Special catalyst for preparing m-phthalonitrile through ammoxidation reaction as well as preparation method and application thereof
A technology of isophthalonitrile and ammoxidation, which is applied in the field of organic chemistry and organic fine chemicals, and can solve the problems of weak force of metal oxides, changes, and easy falling off of metal oxides.
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Embodiment 1
[0024] 25.03 g H 2 C 2 o 4 2H 2 Dissolve O in 150 mL of distilled water at 80°C, add 12.05 g of V 2 o 5 , 28.06 g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 50.43 g (NH 4 ) 3 Sb(C 2 o 4 ) 3 2H 2 O, 2.46 g H 3 BO 3 and 0.49 g Li 2 CO 3 After forming a uniform solution, slowly add 150 mL of 30% silica sol, and then add 10 g of aminopropyltrimethoxysilane. After stirring evenly, the catalyst precursor was obtained by high-speed spray centrifugal drying, dried in a muffle furnace at 110° C., and then gradually raised to 550° C. for 6 hours. After natural cooling, set aside. The active composition of the catalyst is: VMo 1.2 Sb 0.8 B 0.3 Li 0.1 o 7.8 .
[0025] 20g of the above-mentioned solid catalysts are filled in a quartz tube fixed-bed reactor with an internal diameter of 30mm, and the molar ratio of the reaction raw materials is: m-xylene:NH 3 :Air=1:5:35, the reaction temperature is 693±1K, and the catalyst load is 100g / (kgcat·h). After reacting for 8 hours, the...
Embodiment 2~7
[0027] Catalyst formula is different, and reaction condition is with embodiment 1, and result is as follows:
[0028]
Embodiment 8
[0030] 47.81 g H 2 C 2 o 4 2H 2 O was dissolved in 200 mL of distilled water at 85 °C, and then 23.02 g of V 2 o 5 , 35.73 g (NH 4 ) 6 Mo 7 o 24 4H 2 O, 21.80 g Mn(NO 3 ) 2 ·6H 2 O and 50.67 g KSbC 4 h 4 o 7 .1 / 2H 2 O, after forming a homogeneous solution, slowly add the aminopropyl cage polysilsesquioxane ((i-C) of 100 grams of 30% content 4 h 9 ) 7 Si 8 o 12 (CH 2 CH 2 CH 2 NH 2 )) in solution. After uniform stirring, the catalyst precursor was obtained by high-speed spray and centrifugal drying, and the temperature was gradually raised to 500° C. in a high-temperature furnace and kept for 12 hours. After cooling naturally, save for later use. The composition of the catalyst is: VMo 0.8 Sb 0.6 mn 0.3 K 0.6 o 6.7 .
[0031] 20g of catalyst is loaded into a fixed-bed reactor with a quartz tube with an inner diameter of 30mm, and the mixed gas of raw materials passes through the catalyst bed for reaction. The composition of the raw gas mixture i...
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