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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

Active Publication Date: 2017-03-01
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 dimethyl sulfide oxidation method
  • A kind of dimethyl sulfide oxidation method
  • A kind of dimethyl sulfide oxidation method

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preparation example Construction

[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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Abstract

The invention discloses a dimethyl sulfide oxidation method. The method comprises causing a liquid mixture to pass through a catalyst bed layer filled with at least one titanium silicalite molecular sieve under the conditions of oxidation reaction, wherein the liquid mixture contains dimethyl sulfide and at least one oxidizing agent. The method comprises switching the flow direction of the liquid mixture in the catalyst bed layer when the catalytic activity of the titanium silicalite molecular sieve in the catalyst bed layer is lower than an expected value, wherein with the flowing direction of the liquid mixture in the catalyst bed layer prior to the switching as the standard, the liquid mixture performs reverse flowing in the catalyst bed layer after the switching. According to the method, even if long-time continuous running is performed, the activity of the catalyst can be maintained within a high range, so that the stable running time of a device is effectively prolonged, and the running cost of the device is reduced. In addition, the method is simple, convenient, practical and favorable for industrial production and application.

Description

technical field [0001] The invention relates to a dimethyl sulfide oxidation method. Background technique [0002] Dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound. It is a colorless and transparent liquid at room temperature. It has the characteristics of high polarity, high hygroscopicity, flammability, and high boiling point aprotic. 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, polyimid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/04C07C315/02
CPCY02P20/584
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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