Titanium tin molecular sieve and its preparation method and method for catalytic oxidation of cyclohexanone
A molecular sieve and cyclohexanone technology, applied in the direction of molecular sieve catalyst, molecular sieve and base exchange compound, carboxylate preparation, etc., can solve the problem of reducing the diffusion rate of the precursor, affecting the nucleation of molecular sieve, reducing the alkalinity of the crystallization system, and pre-curing Body gel and other problems to achieve the effect of improved performance and high selectivity
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[0029] The present invention also provides a preparation method of titanium tin molecular sieve, comprising the following steps:
[0030] (1) In the presence of an aqueous solvent, mix and dissolve titanium source, polyvinylpyrrolidone, and urea in proportion to obtain a mixture, then add silicon source, mineralizer, structure-directing agent and alkali source to the mixture in proportion, and mix well , to obtain a mixed system;
[0031] (2) add tin source in the mixed system of step (1), obtain each material molar ratio to be SiO 2 : Sn: Ti: mineralizer: structure directing agent: water = 1: (0.002~0.015): (0.001~0.15): (0.3~3): (0.8~5.0): (10~300) reaction mixture, Adjust the pH of the solution to 9.5 to 13.6;
[0032] (3) Transfer the reaction mixture in step (2) into a reaction kettle, conduct crystallization reaction at 70-160° C. for 0.2-14 days, cool to room temperature, then wash, dry and roast to obtain titanium tin molecular sieve.
[0033] According to the prese...
Embodiment 1
[0057] Dissolve tetrabutyl titanate, polyvinylpyrrolidone, and urea in a mixed solution of ethanol and water at a molar ratio of 1:10:0.98, wherein the volume ratio of water and ethanol is 1:2 to obtain a mixed system, and then add to the mixed system Add methyl orthosilicate, sodium fluoride, tetraethylammonium hydroxide and ammonia water, and mix well;
[0058] Add tin nitrate in above-mentioned mixed system, obtain each material molar ratio is SiO 2 :Sn:Ti:mineralizer:structure directing agent:H 2 O=1:0.008:0.005:1:1.1:80 reaction mixture, adding sodium carbonate to adjust the pH value of the solution is 12.8;
[0059] Transfer the reaction mixture into a reaction kettle, conduct crystallization reaction at 100°C for 5 days, cool to room temperature, wash and dry the product to obtain a crystallized product;
[0060] The crystallized product was calcined at 450° C. for 6 hours to obtain titanium tin molecular sieves.
[0061] In the titanium-tin molecular sieve prepared ...
Embodiment 2
[0065] Dissolve tetraethyl titanate, polyvinylpyrrolidone, and urea in a mixed solution of ethanol and water with a molar ratio of 1:6:1.95, where the volume ratio of water and ethanol is 1:3, and then add it to the mixed system in proportion Ethyl orthosilicate, potassium sulfide, tetraethylammonium fluoride and sodium carbonate, mix well;
[0066] Add tin protosulfate in above-mentioned mixed system, obtain each material molar ratio to be SiO 2 :Sn:Ti:mineralizer:structure directing agent:H 2 O=1:0.005:0.05:0.5:2.2:100 reaction mixture, adding sodium carbonate to adjust the pH value of the solution is 10.5;
[0067] Transfer the reaction mixture into a reaction kettle, conduct crystallization reaction at 120°C for 3 days, cool to room temperature, wash and dry the product to obtain a crystallized product;
[0068] The crystallized product was calcined at 400°C for 5 hours to obtain titanium tin molecular sieves.
[0069] The titanium-tin molecular sieve prepared according...
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