Solid super acid and preparation method, glycerol cyclohexanone ketal and preparation method
A cyclohexanone ketal, solid super acid technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as poor catalytic activity of solid super acid catalysts
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[0022] An embodiment of the present invention provides a method for preparing a solid superacid catalyst, which comprises the following steps:
[0023] The zirconium hydroxide is immersed in 0.4mol / L-0.6mol / L ammonium persulfate aqueous solution, filtered to obtain a filter cake; the filter cake is dried and roasted to obtain a solid super acid catalyst, wherein the hydroxide The mass volume ratio of zirconium to the ammonium persulfate aqueous solution is (0.114-16.6): 1 g / mL.
[0024] Specifically, in the step of immersing zirconium hydroxide in a 0.4mol / L-0.6mol / L ammonium persulfate aqueous solution and filtering to obtain a filter cake, zirconium hydroxide is immersed in 0.4mol / L-0.6mol / L 12-36h of ammonium persulfate aqueous solution, suction filtration to obtain a filter cake. The advantage of suction filtration is to remove free water, so as to avoid the formation of vapor pressure of water during drying and roasting, which is unfavorable for catalyst preparation. Ad...
Embodiment 1
[0046] A kind of preparation method of solid super acid catalyst, it comprises the steps:
[0047] Weigh 24g of ZrOCl 2 ·8H 2 O is dissolved in 240 mL of distilled water to prepare ZrOCl with a mass fraction of 10% 2 Solution, in the state of uniform stirring, slowly add ammonia water, adjust the pH to 10, stop adding ammonia water, get white precipitate, let the above precipitate stand at room temperature for 24h, carry out suction filtration, and wash with deionized water until Until there was no chloride ion (no white precipitate was detected with 0.1 mol / L silver nitrate), it was dried in a blast drying oven at 120° C., taken out and ground to obtain zirconium hydroxide.
[0048] Immerse 6g of zirconium hydroxide in 100mL (NH4) of 0.5mol / L 2 S 2 O 8 The solution was left in the solution for 24 hours, and then it was suction filtered to obtain a filter cake, which was then dried at 100 °C for 12 hours, placed in a muffle furnace and calcined at a temperature of 600 °C ...
Embodiment 2
[0052] A preparation method of a solid superacid catalyst, the preparation method is generally the same as that of Example 1, except that 16g of zirconium hydroxide is immersed in 0.5mol / L (NH4) 2 S 2 O 8 50mL solution for 24h.
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