A kind of method that salicylamide continuous method prepares salicylonitrile
A technology of salicylamide and salicylonitrile, which is applied in the field of preparation of nitrile compounds, can solve the problems of low yield, increase the complexity of equipment, and increase the difficulty of separation and purification process, so as to simplify the separation process, improve selectivity and yield efficiency and reduce reaction energy consumption
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Embodiment 1
[0032] The metal-doped supported boron phosphate catalyst comprises the following steps:
[0033] Add 20g of boric acid, 37.3g of phosphoric acid, 0.54g of telluric acid dihydrate, 1.2g of stearic acid and 140mL of water into the reactor in sequence, heat and stir evenly. Then 77.8 g of acidic silica sol with a silica content of 25% was added to the system. Heating and evaporating to dryness under stirring conditions until gelatinous, shaped after drying, and then calcined at 400° C. for 5 hours to obtain catalyst 1. The loading of boron phosphate is 67.3%, the content of tellurium is 0.5%, and the addition of stearic acid is 2%, to obtain the target catalyst.
[0034] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:
[0035] Fill 10mL of Catalyst 1 in the fixed bed reactor, pass N 2 Preheat to 370°C. Preheat the benzonitrile solution of salicylamide with a concentration of 0.1g / mL ...
Embodiment 2
[0037] The metal-doped supported boron phosphate catalyst comprises the following steps:
[0038] Add 5g of boric acid, 9.3g of phosphoric acid, 0.18g of telluric acid dihydrate, 1.0g of hydroxymethylcellulose and 50mL of water into the reactor in sequence, heat and stir evenly. Then add 442.9g of ammonia type alkaline silica sol with silica content of 40% to the system. Heating and evaporating to dryness under stirring conditions until it was gelatinous, dried and shaped, and then calcined at 400° C. for 4 hours to obtain catalyst 2. The loading of boron phosphate is 5%, the content of tellurium is 0.1%, and the addition of stearic acid is 0.5%.
[0039] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:
[0040] Fill 10mL catalyst 2 in the fixed-bed reactor, pass N 2 Preheat to 480°C. Preheat the benzonitrile solution of salicylamide with a concentration of 0.1g / mL and ammonia gas t...
Embodiment 3
[0042] The metal-doped supported boron phosphate catalyst comprises the following steps:
[0043] 20g of boric acid, 37.3g of phosphoric acid, 17.0g of aluminum nitrate nonahydrate, 1.3g of stearic acid and 140mL of water were successively added into the reactor, heated and stirred evenly. Then add 9.7g 3A molecular sieves to the system. Heating and evaporating to dryness under stirring conditions until gelatinous, shaped after drying, and then calcined at 300°C for 4 hours to obtain catalyst 3. The boron phosphate loading was 80%, the aluminum content was 5%, and the carboxymethyl cellulose addition was 5%.
[0044] Adopt above-mentioned catalyzer, prepare the method for salicylonitrile with salicylamide continuous method, operation steps are as follows:
[0045] Fill 10mL catalyst 3 in the fixed-bed reactor, pass through N 2 Preheat to 340°C. Preheat the p-xylene solution of salicylamide with a concentration of 1.1g / mL and ammonia gas to 150°C, and then pass it into the ...
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