Method for simultaneously producing dimethyl sulfone and dimethyl sulfoxide

A technology of dimethyl sulfoxide and dimethyl sulfone, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problem of increasing the complexity of process operations, high cost of hydrogen peroxide, increasing operating costs, etc. problem, to achieve high selectivity, improve conversion rate, and reduce operating costs.

Active Publication Date: 2016-03-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Although dimethyl sulfone can be directly prepared by oxidizing dimethyl sulfide, when dimethyl sulfide is directly oxidized to prepare dimethyl sulfone, hydrogen peroxide is usually used as an oxidizing agent, and the amount and consumption of the oxidizing agent are generally It is higher than the stoichiometric ratio, but after the reaction is over, it is difficult to

Method used

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  • Method for simultaneously producing dimethyl sulfone and dimethyl sulfoxide
  • Method for simultaneously producing dimethyl sulfone and dimethyl sulfoxide
  • Method for simultaneously producing dimethyl sulfone and dimethyl sulfoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] (1) The first oxidation reaction step

[0091] The original powder of titanium silicon molecular sieve TS-1 as catalyst, the first part of dimethyl sulfide, methanol as solvent and hydrogen peroxide as oxidant (provided in the form of hydrogen peroxide with a concentration of 27.5% by weight) were mixed to form a slurry and react. Wherein, the molar ratio of the first part of dimethyl sulfide to the oxidant is 1:5, the weight ratio of the first part of dimethyl sulfide to the catalyst is 10:1, and the weight ratio of the first part of dimethyl sulfide to the solvent is 1 : 5, the temperature in the reactor is 70° C., the pressure in the reactor is 0.5 MPa, and the reaction time is 2 hours.

[0092] After the reaction is completed, it is filtered to obtain the recovered catalyst and the first liquid mixture. The recovered catalyst is directly recycled, and the first liquid mixture is sent to an intermediate separation step for separation. The composition of the first ...

Embodiment 2

[0100] The reaction is carried out in the same method as in Example 1, except that in the first oxidation reaction step, the original powder of titanium-silicon molecular sieve TS-1 is modified as follows before being used as a catalyst: the original powder of titanium-silicon molecular sieve TS-1 is mixed with Hydrochloric acid (mass concentration is the aqueous solution of 36% by weight) is mixed, the mixture obtained is stirred and reacted at 90 DEG C for 5 hours, the temperature of the reaction mixture obtained is down to room temperature and then filtered, and the solid phase material obtained is dried to constant temperature at 120 DEG C. Heavy, to obtain a modified titanium silicon molecular sieve. Among them, titanium silicon molecular sieve TS-1 is made of SiO 2 Calculated, the molar ratio of titanium silicon molecular sieve to HCl is 1:0.2. After characterization, compared with the raw material titanium-silicon molecular sieve TS-1, the peak height of the absorption...

Embodiment 3

[0103] Adopt the same method as Example 1 to react, the difference is that in the first oxidation reaction step, hydrochloric acid (concentration is 36% by weight) is also added in the slurry, and the pH value of the liquid phase mixture in the slurry is adjusted by 6.3 adjusted to 5.0. The experimental results are listed in Table 1.

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Abstract

The invention discloses a method for simultaneously producing dimethyl sulfone and dimethyl sulfoxide. The method comprises the steps that firstly, methyl sulfide reacts under the condition that dimethyl sulfone can be formed, a mixture containing dimethyl sulfone is obtained, and after dimethyl sulfone is freely separated out of the mixture and is further in contact and reacts with the other part of methyl sulfide, an unreacted oxidizing agent is utilized for oxidizing methyl sulfide to form dimethyl sulfoxide. The conversion rate of the oxidizing agent is effectively improved, running cost is reduced, and the requirement for subsequent residual oxidizing agent treatment and other steps is lowered. According to the method, high target oxidation product selectivity can be achieved during the two-step oxidizing reaction.

Description

technical field [0001] The present invention relates to a method for the simultaneous production of dimethyl sulfone and dimethyl sulfoxide. 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...

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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