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Thioether oxidation method

A technology of sulfide oxidation and ethylbenzene hydrogen peroxide, applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., 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 pollutes the environment to achieve high selectivity of the target oxidation product, increase the effective processing capacity of the device, and simplify the process flow

Active Publication Date: 2017-05-10
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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

[0094] (1-1) Ethylbenzene and oxygen are contacted and reacted at a temperature of 120° C. and a pressure of 1 MPa to obtain a reaction mixture containing ethylbenzene hydroperoxide. The composition of the reaction mixture is analyzed by gas chromatography to determine the ethylbenzene The content of benzene hydroperoxide was 15% by weight. Wherein, the molar ratio of ethylbenzene to oxygen is 1:2; oxygen is provided in the form of oxygen-containing gas, and in the oxygen-containing gas, the content of oxygen is 21% by volume, and the content of nitrogen is 79% by volume.

[0095] (1-2) The reaction mixture obtained in step (1-1) is mixed with hydrochloric acid (HCl concentration is 36.5% by weight) in an autoclave, wherein the ethylbenzene peroxidation in the reaction mixture obtained in step (1-1) The molar ratio of hydrogen 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 st...

Embodiment 2

[0100] 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). Table 1 lists the reaction results of titanium silicate molecular sieve TS-1 when it was used for the first time and the 25th time.

Embodiment 3

[0102] 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.

[0103] 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 it at 35°C for 2h 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 experi...

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Abstract

The invention discloses a thioether oxidation method. The method comprises the following steps: (1-1), ethylbenzene and oxygen are subjected to a contact reaction, and the content of EBHP in a reaction mixture obtained by the contact reaction under contact reaction condition is more than 1 weight%; optional (1-2), the reaction mixture in the step (1-1) is mixed with inorganic acid; (2), under condition that thioether is oxidized, a raw material mixture containing the reaction mixture obtained in the step (1-1) and thioether is subjected to a contact reaction with a titanium silicon molecular sieve, or a raw material mixture containing the mixture in the step (1-2) and thioether is subjected to the contact reaction with the titanium silicon molecular sieve. The method is in favor of increasing effective processing amount of equipment, and can obtain high thioether conversion rate and target oxidation product selectivity. The method can directly install a thioether oxidation reaction apparatus at a material outlet end of a current ethylbenzene oxidation apparatus, and is easy to carry out.

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