Dimethyl sulfone preparation method

A technology of dimethyl sulfone and dimethyl sulfoxide, which is applied in the field of preparation of dimethyl sulfone, can solve the problems that the application research of dimethyl sulfone has not been carried out well, and achieves high effective utilization rate of oxidant and mild reaction conditions. , easy-to-control effects

Active Publication Date: 2015-11-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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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

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preparation example Construction

[0010] The invention provides a method for preparing dimethyl sulfone, which comprises contacting dimethyl sulfoxide and at least one oxidizing agent with at least one titanium-silicon molecular sieve under oxidation reaction conditions, wherein at least part of the titanium Silicon molecular sieves are non-fresh titanium silicon molecular sieves.

[0011] According to the method of the present invention, at least part of the titanium-silicon molecular sieve is non-fresh titanium-silicon molecular sieve. Using fresh titanium-silicon molecular sieves in the initial stage of the reaction, and then in the continuous reaction process, the titanium-silicon molecular sieves are separated and recycled after optional regeneration. The titanium-silicon molecular sieves used in the initial stage of the method of the present invention are Non-fresh titanium silicate molecular sieve. That is, in the method of the present invention, at least part of the starting catalyst is non-fresh tita...

Embodiment 1

[0051] The titanium-silicon molecular sieve SH-1 used as a catalyst in this example is obtained by regenerating the titanium-silicon molecular sieve TS-1 unloaded from the ammoximation reaction process of cyclohexanone, wherein the regeneration condition is: at 550°C Under the air atmosphere roasting 4h. The activity of the titanium-silicon molecular sieve SH-1 is 50%, and the activity of the fresh titanium-silicon molecular sieve TS-1 is 95%.

[0052] Send DMSO, SH-1 as a catalyst, hydrogen peroxide as an oxidant and methanol as a solvent into a small slurry bed reactor for oxidation reaction, and separate from the reaction mixture output from the slurry bed reactor The catalyst is removed to obtain a liquid phase mixture containing dimethyl sulfone, and the separated catalyst is recycled. Among them, the molar ratio of dimethyl sulfoxide to oxidant is 1:0.5, the mass ratio of dimethyl sulfoxide to catalyst is 25:1, the mass ratio of methanol to dimethyl sulfoxide is 100:1, an...

Embodiment 2

[0062] Adopt the method identical with embodiment 1 to prepare dimethyl sulfone, difference is:

[0063] The catalyst used is titanium-silicon molecular sieve SH-2, which is obtained by regenerating the hollow titanium-silicon molecular sieve unloaded from the ammoximation reaction process of cyclohexanone. The regeneration condition is: roasting in air atmosphere at 550°C 4h. The activity of the titanium-silicon molecular sieve SH-2 is 47%, and the activity of the fresh hollow titanium-silicon molecular sieve is 96%.

[0064] The obtained liquid phase mixture containing dimethyl sulfone is analyzed by gas chromatography, and the conversion rate of dimethyl sulfoxide, the effective utilization rate of oxidant and the selectivity of dimethyl sulfone are calculated, wherein the reaction is carried out to 0.5 hour and The liquid phase mixtures obtained at 80 hours were analyzed separately, and the results obtained are listed in Table 1.

[0065] Table 1

[0066]

[0067] Th...

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Abstract

The invention discloses a dimethyl sulfone preparation method. The dimethyl sulfone preparation method comprises causing dimethyl sulfoxide and at least one oxidizing agent to be in contact with at least one titanium silicate molecular sieve under the conditions of oxidation reaction, wherein the at least part of the titanium silicate molecular sieve is a non-fresh titanium silicate molecular sieve. Compared with a method of causing dimethyl sulfoxide to undergo contact reaction with the oxidizing agent in the absence of catalysts, the dimethyl sulfone preparation method can achieve the obviously improved dimethyl sulfoxide conversion rate, the effective utilization rate of the oxidizing agent and dimethyl sulfone selectivity. Compared with a method of causing dimethyl sulfoxide and the oxidizing agent to undergo contact reaction with a fresh titanium silicate molecular sieve, the dimethyl sulfone preparation method can achieve a higher effective utilization rate of the oxidizing agent, and in the long-cycle continuous reaction process, the conversion rate of dimethyl sulfoxide and the selectivity of dimethyl sulfone are more stable. In addition, the method is moderate in reaction conditions, easy to control and suitable for devices of various production scales.

Description

technical field [0001] The invention relates to a preparation method of 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, and as a drug. As an organic sulfide, dimethyl sulfone can enhance the ability of the human body to produce insulin, and at the s...

Claims

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Application Information

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