A method for preparing 2,5-dimethoxy-4-chloroaniline
A technology of dimethoxyl and chloroaniline, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of harsh use conditions of liquid reducing agents, affecting product yield and purity, and difficult separation. , to achieve good industrial application prospects, easy separation and high conversion rate
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[0014] According to the method for preparing 2,5-dimethoxy-4-chloroaniline of the present invention, the hydrogen-containing gas can be hydrogen-containing gas or other hydrogen-containing gases, and for the present invention, preferably the hydrogen-containing gas is hydrogen.
[0015] According to the method for preparing 2,5-dimethoxy-4-chloroaniline of the present invention, preferably, the nickel-based amorphous alloy catalyst is an amorphous Ni-Al-M catalyst, and M is other metal elements. In this way, the conversion rate of 2,5-dimethoxy-4-chloro-nitrobenzene and the selectivity of 2,5-dimethoxy-4-chloroaniline can be further improved.
[0016] According to the method for preparing 2,5-dimethoxy-4-chloroaniline of the present invention, preferably based on the total weight of the catalyst, the weight ratio between Ni, Al and M is 1-200:0.5-30:1, Preferably it is 5-60:1-10:1.
[0017] According to the method for preparing 2,5-dimethoxy-4-chloroaniline of the present in...
preparation Embodiment 1
[0048] Add 1.5kg of nickel and 1.5kg of aluminum into a graphite crucible, heat it in a high-frequency furnace until it melts, and then spray the molten liquid from the nozzle of the crucible onto a copper roller with a rotation speed of 600 rpm. Cooling water is passed through, the alloy liquid is rapidly cooled at a cooling rate of 1000°C / s, and then thrown out along the tangent of the copper roll to form scale-like strips, which are ground to a particle diameter of less than 70 microns to obtain a master alloy. Slowly add 50 g of the master alloy into a three-neck flask filled with 500 g of 20 wt % sodium hydroxide aqueous solution, control its temperature at 80° C. and keep stirring at constant temperature for 1 hour. After stopping heating and stirring, filter off the liquid and wash with distilled water at 100°C until the pH value is 10;
[0049] Add 20.0g of the above-prepared Ni-Al alloy to 30mL titanium tetrachloride aqueous solution with a concentration of 20% (weigh...
preparation Embodiment 2
[0051] Add 1.5kg of nickel and 1.5kg of aluminum into a graphite crucible, heat it in a high-frequency furnace until it melts, and then spray the melt from the nozzle of the crucible onto a copper roller with a rotational speed of 1000 rpm. Cooling water is passed through, the alloy liquid is rapidly cooled at a cooling rate of 1000°C / s, and then thrown out along the tangent of the copper roll to form scale-like strips, which are ground to a particle diameter of less than 70 microns to obtain a master alloy. Slowly add 50 g of the master alloy into a three-neck flask filled with 500 g of 20 wt % sodium hydroxide aqueous solution, control its temperature at 80° C. and keep stirring at constant temperature for 1 hour. After stopping heating and stirring, filter off the liquid and wash with distilled water at 100°C until the pH value is 10;
[0052] At 50°C, add 25mL of titanium tetrachloride with a concentration of 20% (weight) to the 20.0g Ni-Al alloy prepared above and stir in...
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