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A kind of thioether oxidation method

A technology of thioether oxidation and thioether, which is applied in the fields of chemical instruments and methods, organic chemistry, chemical recovery, etc., can solve the problems of high cost of anodic oxidation, prolong the stable operation period, prolong the service life of a single pass, and reduce the regeneration frequency Effect

Active Publication Date: 2017-10-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of thioether oxidation method
  • A kind of thioether oxidation method
  • A kind of thioether oxidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11-14 and 16

[0093] Following examples 11-14 and 16 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] The catalyst (being 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 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.

[0099] Dimethyl sulfide, hydrogen peroxide (provided in the form of 30% by weight hydrogen peroxide) as an oxidizing agent and methanol as a solvent were mixed to form a liquid mixture which was fed from the bottom into a fixed bed reactor in parallel flow over the catalyst bed. Among them, in the liquid mixture, the molar ratio of dimethyl sulfide to hydrogen peroxide is 2:1, the molar ratio of dimethyl sulfide to methanol is 1:8, and the weight hourly space velocity of dimethyl sulfide is 2.5h -1 . The temperature in the catalyst bed was 40° C., and the pres...

Embodiment 2

[0103] The same method as in Example 1 is used to oxidize dimethyl sulfide, the difference is that ammonia (24% by weight) is also sent into the fixed-bed reactor, and the amount of ammonia added will be the pH of the liquid mixture in contact with the catalyst. Adjusted from 5.2 to 7.5.

[0104] During the 640 hours of reaction, the dimethyl sulfide feed was stopped 4 times. The results obtained for 0.5 hours and 640 hours of reaction are listed in Table 1.

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Abstract

The invention discloses a sulfoether oxidation method. The method comprises the steps that a liquid mixture is continuously fed into a fixed-bed reactor, and the liquid mixture flows through catalyst bed layers under the oxidation reaction condition to be reacted with titanium silicalite molecular sieves filled in the catalyst bed layers in a contacted mode, wherein the liquid mixture contains sulfoether, at least one oxidizing agent and at least one selectable solvent. The method further comprises the step that when the conversion rate of the oxidizing agent and / or the selectivity of a target oxidation product decreases to a certain degree, feeding of the sulfoether is stopped for a period of time, and then feeding of the sulfoether is restored again. By means of the sulfoether oxidation method, the conversion rate of the oxidizing agent and / or the selectivity of the target oxidation product can be maintained within a higher range for a long time, and the one-way service life of the titanium silicalite molecular sieves serving as a catalyst is effectively prolonged. In addition, the sulfoether oxidation method is simple and easy to carry out.

Description

technical field [0001] The present invention relates to a kind of sulfide oxidation method. 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 pol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/02C07C317/04B01J29/89
CPCY02P20/582
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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