sn-beta molecular sieve, its hydrothermal synthesis method and the method of phenol hydroxylation
A beta molecular sieve, hydrothermal synthesis technology, applied in molecular sieve catalysts, chemical instruments and methods, preparation of organic compounds, etc. Molecular sieve nucleation and other problems, to achieve the effect of small particle size, increase pore volume, and promote crystallization
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[0026] The present invention provides a kind of hydrothermal synthesis method of Sn-beta molecular sieve, comprises the following steps:
[0027] (1) In the presence of an aqueous solvent, mix the silicon source, tin source, structure-directing agent, foaming agent and the first part of the alkali source in proportion to obtain a mixed system, then add a mineralizer to the mixed system, and add the second Part of the alkali source adjusts the pH value of the mixed system to 9.8-13 to obtain a reaction mixture, and the molar ratio of each substance in the reaction mixture is SiO 2 : Sn: mineralizer: structure directing agent: blowing agent: H 2 O=1: (0.01-0.07): (0.01-3.6): (0.5-4.2): (0.05-0.2): (5-500);
[0028] (2) Carry out crystallization reaction to the reaction mixture of step (1), obtain crystallization product;
[0029] (3) acidifying the crystallized product and roasting in the air to obtain the Sn-β molecular sieve.
[0030] The Sn-β molecular sieves prepared in t...
Embodiment 1
[0059] Under stirring conditions, ethyl orthosilicate, sodium stannate, diethylamine, potassium chloride, 4-aminobiphenyl and hydrazine hydrate were mixed and dissolved in deionized water to obtain a molar ratio of SiO 2 : Sn: Structure directing agent: Foaming agent: H 2 O=1:0.05:1.5:0.14:100 reaction mixture (pH 8.9), then according to SiO 2 : Mineralizing agent=1:2.8 molar ratio is added potassium fluoride to the mixing system, then sodium hydroxide is added to the system to adjust the pH value of the system to 10.8, to obtain the Sn-β molecular sieve precursor colloid;
[0060] Transfer 46mL of the above colloid to a 60mL polytetrafluoroethylene reactor, raise the temperature to 160°C at a rate of 5°C / min, and react at a constant temperature under autogenous pressure for 8 days, then cool down to room temperature at a rate of 2°C / min to obtain crystallization product; the crystallized product was centrifuged and washed 3 times with deionized water;
[0061]Mix the washed...
Embodiment 2
[0064] Under stirring conditions, mix and dissolve ethyl orthosilicate, tin chloride, tetraethylammonium hydroxide, sodium fluoride, 1,1,1,2-tetrafluoroethane and alkali source in deionized water (alkali The source is a mixture of sodium bicarbonate and sodium carbonate mass ratio of 1:2), and the obtained molar ratio is SiO 2 : Sn: Structure directing agent: Foaming agent: H 2 O=1:0.06:0.65:0.06:300 reaction mixture (pH is 12.8), then according to SiO 2 : Mineralizing agent=1:1.6 molar ratio adds sodium chloride to the mixing system, then adds the above-mentioned alkali source to the system to adjust the pH value of the system to 12, and obtain the Sn-β molecular sieve precursor colloid;
[0065] Transfer 42mL of the above colloid to a 60mL polytetrafluoroethylene reactor, raise the temperature to 170°C at a rate of 5°C / min, react at a constant temperature under autogenous pressure for 8 days, and cool down to room temperature at a rate of 5°C / min to obtain crystallization ...
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