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Thioether oxidation method

A technology of sulfide oxidation and tert-butyl hydroperoxide, which is applied in the fields of chemical instruments and methods, organic chemistry, and the preparation of organic compounds, can solve the problem that the anodic oxidation method is not suitable for large-scale implementation, reduces the effective processing capacity of the device, and the environment Pollution and other issues, to achieve the effect of high target oxidation product selectivity, high effective treatment capacity of the device, and simplified process flow

Active Publication Date: 2017-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The disadvantages of the nitric acid oxidation method are that the reaction is not easy to control, the equipment is severely corroded, and the environment is polluted.
Ozone oxidation method has the problem of low conversion rate of dimethyl sulfide
Anodizing is not suitable for large-scale implementation
Nitrogen dioxide oxidation law has the problem of environmental pollution
But, as the most commonly used oxidizing agent in the peroxide oxidation method, hydrogen peroxide is usually provided in the form of hydrogen peroxide, and its commercial concentration is generally between 20-50% by weight, so a large amount of water will inevitably be introduced in the reaction system, although Water can act as a solvent, but the amount of thioether dissolved in water as a reactant is still limited. In order to increase the amount of thioether dissolved, the amount of water used is large or an organic solvent needs to be used in conjunction, which inevitably reduces the capacity of the device. Effective processing capacity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093](1-1) Contact reaction between isobutane and oxygen at a temperature of 130°C and a pressure of 2.5 MPa to obtain a reaction mixture containing tert-butyl hydroperoxide, and analyze the composition of the reaction mixture by gas chromatography , Determine the content of tert-butyl hydroperoxide to be 25% by weight. Wherein, the molar ratio of isobutane to oxygen is 1:1; the oxygen is provided in the form of oxygen-containing gas, and in the oxygen-containing gas, the content of oxygen is 80% by volume, and the content of nitrogen is 20% by volume.

[0094] (1-2) Mix the reaction mixture obtained in step (1-1) with hydrochloric acid (HCl concentration is 36.5% by weight) in an autoclave, wherein the reaction mixture obtained in step (1-1) contains tert-butyl The molar ratio of hydrogen oxide to HCl was 1:0.005, the temperature in the autoclave was controlled to 40° C., the pressure in the autoclave was controlled to normal pressure (ie, 1 standard atmosphere), and the mix...

Embodiment 2

[0098] Dimethyl sulfide was oxidized in the same manner as in Example 1, except that step (1-2) was not carried out, and the reaction mixture obtained in step (1-1) was directly sent to step (2). The experimental results are listed in Table 1.

Embodiment 3

[0100] Dimethyl sulfide was oxidized by the same method as in Example 1, except that in step (2), titanium-silicon molecular sieve TS-1 was prepared by the following method.

[0101] 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 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 6h, then cool the mixture down to 30°C and expe...

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Abstract

The present invention discloses a thioether oxidation method, which comprises that (1-1) isobutane and oxygen are subjected to a contact reaction, wherein the tert-butyl hydroperoxide content in the reaction mixture obtained through the contact reaction is more than 1 wt% through the contact reaction condition; optional (1-2) the reaction mixture obtained in the step (1-1) is mixed with an inorganic acid; and (2) under conditions sufficient to oxidize thioether, a raw material mixture containing the reaction mixture obtained in the step (1-1) and thioether and a titanium-silicon molecular sieve are subjected to a contact reaction, or a raw material mixture containing the reaction mixture obtained in the step (1-2) and thioether and a titanium-silicon molecular sieve are subjected to a contact reaction. With the method of the present invention, the high through put of the apparatus can be obtained, and the high thioether conversion rate and the high target oxidation product selectivity can be obtained; and the method can be performed only by additionally arranging the thioether oxidation reaction apparatus on the material outlet end of the existing isobutane oxidation apparatus, such that the method is easy to perform.

Description

technical field [0001] The present invention relates to a kind of sulfide oxidation method. Background technique [0002] Sulfoxides are important sulfur-containing compounds. For example, dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound. It is a colorless and transparent liquid at room temperature. properties such as protons. 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, polyimide and pol...

Claims

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Application Information

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IPC IPC(8): C07C315/02C07C317/04C07C317/14
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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