Titanium silicon molecular sieve, preparation method and application thereof and phenol hydroxylation method
A titanium-silicon molecular sieve and molecular sieve technology, applied in the field of molecular sieves, can solve the problems of occupying land resources and storage space, and achieve good catalytic effects
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[0028] The present invention also provides a preparation method of a titanium-silicon molecular sieve, the method comprising:
[0029] (1) Mix the catalyst containing titanium-silicon molecular sieve with the first heat treatment liquid, then perform the first heat treatment, and then separate to obtain the first solid, the first heat treatment liquid is an acid solution with a concentration>0.1mol / L, and the first heat treatment liquid is an acid solution with a concentration>0.1mol / L. 1. The temperature of heat treatment is 10-200°C, preferably, the time is 0.5-36h;
[0030] (2) Mix the first solid with the second treatment liquid, and then perform the second heat treatment, the second treatment liquid contains titanium source, silicon source, alkali source and water, the temperature of the second heat treatment is 100- 200°C, preferably, the time is 6-96h;
[0031] Among them, SiO 2 In other words, the molar ratio of the catalyst containing titanium-silicon molecular sieve ...
Embodiment approach
[0050] According to a preferred embodiment of the present invention, the maintenance time of the preferred stage (1) is 2-24 hours, preferably 4-16 hours; the maintenance time of the stage (2) is 0.1-12 hours, preferably 2-6 hours ; The maintenance time of stage (3) is 4-24 hours, preferably 4-12 hours.
[0051] According to the method provided by the present invention, preferably, with SiO 2 In other words, the molar ratio of the catalyst containing titanium-silicon molecular sieve in step (1) to the silicon source in step (2) is 100:(1-15), more preferably 100:(4-10). Adopting the preferred embodiment of the present invention is more conducive to adjusting the micropore size distribution of the prepared titanium-silicon molecular sieve, and enables the prepared titanium-silicon molecular sieve to be used in the phenol hydroxylation reaction process to obtain a more stable catalytic effect.
[0052] According to the method of the present invention, preferably, the method of ...
Embodiment 1
[0102] This example illustrates the methods and products provided by the invention.
[0103] 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-1 was mixed with 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, silicon-sourced ethyl orthosilicate, titanium-sourced 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 molar composition of the material is an inactivated cyclohexanone oximation catalyst: silicon source: titanium source: acid: alkali: water = 100:5:1:10 :5:250, deactivated cyclohexanone oximation catalyst wi...
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Abstract
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