A kind of dimethyl sulfide oxidation method
A technology of dimethyl sulfide and oxidant, applied in chemical instruments and methods, chemical recycling, organic chemistry, etc., can solve the problem of high cost of anodizing method, prolong the stable operation period, the method is simple and easy, and reduce the operation cost Effect
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[0029] In a preferred embodiment of the present invention, the preparation method of the shaped titanium-silicon molecular sieve comprises: under hydrolysis reaction conditions, at least one organosilicon compound capable of hydrolysis reaction and at least one water-soluble alkali and water Contacting, mixing the contacted mixture with titanium-silicon molecular sieves, and successively molding and roasting the obtained mixture containing titanium-silicon molecular sieves. The shaped catalyst obtained according to this embodiment not only has higher strength and thus is more resistant to wear and crushing, the bed containing the catalyst has a higher resistance to collapse; and can obtain higher The conversion rate of dimethyl sulfide and the selectivity of the target oxidation product.
[0030] In this preferred embodiment, the amount of the organosilicon compound, the water-soluble base and the titanium-silicon molecular sieve should be used to form the titanium-silicon mol...
Embodiment 6、12 and 13
[0093] Following examples 6, 12 and 13 adopt the following method to measure the activity of catalyst:
[0094] Catalyst, 36% by weight of ammonia water (as NH 3 meter), 30% by weight of hydrogen peroxide (as H 2 o 2 ), tert-butanol and cyclohexanone by mass ratio = 1:7.5:10:7.5:10 and then stirred and reacted at 80°C under atmospheric pressure for 2h, filtered the reactant, and analyzed the obtained liquid phase by gas chromatography The composition of the catalyst is analyzed, and the conversion rate of cyclohexanone is calculated by the following formula and used as the activity of the catalyst,
[0095] The conversion rate (%) of cyclohexanone=[(the molar amount of cyclohexanone added−the molar amount of unreacted cyclohexanone) / the molar amount of cyclohexanone added]×100%.
Embodiment 1
[0098] (1) Mix titanium-silicon molecular sieve TS-1 with silica sol (silicon dioxide content is 30% by weight) and water, wherein, the mass ratio of titanium-silicon molecular sieve TS-1, silica sol and water in terms of silicon dioxide It is 1:0.2:1.5. The obtained mixture was granulated by rolling balls, and the obtained wet granules were calcined at 550° C. for 5 hours to obtain a shaped titanium-silicon molecular sieve with an average particle size of 200 μm, wherein the content of the titanium-silicon molecular sieve was 83% by weight.
[0099] (2) The catalyst prepared in step (1) is packed in two fixed-bed reactors connected in series to form a catalyst bed, wherein the number of catalyst beds in each reactor is 1 layer.
[0100] Dimethyl sulfide, hydrogen peroxide and methanol are combined to form a liquid mixture. Ammonia water (concentration: 25% by weight) was added to the liquid mixture to adjust the pH value of the liquid mixture from 5.1 to 6.5. Then, the liqu...
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