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 high cost, high price of oxidant, and large dosage, and achieve easy control, improved conversion rate, and selective The effect of sexual stability

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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Benefits of technology

The present inventors have developed an efficient way to convert dimethy Sulfur into Dimethyl Sulfinate by reacting them under specific chemical reactions at high temperatures or near atmospheric pressure. This results in increased efficiency and stability over time during this transformation.

Problems solved by technology

This patented describes methods for producing dimethy Sulfoxide from dimethanesulfinate. These processes involve converting dimethyllithium bistris(dimethylsilyltrichloroselenolate), which contains two atoms called selenium dioxide, between thiononium tetrafluoroacene complexes and dichlorobenzene. By reacting these chemical substances together under specific conditions, they form dimethylethanols containing three unsaturated carbon double bondings - one being attached to each other through another molecule called vinyl group). Different types of dimers have been found depending on their properties such as melting points, solvabilities, odors, etc., making them useful ingredients like medicines. Additionally, dimmethylselenoferdinum bis(2-(dihydroxyphenothiazolin-3)) was identified earlier than dimethystrachlorophenazoline, suggesting its potential use as a medicine intermediate. Overall, this technology provides various benefits over existing techniques while reducing costs associated therewith.

Method used

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

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preparation example Construction

[0012] The present invention provides a kind of preparation method of dimethyl sulfoxide, and this method comprises under oxidation reaction condition, in fixed bed reactor, make dimethyl sulfide and at least one kind of peroxide and at least one kind of The catalyst beds of the titanium-silicon molecular sieves are contacted to obtain a reaction mixture containing dimethyl sulfoxide, wherein at least part of the titanium-silicon molecular sieves are non-fresh titanium-silicon molecular sieves.

[0013] The titanium-silicon molecular sieve is a general term for a class of zeolites in which titanium atoms replace a part of the silicon atoms in the lattice framework, and can be represented by the chemical formula xTiO 2 ·SiO2 2 express. The present invention has no special limitation on the content of titanium atoms in the titanium-silicon molecular sieve, which can be a conventional choice in the field. Specifically, x may be 0.0001-0.05, preferably 0.01-0.03, more preferably...

Embodiment 1

[0066] The catalyst C1 used in this example is obtained by regenerating the shaped titanium-silicon molecular sieve TS-1 (average particle size: 55 μm) unloaded from the cyclohexanone ammoximation reaction device, wherein the regeneration conditions are: at 550 ℃ in the air atmosphere for 4h. Based on the total amount of shaped titanium-silicon molecular sieve TS-1, the content of titanium-silicon molecular sieve TS-1 is 85% by weight, and the content of silicon oxide is 15% by weight; the activity after regeneration is 50% (its activity when fresh is 95%).

[0067] Catalyst C1 was packed in a stainless steel fixed-bed microreactor (loading volume: 15 mL, reactor height-to-diameter ratio: 15) to form a catalyst bed, where the number of catalyst beds was one.

[0068] Dimethyl sulfide, hydrogen peroxide and methanol are combined to form a liquid mixture. Aqueous ammonia (concentration: 25% by weight) was added to the liquid mixture to adjust the pH of the liquid mixture to 6....

Embodiment 2

[0076] Dimethyl sulfoxide was prepared by the same method as in Example 1, except that ammonia water was not added to the liquid mixture (the pH of the liquid mixture was 5.8). The reaction mixture obtained at 0.5 hour and 200 hours 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 following steps: contacting dimethyl sulfide and at least one peroxide with a catalyst bed filled with at least one titanium silicalite molecular sieve in a fixed bed reactor under an oxidation condition to obtain a reaction mixture containing dimethyl sulfoxide, wherein at least part of the titanium silicalite molecular sieve is a non-fresh titanium silicalite molecular sieve. Compared with a reaction that dimethyl sulfide is contacted with peroxide without existence of the titanium silicalite molecular sieve, the method has the advantages of improving the conversion rate of dimethyl sulfide, effective utilization rate of oxidant and selectivity of dimethyl sulfoxide. Compared with the reaction that dimethyl sulfide and peroxide are contacted with fresh titanium silicalite molecular sieve, the method has the advantages that a higher oxidant effective utilization rate can be obtained, and the conversion rate of dimethyl sulfide and selectivity of dimethyl sulfoxide can be more stable in a continuous reacting process. Furthermore, the method is mild in reacting condition and easy to control, and is suitable for devices with various production scales.

Description

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Claims

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Application Information

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Owner CHINA PETROLEUM & CHEM CORP
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