Preparation method of 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 high cost and unsuitability for large-scale production of anodic oxidation, and achieve easy Controlled, suitable for large-scale production, mild reaction conditions

Active Publication Date: 2014-05-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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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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  • Preparation method of dimethyl sulfoxide
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preparation example Construction

[0020] In a preferred embodiment of the present invention, the preparation method of the shaped catalyst comprises: contacting at least one organosilicon compound capable of hydrolysis reaction and at least one water-soluble base with water under hydrolysis reaction conditions, The mixture obtained by contacting is mixed with the titanium-silicon molecular sieve, and the obtained mixture containing the titanium-silicon molecular sieve is successively shaped and roasted. The shaped catalyst obtained according to this embodiment not only has higher strength and thus is more wear-resistant and has a higher resistance to crushing, the bed containing the catalyst has a higher resistance to collapse; and can obtain a higher Dimethyl sulfide conversion and dimethyl sulfoxide selectivity.

[0021] In this preferred embodiment, the amount of the organosilicon compound, the water-soluble base and the titanium-silicon molecular sieve should be used to form the titanium-silicon molecular ...

Embodiment 1

[0071] Send dimethyl sulfide, hydrogen peroxide, methanol and titanium silicon molecular sieve TS-1 into the reaction kettle, and react for 2 hours with stirring. The resulting mixture is filtered to obtain recovered titanium silicate molecular sieves 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 titanium silicon molecular sieve is 25:1, the mass ratio of methanol to dimethyl sulfide The ratio is 200:1, the reaction temperature is 30°C, and the pressure in the reactor is 0.5MPa.

[0072] The recovered titanium-silicon molecular sieve is re-mixed with dimethyl sulfide, hydrogen peroxide and methanol according to the above method, and then sent into the reactor to continue the next reaction. Among them, the titanium-silicon molecular sieve is recycled 50 times.

[0073] During the reaction, the composition of the mixture output...

Embodiment 2

[0077] Dimethyl sulfoxide was prepared by the same method as in Example 1, except that a hollow titanium-silicon molecular sieve was used instead of the titanium-silicon molecular sieve TS-1 in Example 1.

[0078] During the reaction, the composition of the mixture output from the reactor is detected each time, and the conversion rate of dimethyl sulfide, the effective utilization rate of the oxidant and the selectivity of dimethyl sulfoxide are calculated.

[0079] Among them, the results of the first reaction are as follows: the conversion rate of dimethyl sulfide is 93.1%, the effective utilization rate of oxidant is 95%, and the selectivity of dimethyl sulfoxide is 94%;

[0080] The results of the 50th reaction were as follows: the conversion rate of dimethyl sulfide was 92.6%, the effective utilization rate of oxidant was 93%, and the selectivity of dimethyl sulfoxide was 92%.

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Abstract

The invention provides a preparation method of dimethyl sulfoxide, the method is as follows: in oxidation reaction conditions, dimethyl sulfide is contacted with at least one oxidant, and the catalyst contains at least one titanium silicon molecular sieve. According to the preparation method of the dimethyl sulfoxide, the dimethyl sulfide conversion rate is high, the effective utilization rate of the oxidant is high, the dimethyl sulfoxide selectivity is good, the usage amount of the dimethyl sulfide and the oxidant can be effectively reduced, and the production cost of the dimethyl sulfoxide can be reduced. According to the method of the invention, the activity stability of the catalyst is good, even by long-time continuous operation and multiple-times of cycle use of the catalyst, a high dimethyl sulfide conversion rate, a high effective utilization rate of the oxidant and high dimethyl sulfoxide selectivity also can be achieved. In addition, the method of the invention is mild in reaction condition, easy to control, and suitable for mass production.

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, and is widely used as a solvent and reaction reagent. Moreover, 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. In the polymerization reaction, it is used as a processing solvent and spinning solvent, as a synthetic solvent and spinning solvent of polyurethane, and as a synthetic solvent of polyamide, fluorochloroaniline, pol...

Claims

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Application Information

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