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A kind of preparation method of sulfone

A titanium-silicon molecular sieve and modification technology, which is applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems that the application research of dimethyl sulfone has not been carried out well, and achieve easy implementation, The effect of delaying the deactivation speed and prolonging the service life of a single pass

Active Publication Date: 2019-11-05
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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  • A kind of preparation method of sulfone
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  • A kind of preparation method of sulfone

Examples

Experimental program
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Effect test

preparation example Construction

[0014] The invention provides a method for preparing sulfone, which comprises contacting and reacting a reaction mixture with a titanium-silicon molecular sieve in a reactor to obtain a product mixture containing sulfone, the reaction mixture containing sulfide, at least one oxidizing agent and Optionally at least one solvent.

[0015] In the present invention, "at least one" means one or more than two; "optional" means containing or not.

[0016] According to the method of the present invention, titanium-silicon molecular sieve is the general name of a class of zeolites in which titanium atoms replace a part of silicon atoms in the lattice framework, and can be obtained by 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 0.015-0.025.

[00...

Embodiment 1

[0104] The titanium-silicon molecular sieve TS-1 used in this example was prepared according to the method described in Zeolites, 1992, Vol.12, pages 943-950, and the specific method is as follows.

[0105] At room temperature (20°C), mix 22.5g tetraethyl orthosilicate with 7.0g tetrapropylammonium hydroxide as a template, add 59.8g distilled water, stir and mix, then hydrolyze at normal pressure and 60°C for 1.0h , 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 mixture was stirred at 75° C. for 3 h to obtain a clear transparent colloid. The colloid was placed in a sealed stainless steel reaction kettle, and kept at a constant temperature of 170° C. for 36 hours to obtain a mixture of crystallized products. The obtained mixture was filtered, the collected solid matter was washed with wate...

Embodiment 2

[0114] Adopt the same method as Example 1 to prepare dimethyl sulfone, the difference is that the prepared titanium-silicon molecular sieve TS-1 is modified by the following method before molding (that is, the same method as in Example 1 will be used to prepare Titanium-silicon molecular sieve TS-1 was used as a raw material for modification treatment), and the obtained modified titanium-silicon molecular sieve TS-1 was molded by the same method as in Example 1 to obtain the catalyst used in this example.

[0115] Titanium silicate molecular sieve TS-1 with HNO 3 (HNO 3 The mass concentration of hydrogen peroxide is 10%) and the aqueous solution of hydrogen peroxide (the mass concentration of hydrogen peroxide is 7.5%) is mixed, and the obtained mixture is stirred and reacted at 70 ℃ for 5h in a closed container, and the temperature of the obtained reaction mixture is down to room temperature After filtering, the obtained solid-phase substance was dried at 120° C. to a consta...

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Abstract

The invention discloses a method for preparing sulfone. The method comprises that a contact reaction between a reaction mixture and a titanium-silicalite molecular sieve is performed in a reactor forobtaining a product mixture containing sulfone, wherein the reaction mixture comprises thioether, an oxidizing agent and an optional solvent, and when the selectivity of the target oxidation product is lower than an expected value, the method also comprises increasing the pressure in the reactor until the selectivity of the target oxidation product rises above the expected value. The method can effectively delay the deactivation rate of the titanium-silicon molecular sieve which is used as a catalyst, prolong the one-way service life of the titanium-silicon molecular sieve, reduce the regeneration frequency of the titanium-silicon molecular sieve, reduce the production cost, and also can improve the operation efficiency of the device.

Description

technical field [0001] The invention relates to a preparation method of sulfone. Background technique [0002] Sulfones are important sulfur-containing compounds. For example, dimethyl sulfone is a white crystalline powder, easily soluble in water, ethanol, benzene, methanol and acetone, and 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 th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C317/04C07C317/14C07C315/02B01J29/89
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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