Method for oxidizing dimethyl sulfide

A technology for oxidizing dimethyl sulfide and dimethyl sulfide, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems that dimethyl sulfone application research has not yet been carried out well, and achieves Effects of high effective utilization rate of oxidant, ease of implementation, and high conversion rate of dimethyl sulfide

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In foreign countries, dimethyl sulfone is widely used as a nutritional product that is as important as vitamins. The research on the application of dimethyl sulfone in my country has not yet been carried out well. At present, the products are mainly used for export.

Method used

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  • Method for oxidizing dimethyl sulfide
  • Method for oxidizing dimethyl sulfide
  • Method for oxidizing dimethyl sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Send dimethyl sulfide, titanium-silicon molecular sieve TS-1 as catalyst, hydrogen peroxide as oxidant, methanol and hydrochloric acid (36% aqueous solution) as solvent into a small slurry bed reactor for oxidation reaction, the catalyst is separated from the reaction mixture output from the slurry bed reactor to obtain a liquid phase mixture containing dimethyl sulfone, and the separated catalyst is recycled. Among them, the molar ratio of dimethyl sulfide to oxidant is 1:2.5, the mass ratio of dimethyl sulfide to catalyst is 25:1, the mass ratio of solvent to catalyst is 200:1, and the amount of hydrochloric acid makes the The pH value of the mixture formed by the base sulfide, the oxidizing agent and the solvent is 3.5; the reaction temperature is 30° C., the pressure in the reactor is 0.5 MPa, and the total feed rate of the reaction materials is 50 mL / min.

[0052] The liquid phase mixture obtained when the reaction was carried out to 0.5 hour and 2 hours was analyz...

Embodiment 2

[0057] Dimethyl sulfide was oxidized by the same method as in Example 1, except that an equal amount of hollow titanium-silicon molecular sieve was used instead of titanium-silicon molecular sieve TS-1.

[0058] The liquid phase mixture obtained when the reaction was carried out to 0.5 hour and 2 hours was analyzed by gas chromatography, and the conversion rate of dimethyl sulfide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfone were calculated. The results obtained are shown in the table 1 listed.

[0059] Table 1

[0060]

[0061] Comparing Example 1 with Comparative Example 1, it can be seen that the method of the present invention can obtain higher conversion rate of dimethyl sulfide, effective utilization rate of oxidant and selectivity of dimethyl sulfone.

Embodiment 3

[0063] Send dimethyl sulfide, hollow titanium silicate molecular sieve as catalyst, hydrogen peroxide as oxidant, methanol and phosphoric acid as solvent (aqueous solution with a mass concentration of 36%) into a small slurry bed reactor for oxidation reaction, The catalyst is separated from the reaction mixture output from the slurry bed reactor to obtain a liquid phase mixture containing dimethyl sulfone, and the separated catalyst is recycled. Among them, the molar ratio of dimethyl sulfide to oxidant is 1:3, the mass ratio of dimethyl sulfide to catalyst is 10:1, the mass ratio of solvent to catalyst is 25:1, and the amount of phosphoric acid is such that the The pH value of the mixture formed by the base sulfide, the oxidizing agent and the solvent is 3.5; the reaction temperature is 90° C., the pressure in the reactor is 1.5 MPa, and the total feed rate of the reaction materials is 50 mL / min.

[0064] The liquid phase mixture obtained when the reaction was carried out to...

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Abstract

The invention provides a method for oxidizing dimethyl sulfide. The method comprises the step of contacting a liquid mixture with a least one titanium silicate molecular sieve serving as a catalyst under the condition of an oxidation reaction, wherein the liquid mixture contains dimethyl sulfide and at least one oxidant, and the pH value of the liquid mixture is 0.5-5.5. Compared with the method for directly contacting a liquid mixture of dimethyl sulfide and the oxidant with a titanium silicate molecular sieve, the method can be used for remarkably improving the selectivity of dimethyl sulfone and receiving high dimethyl sulfide conversion rate and high oxidant effective utilization rate. Furthermore, under a situation that other conditions are the same, a basically same dimethyl sulfide conversion rate, a higher oxidant effective utilization rate and dimethyl sulfone selectivity can be obtained by the method even at a lower temperature. Furthermore, the method is easy to implement.

Description

technical field [0001] The present invention relates to a method for oxidizing dimethyl sulfide, more particularly, the present invention relates to a method for oxidizing dimethyl sulfide to prepare dimethyl sulfone. Background technique [0002] Dimethyl sulfone is white crystalline powder, easily soluble in water, ethanol, benzene, methanol and acetone, slightly soluble in ether. Potassium permanganate cannot be discolored at room temperature, and strong oxidizing agents can oxidize dimethyl sulfone to methanesulfonic acid. Aqueous solution of dimethyl sulfone is neutral. At 25°C, there is a small amount of sublimation, and the sublimation speed is accelerated at 60°C, so the drying of dimethyl sulfone products should be carried out at low temperature and vacuum. [0003] Dimethyl sulfone is used in industry as a high-temperature solvent and raw material for organic synthesis, as a stationary liquid for gas chromatography, as a analytical reagent, as a food additive, an...

Claims

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Application Information

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