Tin-titanium-silicon molecular sieve, its preparation method and application, and a method for cyclic ketone oxidation
A technology of tin-titanium-silicon molecular sieve and cyclic ketone, which is applied in molecular sieve catalyst, oxidative preparation of carboxylic acid, chemical instruments and methods, etc., can solve the problems of occupying land resources and storage space, and achieve good catalytic effect.
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[0026] 因此,如前所述,本发明提供了一种本发明所述的锡钛硅分子筛的制备方法,该方法包括:
[0027] (1)将卸出剂与酸溶液混合打浆,将得到的浆液进行第一热处理,分离得到第一固体,其中,所述卸出剂为以钛硅分子筛作为催化剂活性组分的反应装置的卸出剂;
[0028] (2)将所述第一固体、锡源、钛源与碱源在含水溶剂存在下混合后进行第二热处理。
[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, it can be from The unloading agent unloaded from the oxidation reaction device with titanium silicon molecular sieve as the active component of the catalyst. The oxidation reaction can be various oxidation reactions, for example, the unloading agent of the reaction device using titanium silicon molecular sieve as the catalyst active component can be the unloading agent of the ammoximation reaction device, the unloading agent of the hydroxylation reaction device and one or more of the unloading agent of the epoxidation ...
Embodiment 1
[0105] This example illustrates the methods and products provided by the invention.
[0106] 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, tin source tin chloride pentahydrate, titanium source titanium sulfate and sodium hydroxide aqueous solution (pH 12) were mixed and mixed Put the liquid into a stainless steel sealed reaction kettle, and treat it at 170°C for 12 hours, wherein, the mass composition of the material is an inactivated cyclohexanone oximation catalyst: titanium source: tin source: acid: alkali: water = 100:1:2:10 :5:250, deactivated cyclohexanone oximation catalyst with SiO 2 In ter...
Embodiment 2
[0111] This example illustrates the methods and products provided by the invention.
[0112] 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, Tin source tin chloride pentahydrate, titanium source tetrabutyl titanate and tetrapropyl ammonium hydroxide aqueous solution (pH 10) are mixed, and the mixture is put into a stainless steel sealed reaction kettle, and treated at 150°C for 12 hours, the mass of the material Composed of deactivated cyclohexanone oximation catalyst: titanium source: tin source: acid: alkali: water = 100: 2: 3.5: 15: 15: 200, 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 obtain a tin-titanium-silicon molecular si...
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