A method of producing dimethyl sulfoxide
A technology of dimethyl sulfoxide and dimethyl sulfide, used in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of unsuitable large-scale production and high cost of anodization, and achieve high selectivity. the effect of oxidant and oxidant availability
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Embodiment 9-12、16 and 17
[0089] Following examples 9-12, 16 and 17 adopt the following method to measure the activity of catalyst:
[0090] 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,
[0091] 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
[0094] Catalyst (that is, shaped titanium-silicon molecular sieve TS-1 is a spherical catalyst with a volume average particle diameter of 500 μm, the content of titanium-silicon molecular sieve TS-1 in the catalyst is 80% by weight, the content of silicon oxide is 20% by weight, and the density is 0.78g / 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.
[0095] Dimethyl sulfide, hydrogen peroxide (provided as 30% by weight hydrogen peroxide) as an oxidant, and methanol as a solvent were mixed to form a liquid feed that was fed from the bottom into a fixed-bed reactor and flowed over the catalyst The bed layer is in contact with the titanium silicon molecular sieve to react. Among them, the molar ratio of dimethyl sulfide to hydrogen peroxide is 2:1, and the molar ratio of dimethyl sulfide to methanol is 1:10. The temperature in the reactor is 40°C, the pressure in...
Embodiment 2
[0102] Adopt the method identical with embodiment 1 to produce dimethyl sulfoxide, difference is, also send into ammoniacal liquor (concentration is 25% by weight) in the fixed-bed reactor, to form by dimethyl sulfide, hydrogen peroxide and methanol The pH of the liquid feed was adjusted from 6.2 to 7.0.
[0103] The experimental results are listed in Table 1.
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