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Method for producing dimethyl sulfoxide

A technology of dimethyl sulfone and dimethyl sulfide, 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 selectivity performance, high effective utilization

Active Publication Date: 2017-05-10
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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  • Method for producing dimethyl sulfoxide
  • Method for producing dimethyl sulfoxide
  • Method for producing dimethyl sulfoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0086] The catalyst used in this embodiment is shaped titanium-silicon molecular sieve TS-1, which is a spherical catalyst with a volume average particle diameter of 500 μm. In the catalyst, the content of titanium-silicon molecular sieve TS-1 is 80% by weight, and the content of silicon oxide is 20% by weight. %. Among them, the titanium-silicon molecular sieve TS-1 is prepared according to the method described in Zeolites, 1992, Vol.12, pages 943-950, and the specific method is as follows.

[0087] At room temperature (20°C), mix 22.5 grams of tetraethyl orthosilicate with 7.0 grams of tetrapropylammonium hydroxide as a template, add 59.8 grams of distilled water, stir and mix, then hydrolyze at normal pressure and 60°C for 1.0 hour , to obtain a hydrolysis solution of tetraethyl orthosilicate. Under vigorous stirring, a solution consisting of 1.1 g of tetrabutyl titanate and 5.0 g of anhydrous isopropanol was slowly added to the hydrolysis solution, and the resulting mixtu...

Embodiment 2

[0092] Dimethyl sulfone was produced by the same method as in Example 1, except that the titanium-silicon molecular sieve TS-1 in the shaped titanium-silicon molecular sieve TS-1 was prepared by the following method.

[0093] 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 2 hours with magnetic stirring to re-disperse it. Transfer the re-dispersed dispersion liquid to a sealed reaction kettle, undergo the first stage of crystallization at 140°C for 6...

Embodiment 3

[0095] Dimethyl sulfone was prepared by the same method as in Example 2, except that the crystallization temperature in the third stage was also 140° C. when preparing titanium-silicon molecular sieve TS-1. The XRD crystal phase diagram of the obtained sample is consistent with the titanium-silicon molecular sieve TS-1 prepared in Example 1, indicating that what is obtained is the TS-1 molecular sieve with MFI structure; -1 Absorption peaks appear nearby, indicating that titanium has entered the framework of the molecular sieve. In the titanium-silicon molecular sieve, the surface silicon-titanium ratio / bulk phase silicon-titanium ratio is 4.21, and the titanium oxide content is 3.1% by weight. The results determined from the reaction mixture output from the reactor at the reaction times listed in Table 1 are listed in Table 1.

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Abstract

The invention discloses a method for producing dimethyl sulfoxide. The method comprises the following steps: under oxidation reaction condition, the reaction raw materials containing dimethyl thioether, an oxidizing agent and an optional solvent can be contacted with a titanium silicon molecular sieve to obtain a reaction mixture containing dimethyl sulfoxide; the reaction mixture is subjected to gas-liquid separation to obtain a liquid material flow containing dimethyl sulfoxide and a gas material flow; and dimethyl sulfoxide can be separated from the liquid material flow. The method can obtain high dimethyl sulfoxide selectivity and effective utilization rate of the oxidizing agent.

Description

technical field [0001] The present invention relates to a method for producing 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 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 sulfone can enhance the ability of the human body to produce insulin, and at the same time, ...

Claims

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Application Information

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