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A kind of method for producing dimethyl sulfone from hydrogen sulfide

A technology of dimethyl sulfone and dimethyl sulfoxide, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems that the application research of dimethyl sulfone has not been carried out well, and achieve high raw material conversion rate effect

Active Publication Date: 2020-06-12
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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  • A kind of method for producing dimethyl sulfone from hydrogen sulfide
  • A kind of method for producing dimethyl sulfone from hydrogen sulfide
  • A kind of method for producing dimethyl sulfone from hydrogen sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0111] (1) Preparation of dimethyl sulfide

[0112] γ-Al 2 o 3 Packed in a fixed-bed reactor to form a catalyst bed, wherein the number of the catalyst bed is 1 layer, and the aspect ratio of the catalyst bed is 12:1.

[0113] Send hydrogen sulfide and methanol into a fixed-bed reactor for reaction to obtain a mixture containing dimethyl sulfide, wherein the temperature in the catalyst bed of the fixed-bed reactor is 350°C, and the pressure in the fixed-bed reactor is controlled At 0.4MPa, the molar ratio of hydrogen sulfide to methanol is 1:2.2, based on the total amount of hydrogen sulfide and methanol, the gas hourly volume space velocity is 15h -1 .

[0114] (2) Gas-liquid separation

[0115] The mixture containing dimethyl sulfide obtained in step (1) is condensed to obtain a gas phase stream and a liquid phase stream.

[0116] (3) The gaseous phase stream separated in step (2) is discharged from the device.

[0117] (4) oxidation reaction

[0118] The titanium-sil...

Embodiment 2

[0150] Adopt the same method as Example 1 to prepare dimethyl sulfone, the difference is that the prepared titanium-silicon molecular sieve TS-1 is modified by the following method before molding (that is, the same method as in Example 1 will be used to prepare Titanium-silicon molecular sieve TS-1 is used as a raw material for modification treatment), and the obtained modified titanium-silicon molecular sieve TS-1 is molded in the same manner as in Example 1 to obtain the first fixed-bed reactor and the first fixed-bed reactor of this embodiment. Two catalysts used in fixed bed reactors.

[0151] The prepared titanium silicate molecular sieve TS-1 was mixed with HNO 3 (HNO 3 The mass concentration of hydrogen peroxide is 10%) and the aqueous solution of hydrogen peroxide (the mass concentration of hydrogen peroxide is 7.5%) is mixed, and the obtained mixture is stirred and reacted at 70 ℃ for 5h in a closed container, and the temperature of the obtained reaction mixture is d...

Embodiment 3

[0153] The same method as in Example 2 was used to prepare dimethyl sulfone, except that the following method was used to prepare titanium-silicon molecular sieve TS-1, and the same method as in Example 1 was used for molding to obtain the first fixed-bed reaction in this example. and the catalyst used in the second fixed bed reactor.

[0154] Dissolve tetrabutyl titanate in the alkali source template agent tetrapropyl ammonium hydroxide aqueous solution first, then add silica gel (purchased from Qingdao Silica Gel Factory) to obtain a dispersion. In the dispersion, silicon source: titanium source: alkali source Template agent: water molar ratio is 100:4:12:400, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of alkali source template agent in N. Seal the above dispersion in the beaker with a parafilm and let it stand at room temperature (25°C, the same below) for 24h, then stir it at 35°C for 2h with magnetic stirring to re-disperse it. Transfer the r...

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Abstract

The invention discloses a method for producing dimethyl sulfone from hydrogen sulfide. The method includes: (1) subjecting hydrogen sulfide and methyl alcohol to contacting to obtain a mixture containing dimethyl sulfide; optionally, (2) subjecting the mixture containing dimethyl sulfide to gas-liquid separation to obtain a gas-phase material flow and a liquid-phase material flow containing dimethyl sulfide; optionally, (3) cyclically feeding at least part of the gas-phase material flow to the step (1); (4) subjecting the mixture containing dimethyl sulfide or a liquid phase low in hydrogen sulfide content to contact oxidation reaction with an oxidizing agent and titanium silicate molecular sieves to obtain a mixture containing dimethyl sulfone, wherein a mole ratio of the oxidizing agentto dimethyl sulfide is larger than 2. According to the method, continuous production of dimethyl sulfone from hydrogen sulfide is realized, and high raw material conversion rate and dimethyl sulfone selectivity can be obtained even oxidation reaction is carried out under mild conditions.

Description

technical field [0001] The present invention relates to a method for producing dimethyl sulfone from hydrogen sulfide. Background technique [0002] Sulfones are important sulfur-containing compounds. For example, dimethyl sulfone is a white crystalline powder, easily soluble in water, ethanol, benzene, methanol and acetone, and 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 dimethyl sulfone product should be dried 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C315/02C07C317/04
CPCC07C315/02C07C319/14C07C317/04C07C321/14
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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