Thioether oxidation method

A technology for oxidizing sulfide and sulfide, applied in chemical instruments and methods, preparation of organic compounds, chemical recovery, etc., can solve the problem of high cost of anodization, achieve stable oxidant conversion rate, prolong single-pass service life, and reduce regeneration. The effect of frequency

Active Publication Date: 2016-03-09
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0007] Dimethyl sulfoxide can also be produced from dimethyl sulfide by anodic oxidation, but the cost of anodic oxidation is higher

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 4、9-16 and 19

[0091] Following examples 4, 9-16 and 19 adopt the following method to measure the activity of catalyst:

[0092] 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,

[0093] 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

[0096] The catalyst (i.e. 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 0.79 g / 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.

[0097] Dimethyl sulfide, hydrogen peroxide (provided in the form of 30% by weight hydrogen peroxide) as an oxidizing agent and acetone as a solvent were mixed and fed into a fixed bed reactor and flowed through the catalyst bed. Among them, the molar ratio of dimethyl sulfide to hydrogen peroxide is 1:0.5, the initial molar ratio of dimethyl sulfide to acetone is 1:5, and the initial weight hourly space velocity of solvent acetone is 15h -1 . The temperature in the catalyst bed was 40° C., and the pressure in the...

Embodiment 2

[0103] Adopt the method identical with embodiment 1 to oxidize dimethyl sulfide, difference is, also send into the ammoniacal liquor (concentration is 25% by weight) in the fixed-bed reactor, to form by dimethyl sulfide, hydrogen peroxide and acetone The pH of the liquid mixture was adjusted to 7.0. When the reaction reaches 640 hours, the weight hourly space velocity of acetone is 27.2h -1 . The results obtained for 0.5 hours and 640 hours of reaction are listed in Table 1.

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Abstract

The present invention discloses a thioether oxidation method, which comprises: continuously conveying a liquid mixture into a fixed-bed reactor to make the liquid mixture contact a titanium silicon molecular sieve loaded in the fixed-bed reactor under an oxidation reaction condition, wherein the liquid mixture contains thioether, at least an oxidizing agent and at least a solvent, and the method further comprises that: when the oxidizing agent conversion rate or the target oxidation product selectivity is reduced to a certain degree, the weight hourly space velocity of the solvent is improved until the oxidizing agent conversion rate and / or the target oxidation product selectivity meets the requirement. With the method of the present invention, the one way service life of the titanium silicon molecular sieve adopted as the catalyst can be effectively prolonged, the regeneration frequency of the catalyst can be reduced, the production efficiency can be improved, the operation stability can be improved, and the total service life of the catalyst can be prolonged.

Description

technical field [0001] The present invention relates to a method for oxidizing thioethers. Background technique [0002] Sulfoxides are important sulfur-containing compounds. For example, dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound. It is a colorless and transparent liquid at room temperature. properties such as protons. Dimethyl sulfoxide is soluble in water, ethanol, acetone, ether and chloroform, is a highly polar inert solvent, and is widely used as a solvent and reaction reagent. Moreover, dimethyl sulfoxide has a high selective extraction ability and can be used as an extraction solvent for the separation of alkanes and aromatics. For example: dimethyl sulfoxide can be used for the extraction of aromatics or butadiene. In the polymerization reaction, it is used as a processing solvent and spinning solvent, as a synthetic solvent and spinning solvent of polyurethane, and as a synthetic solvent of polyamide, fluorochloroaniline, polyimide and poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/04C07C317/14C07C315/02
CPCY02P20/584
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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