Sulfoether oxidation method
A sulfide oxidation and sulfide technology, which is applied in chemical instruments and methods, chemical recycling, organic chemistry, etc., can solve the problems of reducing the catalytic activity of titanium silicon molecular sieve, increasing the operating cost of the device, and fluctuating greatly in the activity of the catalyst. The effect of industrial production application, prolonging the service life of one-way, and prolonging the stable operation time
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Embodiment 4、12-15 and 17
[0085]Following examples 4, 12-15 and 17 adopt the following method to measure the activity of catalyst:
[0086] 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,
[0087] 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
[0090] The catalyst (being a spherical catalyst with a volume particle diameter of 500 μm, the content of titanium-silicon molecular sieve TS-1 in the catalyst is 85% by weight, the content of silicon oxide is 15% by weight, and the density is 0.79g / cm 3 ) is packed in a fixed-bed reactor to form a catalyst bed, wherein the number of the catalyst bed is 1 layer, and the aspect ratio of the catalyst bed is 10.
[0091] Dimethyl sulfide, hydrogen peroxide as an oxidizing agent (provided in the form of hydrogen peroxide, the initial concentration of hydrogen peroxide in hydrogen peroxide is 30% by weight) and acetone as a solvent are mixed to form a liquid mixture, and the liquid mixture is removed from the bottom into a fixed bed reactor and flow through the catalyst bed. Among them, the initial molar ratio of dimethyl sulfide to hydrogen peroxide is 4:1, the molar ratio of dimethyl sulfide to acetone is 1:15, and the weight hourly space velocity of dimethyl sulfide is 2h -1 . ...
Embodiment 2
[0097] Dimethyl sulfide was oxidized by the same method as in Example 1, except that aqueous ammonia (concentration: 25% by weight) was also fed into the fixed-bed reactor to adjust the pH of the liquid mixture to 7.5.
[0098] The reaction was carried out for 620 hours, and the concentration of hydrogen peroxide in the hydrogen peroxide was 55% by weight at the end of the reaction. The results obtained for 0.5 hours and 620 hours of reaction are listed in Table 1.
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