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A kind of preparation method of dimethyl sulfone

A technology of dimethyl sulfone and dimethyl sulfoxide, which is applied in the field of preparation of dimethyl sulfone, can solve the problems of flying temperature, affecting reaction efficiency, shutdown, etc., and achieves extended service life, high conversion rate, and avoidance of flying temperature. Effect

Active Publication Date: 2018-03-20
CHINA PETROLEUM & CHEM CORP +1
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  • Description
  • Claims
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Problems solved by technology

[0006] Using titanium-silicon molecular sieves as a catalyst, when dimethyl sulfoxide is oxidized to prepare dimethyl sulfone, it can be carried out in a fixed-bed reactor, but when the contact reaction is carried out in a fixed-bed reactor, a catalyst bed is likely to appear during the reaction process The local temperature in the layer is too high, and the problem of overheating occurs, which not only affects the reaction efficiency, but also shortens the regeneration cycle of the catalyst; in addition, when the catalyst is deactivated and then regenerated, it generally needs to be shut down

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  • A kind of preparation method of dimethyl sulfone
  • A kind of preparation method of dimethyl sulfone

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preparation example Construction

[0010] The invention provides a method for preparing dimethyl sulfone, the method comprising: under oxidation reaction conditions, using dimethyl sulfoxide and at least one oxidizing agent and at least one titanium-silicon molecular sieve as a catalyst in the reaction zone of the reactor During the contact process, the titanium-silicon molecular sieve moves in the reaction zone along the axial direction of the reactor.

[0011] According to the method of the present invention, during the contact process, the titanium-silicon molecular sieve as the catalyst moves in the reaction zone along the axial direction of the reactor (ie, the reaction zone), which can effectively avoid fixing the catalyst bed. When in the reactor, it is prone to the problem of excessive local temperature in the catalyst bed during the reaction. In the present invention, the "reaction zone" refers to a zone for bringing dimethyl sulfoxide into contact with an oxidizing agent and a catalyst to carry out an...

Embodiment 1

[0055] Dimethyl sulfoxide, oxidant, methanol as a solvent, and a shaped hollow titanium-silicon molecular sieve as a catalyst (the average particle diameter is 1.2 μm, based on the total amount of the shaped hollow titanium-silicon molecular sieve, the content of the hollow titanium-silicon molecular sieve is 80 % by weight, the content of silicon oxide as a binder is 20% by weight) respectively and continuously sent into the moving bed reactor for contact reaction. Wherein, dimethyl sulfoxide is sent from the lower feed port of the reactor, and the mixture of oxidant and solvent and the catalyst are sent into the reactor from the liquid phase feed port and the solid phase feed port at the top of the reactor respectively. . Wherein, the oxidizing agent is 27.5% by weight of hydrogen peroxide, the molar ratio of dimethyl sulfoxide to the oxidizing agent in terms of hydrogen peroxide is 1:1.5, the mass ratio of dimethyl sulfoxide to methanol as a solvent is 1:5, two The mass ra...

Embodiment 2

[0058] Adopt the same method as Example 1 to prepare dimethyl sulfone, the difference is that the same amount of shaped titanium-silicon molecular sieve TS-1 (average particle size is 1.2 μm, based on the total amount of shaped titanium-silicon molecular sieve TS-1 , the content of titanium-silicon molecular sieve TS-1 is 80% by weight, and the content of silicon oxide as a binder is 20% by weight) instead of forming hollow titanium-silicon molecular sieve.

[0059] The reaction mixture obtained at 0.5h and 100h after the start of the reaction was analyzed by gas chromatography, and the conversion rate of dimethyl sulfoxide, the effective utilization rate of the oxidant and the selectivity of dimethyl sulfone were calculated. The results are listed in Table 1.

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Abstract

The invention discloses a method for preparing dimethyl sulfone. The method comprises: under oxidation reaction conditions, combining dimethyl sulfoxide and at least one oxidizing agent with at least one titanium-silicon molecular sieve as a catalyst in the reaction zone of the reactor During the contact process, the titanium-silicon molecular sieve moves in the reaction zone along the axial direction of the reactor. The method according to the present invention can effectively avoid problems such as catalyst bed overheating that may occur in a fixed-bed reactor, not only can obtain high dimethyl sulfoxide conversion rate, oxidant effective utilization rate and dimethyl sulfone selectivity, but also The service life of the catalyst can be extended; at the same time, the titanium-silicon molecular sieve whose activity cannot meet the requirements can be removed from the reaction system for regeneration without stopping the device.

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