Preparation method and application of composite solid superacid catalyst
A solid superacid and catalyst technology, which is applied in the preparation of organic compounds, catalytic reactions, and carboxylate preparations, etc., can solve the problems of cumbersome catalyst preparation steps, and achieve the effects of easy recycling, wide application range, and obvious economic benefits
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Embodiment 1
[0036] Add the perfluorosulfonic acid resin with an exchange capacity of 1.05 to the alcohol-water solution, and mechanically stir at 250° C. for 5.0 h under high pressure and reflux, evaporate and concentrate to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.
[0037]Add 17.30 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.50 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 42.39 In the mixed solution of perfluorosulfonic acid resin solution and 46.63g 0.05mol / L NaOH solution, the solution gels quickly; cover the gel with aluminum foil and dry at 75°C for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain completely d...
Embodiment 2
[0041] Add the perfluorosulfonic acid resin with an exchange capacity of 1.10 to the alcohol-water solution, and mechanically stir at 250°C for 8.0 hours under high pressure and reflux, evaporate and concentrate to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.
[0042] Add 17.30 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.50 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 48.05 g perfluorosulfonic acid resin solution and 48.05g 0.05mol / L NaOH solution, the solution gels quickly; dry the gel at 75°C covered with aluminum foil for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain completely dried solid particles. ...
Embodiment 3
[0046] Add the perfluorosulfonic acid resin with an exchange capacity of 0.98 to the alcohol-water solution, and mechanically stir at 250° C. for 6.0 h under high pressure and reflux, evaporate and concentrate to obtain a perfluorosulfonic acid resin solution with a solid content of 5%.
[0047] Add 16.50 g of deionized water to 50.00 g of tetraethyl orthosilicate, add 12.00 g of 0.04 mol / L HCl solution while stirring, and keep stirring until the solution is clear; add the hydrolyzed tetraethyl orthosilicate solution to 48.05 g perfluorosulfonic acid resin solution and 52.86g 0.05mol / L NaOH solution in the mixed solution, the solution gels quickly; dry the gel at 75°C covered with aluminum foil for 2 days to remove liquid water; then remove the aluminum foil Paper was placed in a constant temperature drying oven at 95°C for 2 days to obtain solid particles; finally, the solid particles were placed in a vacuum oven at 140°C for 2 days to remove all water to obtain completely dri...
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