Preparation method for nitrobenzene catalytic hydrogenation catalyst
A technology for catalytic hydrogenation and catalyst, which is applied in the preparation of amino compounds, preparation of organic compounds, catalysts for physical/chemical processes, etc., and can solve problems such as poor thermal stability and reduced activity.
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Embodiment 1
[0017] (1) Add 5g of bentonite to 300mL of 0.1mol / L NiCl 2 In the aqueous solution, the mixture was vigorously stirred for 4 hours and then allowed to stand for 8 hours. This was repeated twice. After suction filtration, the sample was washed three times with deionized water. The filter cake was dried at 80 °C and ground to below 100 mesh to obtain m Ni / m 膨润土 Ni-intercalated bentonite of 0.002;
[0018] (2) 2g Ni intercalated bentonite and CH 3 COONa press n Ni / n CH3COONa =2 Dissolve in deionized water, press n under heating and stirring in a 30°C water bath p / n Ni =1 Add NaH 2 PO 2 ·H 2 O, 0.5mol / L NaOH solution adjusts the pH of the solution to 9, and reacts until the solution no longer produces bubbles. Through the electrostatic attraction between Ni and P, the intercalation of P is intercalated into the bentonite layer, and the product is subjected to suction filtration, and the filter cake Wash three times with ammonia water, deionized water, and absolute etha...
Embodiment 2
[0021] (1) 5g sodium bentonite was added to 300mL 0.5mol / L of NiCl 2 In aqueous solution; the mixture was vigorously stirred for 4h and then left to stand for 8h, repeated 6 times. After suction filtration, the sample was washed 10 times with deionized water, and the filter cake was dried at 120°C and ground to below 100 mesh to obtain m Ni / m 膨润土 Ni-intercalated bentonite of 0.084;
[0022] (2) 2g Ni intercalated bentonite and CH 3 COONa press n Ni / n CH3COONa =2 Dissolve in deionized water, press n under heating and stirring in a 90°C water bath p / n Ni =6 Add NaH 2 PO 2 ·H 2 O, 5mol / L NaOH solution to adjust the pH of the solution to 12, react until the solution no longer produces bubbles, through the electrostatic attraction between Ni and P, intercalate P into the bentonite layer, the product is suction filtered, and the filter cake is used Ammonia water, deionized water, and absolute ethanol were washed 6 times each, and sealed with alcohol for use.
[0023] Us...
Embodiment 3
[0025] (1) 5g sodium bentonite was added to 252mL 0.25mol / L of NiCl 2 In the aqueous solution, the mixture was vigorously stirred for 4 hours and then left to stand for 8 hours. This was repeated 4 times. After suction filtration, the sample was washed 6 times with deionized water. The filter cake was dried at 110°C and ground to below 100 mesh to obtain m Ni / m 膨润土 Ni-intercalated bentonite of 0.098;
[0026] (2) 2g Ni intercalated bentonite and CH 3 COONa press n Ni / n CH3COONa =2 Dissolve in deionized water, press n under heating and stirring in a water bath at 70°C p / n Ni =4 add NaH 2 PO 2 ·H 2 O, 2mol / L NaOH solution to adjust the pH of the solution to 11, react until the solution no longer produces bubbles, through the electrostatic attraction between Ni and P, the P intercalation is intercalated into the bentonite layer, the product is suction filtered, and the filter cake is used Ammonia water, deionized water, and absolute ethanol were washed 4 times each, a...
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