result shows that the conversion rate of the catalyst chl...
Embodiment 3
[0024] Embodiment 3: take nickel nitrate hexahydrate 1g and add 50ml deionized water to be mixed with nickel nitrate solution, add 10ml ammoniacal liquor in the solution, stir 1 hour; 0.4g sodium borohydride is joined in 10ml deionized water; The sodium hydride solution was added dropwise to the nickel-containing solution, and the reaction proceeded immediately and hydrogen gas was emitted. After the dropwise addition, when no hydrogen gas was released, it was washed with deionized water, and then the obtained black solid was stored in absolute ethanol.
[0025] The prepared catalyst was used in the liquid-phase hydrodechlorination reaction of chlorobenzene, the reaction conditions were: reaction temperature 80°C, pressure 1.2MPa, using a 500ml reactor, adding 2.0g black precipitate NiB as catalyst and 5.0g chlorobenzene, 200ml of absolute ethanol, the rotation speed is 900rpm, and the reaction time is 2 hours; the final result is that the conversion rate of chloronitrobenzene ...
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