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Method for preparing dimethyl sulfoxide

A technology of dimethyl sulfoxide and dimethyl sulfide, which is applied in the field of preparation of dimethyl sulfoxide, can solve the problems of unsuitable large-scale production and high cost of anodization, and achieves easy control, good activity stability, The effect of reducing production costs

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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
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Effect test

preparation example 1

[0076] The tin-silica molecular sieve Sn-β was prepared according to the method described in NATURE, 2001, Vol. 412, pages 423-425. The specific preparation process is as follows.

[0077] At 25°C, add 30g of ethyl orthosilicate (TEOS) to 32.99g of tetraethylammonium hydroxide (TEAOH, 35% by weight) aqueous solution, stir to mix and hydrolyze, add tin tetrachloride aqueous solution after 90 minutes (It is formed by dissolving 0.43 g of tin tetrachloride pentahydrate in 2.75 g of water), continue to stir until a clear solution is obtained. Add 3.2 g of hydrofluoric acid (48% by weight) to the above clear solution to obtain a paste-like mixture, and then add the seed suspension (formed by suspending 0.36 g of dealuminated β molecular sieve in 1.75 g of water) and stir well. The obtained mixture was transferred into a stainless steel reaction kettle lined with polytetrafluoroethylene and dynamically crystallized at 140°C for 480 hours. The crystallization product is subjected to s...

preparation example 2

[0080] According to Zeolites, 1992, Volume 12, page 943-950 described in the preparation of titanium silicate molecular sieve SnS-1, the difference is that the tetrabutyl titanate is replaced by tin tetrachloride pentahydrate , The specific preparation process is as follows.

[0081] At room temperature (20°C), 22.5g of tetraethylorthosilicate, 7.0g of tetrapropylammonium hydroxide and 59.8g of distilled water were stirred and reacted under normal pressure and 60°C for 1.0 hour to obtain a tetraethylorthosilicate Hydrolysis solution. With vigorous stirring, a tin tetrachloride solution (formed by dissolving 1.1 g of tin tetrachloride pentahydrate in 5.0 g of anhydrous isopropanol) was slowly added to the hydrolysis solution, and the resulting mixture was stirred at 75°C for 3 Hours, a clear transparent colloid is obtained. This colloid was placed in a stainless steel sealed reactor and placed at a constant temperature of 170°C for 72 hours. Then, the obtained crystallization m...

Embodiment 1

[0085] Put dimethyl sulfide, hydrogen peroxide, methanol and tin-silica molecular sieve Sn-β into the reaction kettle, with stirring, and react for 2 hours. The obtained mixture is filtered to obtain the recovered tin silicon molecular sieve and a liquid phase containing dimethyl sulfoxide. Among them, the reaction conditions include: the molar ratio of dimethyl sulfide to hydrogen peroxide is 1:1, the mass ratio of dimethyl sulfide to tin silicon molecular sieve is 25:1, the mass ratio of methanol to dimethyl sulfide It is 200:1, the reaction temperature is 30°C, and the pressure in the reactor is 0.5MPa.

[0086] The recovered tin-silicon molecular sieve is re-mixed with dimethyl sulfide, hydrogen peroxide and methanol according to the above method, and then sent to the reactor to continue the next reaction. Among them, tin-silica molecular sieve is recycled 10 times. During the reaction process, the composition of the mixture output from the reactor was detected each time, a...

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Abstract

The invention provides a method for preparing dimethyl sulfoxide. The method comprises the following step of contacting dimethyl sulfide and at least one oxidant with at least one tin silicate molecular sieve under an oxidation condition. According to the method, especially when peroxide is used as an oxidant, the conversion rate of dimethyl sulfide and the effective utilization rate of the oxidant are high, the selectivity of dimethyl sulfoxide is good, the using amount of dimethyl sulfide and the oxidant can be effectively reduced, and the production cost of dimethyl sulfoxide can be reduced. Furthermore, by adopting the method, the catalyst has good activity stability, and high dimethyl sulfide conversion rate, oxidant effective utilization rate and dimethyl sulfoxide selectivity can stilled be obtained even the catalyst runs continuously for a long time or is recycled for multiple times. Furthermore, the method is mild in reacting condition and easy to control, and is suitable for large-scale production.

Description

Technical field [0001] The invention relates to a preparation method of 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 aproton. Dimethyl sulfoxide is soluble in water, ethanol, acetone, ether and chloroform. It is an inert solvent with strong polarity and is widely used as a solvent and reaction reagent. In addition, dimethyl sulfoxide has a high selective extraction ability, and can be used as an extraction solvent for the separation of alkanes and aromatics. For example, dimethyl sulfoxide can be used for the extraction of aromatics or butadiene. As a processing solvent and spinning solvent in the polymerization reaction, as a synthetic solvent and spinning solvent for polyurethane, as a synthetic solvent for polyamide, fluorochloroaniline, polyim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/04C07C315/02B01J38/06B01J29/06B01J29/70
CPCY02P20/50Y02P20/584
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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