Titanium-silicon-aluminum molecular sieve, its preparation method and application, and a method for cyclic ketone oxidation
A molecular sieve and titano-silicate-alumina technology, which is applied in the direction of molecular sieves and alkali exchange compounds, molecular sieve catalysts, oxidative preparation of carboxylic acids, etc., can solve the problems of occupying land resources and storage space, and achieve good catalytic effects
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[0026] Therefore, as previously mentioned, the present invention provides a method for preparing the titano-silicon-aluminum molecular sieve of the present invention, the method comprising:
[0027] (1) Mix the unloading agent with the acid solution for beating, carry out the first heat treatment to the obtained slurry, and separate and obtain the first solid, wherein the unloading agent is the unloading agent of the reaction device using titanium silicon molecular sieve as the catalyst active component. Dispensing;
[0028] (2) The second heat treatment is performed after mixing the first solid, the aluminum source, the titanium source and the alkali source in the presence of an aqueous solvent.
[0029]In the present invention, the unloading agent of the reaction device using titanium-silicon molecular sieve as the catalyst active component can be the unloading agent from various devices that use titanium-silicon molecular sieve as the catalyst active component, for example,...
Embodiment 1
[0108] This example illustrates the methods and products provided by the invention.
[0109] At normal temperature (20°C, the rest of the comparative examples are the same as the examples) and normal pressure (0.1MPa, the rest of the comparative examples are the same as the examples), the deactivated cyclohexanone oximation catalyst SH-2 and 1mol / L hydrochloric acid The aqueous solution was mixed and beaten, and then the mixed slurry was mixed and stirred at 80°C for 12 hours; after solid-liquid separation, the solid, aluminum source aluminum sulfate, titanium source titanium sulfate and sodium hydroxide aqueous solution (pH 12) were mixed and the mixture was put into Stainless steel sealed reaction kettle, treated at 170°C for 12 hours, wherein, the mass composition of the material is deactivated cyclohexanone oximation catalyst: titanium source: aluminum source: acid: alkali: water = 100: 1: 1: 10: 5: 250, deactivated cyclohexanone oximation catalyst with SiO 2 In terms of ...
Embodiment 2
[0114] This example illustrates the methods and products provided by the invention.
[0115] At normal temperature and pressure, first mix the deactivated cyclohexanone oximation catalyst SH-3 with 5mol / L hydrochloric acid solution for beating, then mix and stir the mixed slurry at 60°C for 1 hour; after solid-liquid separation, separate the solid, Aluminum source aluminum sol (content is 20% by weight), titanium source tetrabutyl titanate and tetrapropyl ammonium hydroxide aqueous solution (pH is 10) are mixed, and the mixed solution is put into a stainless steel sealed reaction kettle, and treated at 150°C for 12h , wherein the quality of the material is composed of deactivated cyclohexanone oximation catalyst: titanium source: aluminum source: acid: alkali: water=100:2:0.5:15:15:200, and the deactivated cyclohexanone oximation catalyst is SiO 2 In terms of acid, H + In terms of alkali in OH - count. Then the product was recovered according to the method of Example 1 to ...
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Abstract
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