Activated carbon-based solid acid catalyst and preparation method thereof
A solid acid catalyst, activated carbon technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of weak acidity, small reaction specific surface, high cost, easy production and thermal stability. Good, high mechanical strength effect
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Embodiment 1
[0021] Add 2.0 g of activated carbon into the three-necked flask, reflux reaction with 25 ml of 7 mol / L nitric acid for 8 h; wash with distilled water until neutral, and dry in an oven at 110°C for 12 h to obtain carboxylated activated carbon; in the three-necked flask Add 5.5 g of 4-aminoisophthalic acid into a beaker, add 100 ml of 3mol / L HCl, and heat and stir. The above solution was cooled to room temperature, and 12wt% NaNO was added 2 Solution 18ml, use starch-KI test paper to control the reaction end point, stir and react at 0-5°C for 30min to obtain the diazonium isophthalic acid salt; then add the above-mentioned activated carbon rich in carboxyl groups and react at 58°C for 80min, filter, and use Reflux washing with distilled water for 12 h, ethanol back washing for 12 h, and drying in a drying oven at 110°C for 24 h.
[0022] Catalytic effect: Add 0.1 mol of acetic acid, 1 mol of absolute ethanol, and 0.3 g of activated carbon-based solid acid catalyst into a round...
Embodiment 2
[0024] 2.0 g of activated carbon was added to the three-necked flask, and 25 ml of 7 mol / L nitric acid was refluxed for 8 h. Wash with distilled water until neutral and dry in an oven at 120°C for 10 hours to obtain carboxyl-rich activated carbon. Put 7.28g of 5-aminoisophthalic acid into a beaker in a three-necked flask, add 100ml of 3mol / L HCl to it, and heat and stir. The above solution was cooled to room temperature, and 12% NaNO was added 2 The solution was 24 ml, and the end point of the reaction was controlled by starch-KI test paper, and the reaction was stirred at 0-5°C for 30 minutes to obtain the diazonium phthalate. Then add the above carboxyl-rich activated carbon and react at 60°C for 60 minutes, filter, wash with distilled water for 12 hours at reflux, ethanol for 16 hours at reflux, and dry in a drying oven at 110°C for 12 hours.
[0025] Catalytic effect: Add 0.1 mol of acetic acid, 1 mol of anhydrous n-butanol, and 0.3 g of activated carbon-based solid acid...
Embodiment 3
[0027] 1.0 g of activated carbon was added to the three-necked flask, and 15 ml of 7 mol / L nitric acid was refluxed for 8 h. Wash with distilled water until neutral and dry in an oven at 130°C for 8 hours to obtain carboxyl-rich activated carbon. Add 4.7 g of 5-amino-1,2,3-benzenetricarboxylic acid in a three-necked flask to a beaker, then add 50 ml of 3mol / L HCl to dissolve, heat and stir. The above solution was cooled to room temperature, and 12% NaNO was added 2 The solution was 22 ml, and the end point of the reaction was controlled with starch-KI test paper, and the reaction was stirred at 0-5°C for 30 minutes to obtain the diazonium salt of isophthalic acid. Then add the above carboxyl-rich activated carbon and react at 60°C for 90 minutes, filter, wash with distilled water for 12 hours and ethanol for 16 hours, and dry at 110°C for 12 hours.
[0028] Catalytic effect: Add 0.1mol of acetic acid, 1mol of anhydrous n-butanol, and 0.3g of activated carbon-based solid acid...
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