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Thioether oxidation method

A technology of thioether oxidation and cumene hydroperoxide, which is applied in the fields of chemical instruments and methods, preparation of peroxygen compounds, organic chemistry, etc., can solve the problem that the anodic oxidation method is not suitable for large-scale implementation, the amount of sulfide dissolution is limited, and the environment Pollution and other issues, to achieve high target oxidation product selectivity, increase effective treatment capacity, and simplify the process

Active Publication Date: 2017-10-10
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
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Effect test

Embodiment 1

[0095](1-1) Cumene and oxygen are contacted and reacted at a temperature of 120° C. and a pressure of 1 MPa to obtain a reaction mixture containing cumene hydroperoxide, and the composition of the reaction mixture is analyzed by gas chromatography, The content of cumene hydroperoxide was determined to be 40% by weight. Wherein, the molar ratio of cumene to oxygen is 1:3; the 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.

[0096] (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 hydrogen peroxide in the reaction mixture obtained in step (1-1) is The molar ratio of propylbenzene to HCl was 1:0.004, the temperature in the autoclave was controlled to 50° C., the pressure in the autoclave was controlled to normal pressure (ie, 1 standard atmosphere), and ...

Embodiment 2

[0101] 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

[0103] 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.

[0104] 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 which comprises the following steps: (1-1) performing a contact reaction on cumene and oxygen under certain conditions so that the content of cumene hydroperoxide in the reaction mixture obtained by the contact reaction is 1 wt% or above; optional (1-2) mixing the reaction mixture obtained by the step (1-1) with an inorganic acid; and (2) under the conditions sufficient to oxidize thioethers, performing a contact reaction on a raw material mixture (containing the reaction mixture obtained in the step (1-1) and thioethers) and a titanium silicon molecular sieve, or performing a contact reaction a raw material mixture (containing the mixture obtained in the step (1-2) and thioethers) and a titanium silicon molecular sieve. The method is beneficial to enhancing the effective treatment capacity of devices, and can obtain higher thioether conversion rate and target oxidation product selectivity. According to the method, a thioether oxidation reaction device is directly installed at a material outlet end of the existing cumene oxidation device, so the method is easy to implement.

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): C07C315/02C07C317/04C07C317/14C07C407/00C07C409/10B01J29/89
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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