Preparation and application of composite solid acid catalyst used for condensation reaction
A composite solid acid and condensation reaction technology, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, physical/chemical process catalysts, etc., can solve the problems of poor reaction selectivity and achieve high activity, good reusability, and acid content big effect
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Embodiment 1
[0018] A method for preparing a composite solid acid catalyst using silica gel as a carrier, the steps are as follows:
[0019] 1) Add 20g of inert carrier silica gel dried at a temperature of 80-200°C in advance to the container connected with the air guide tube and the constant pressure dropping funnel, slowly add 8mL of chlorosulfonic acid from the dropping funnel, and keep stirring or vibrating Mix and mix, and then continue to stir for 30 minutes to obtain a mixed material;
[0020] 2) Add the above mixture into 50mL methanol solution containing 25mmol zinc chloride in a three-necked flask, soak for 1h, dry at 80°C for 1h, and then roast at 350°C for 3h to obtain a composite solid acid catalyst.
[0021] The application of the composite acid solid catalyst:
[0022] 1) Used in quinazoline condensation reaction
[0023] Add 0.5g of o-aminobenzonitrile into 2mL of anhydrous cyclohexanone, add 1g of the above-mentioned catalyst under stirring, raise the temperature to sli...
Embodiment 2
[0034] A kind of preparation method that adopts aluminum oxide as the composite solid acid catalyst of carrier, the steps are as follows:
[0035] 1) Add 20g of inert carrier alumina that has been dried at 80-200°C in advance in a container connected with an air duct and a constant pressure dropping funnel, slowly add 6mL of chlorosulfonic acid from the dropping funnel, and keep stirring or Shake and mix well, then continue to stir for 40 minutes to obtain the mixed material;
[0036] 2) Add the above mixture into 50mL methanol solution containing 20mmol aluminum chloride in a three-necked flask, soak for 1h, dry at 100°C for 2h, and then roast at 400°C for 3h to obtain a composite solid acid catalyst.
[0037] The application of the composite acid solid catalyst:
[0038] Add 4mL (44mmol) of n-butanol, 3.0mL (52mmol) of acetic acid, and 0.7g of the above solid catalyst into the three-necked flask, stir and mix evenly, heat the oil bath to 120°C, and react at constant temper...
Embodiment 3
[0044] A method for preparing a composite solid acid catalyst using titanium oxide as a carrier, the steps are as follows:
[0045]1) Add 25g of titanium oxide, an inert carrier dried at 80-200°C, to a container connected with an air duct and a constant pressure dropping funnel, and slowly add 8mL of chlorosulfonic acid from the dropping funnel, stirring or Shake and mix well, then continue to stir for 30 minutes to obtain the mixed material;
[0046] 2) Add the above mixture into 30mL dichloromethane solution containing 18mmol ferric chloride in a three-necked flask, soak for 1h, dry at 100°C for 2h, and then roast at 450°C for 3h to get Composite solid acid catalyst.
[0047] The application of the composite acid solid catalyst:
[0048] Add 4mL (44mmol) of n-butanol, 5.5g (45mmol) of benzoic acid, and 0.7g of the above solid catalyst into the three-necked flask, stir and mix evenly, heat the oil bath to 130°C, and react at a constant temperature for 2.5h; then cool with a...
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