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Method for preparing dimethyl sulfoxide

A technology of dimethyl sulfoxide and dimethyl sulfide, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of unsuitable large-scale production and high cost of anodic oxidation, and avoid catalysts The effect of bed temperature flying and high conversion rate

Active Publication Date: 2015-03-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Dimethyl sulfoxide can also be produced from dimethyl sulfide by anodic oxidation, but the cost of anodic oxidation is high and it is not suitable for large-scale production

Method used

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  • Method for preparing dimethyl sulfoxide
  • Method for preparing dimethyl sulfoxide
  • Method for preparing dimethyl sulfoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Dimethyl sulfide, oxidant, ammonia water, methanol as a solvent and hollow titanium-silicon molecular sieve HTS are respectively continuously fed into the moving bed reactor for contact reaction. Among them, dimethyl sulfide is fed from the bottom of the reactor, and the mixture of oxidant and solvent, ammonia water (concentration is 25% by weight) and titanium silicon molecular sieve are respectively fed from the liquid phase feed port at the top of the reactor, the auxiliary agent The feed port and the solid phase feed port feed into the reactor. Wherein, the oxidant is 27.5% by weight of hydrogen peroxide, the molar ratio of dimethyl sulfide to hydrogen peroxide is 1:1, the weight ratio of dimethyl sulfide to solvent is 1:5, dimethyl sulfide The feed weight ratio of ether to titanium silicon molecular sieve is 10:1, and the weight hourly space velocity of dimethyl sulfide in the reactor is 1.0h -1 , the temperature in the reactor is 60° C., the gauge pressure is 0.2...

Embodiment 2

[0080] Dimethyl sulfoxide was prepared by the same method as in Example 1, except that the hollow titanium-silicon molecular sieve HTS was replaced by the same amount of titanium-silicon molecular sieve TS-1. 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 sulfide, the effective utilization rate of the oxidant and the selectivity of dimethyl sulfoxide were calculated. The results are listed in Table 1.

Embodiment 3

[0082] Dimethyl sulfoxide was prepared in the same manner as in Example 1, except that ammonia was not sent into the reactor. 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 sulfide, the effective utilization rate of the oxidant and the selectivity of dimethyl sulfoxide were calculated. The results are listed in Table 1.

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Abstract

The invention provides a method for preparing dimethyl sulfoxide. The method comprises the steps as follows: dimethyl sulfide and at least one oxidant come into contact with at least one titanium-silicalite molecular sieve in a reaction region of a reactor under an oxidative reaction condition; and the titanium-silicalite molecular sieve moves along the radial direction of the reactor in the reaction region in the contact process. According to the method disclosed by the invention, high dimethyl sulfide conversion rate, effective utilization rate of the oxidant and dimethyl sulfoxide selectivity can be obtained; the problems such as temperature runaway which can be generated by a fixed bed reactor can be effectively avoided; meanwhile, the titanium-silicalite molecular sieve of which the activity cannot meet the requirements can be moved out of a reaction system to be regenerated under the condition that the device is not shut down.

Description

technical field [0001] The invention relates to a method for preparing dimethyl sulfoxide. Background technique [0002] Dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound. It is a colorless and transparent liquid at room temperature. It has the characteristics of high polarity, high hygroscopicity, flammability and high boiling point aprotic. Dimethyl sulfoxide is soluble in water, ethanol, acetone, ether and chloroform, is a highly polar inert solvent, widely used as a solvent and reaction reagent, for example, as a processing solvent and spinning solvent in acrylonitrile polymerization, as Polyurethane synthesis solvent and spinning solvent, as a synthesis solvent of polyamide, fluorochloroaniline, polyimide and polysulfone. Moreover, dimethyl sulfoxide has high selective extraction ability and can be used as an extraction solvent for the separation of alkanes and aromatic hydrocarbons. For example, dimethyl sulfoxide can be used for the extraction of arom...

Claims

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Application Information

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