Thioether oxidation method

A technology of thioether oxidation and thioether, which is applied in chemical instruments and methods, chemical recovery, organic chemistry, etc., can solve the problems of limited thioether dissolution, cost burden, and low thioether conversion rate, and achieve an increase in processing capacity and Operational efficiency, reduced operating costs, and the effect of high sulfide conversion

Active Publication Date: 2016-10-05
CHINA PETROLEUM & CHEM CORP +1
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  • Claims
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Problems solved by technology

[0005] 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 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 aqueous solution, and its commodity concentration is generally between 20-50% by weight, will inevitably introduce a large amount of water in the reaction system like this, 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 treatment capacity; at the same time, the introduction of a large amount of water also brings cost burdens to subsequent product separation and purification

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 5-14、18、19、21 and 24-31

[0064] Embodiment 5-14, 18, 19, 21 and 24-31 adopt the following method to measure the activity of catalyst:

[0065] Catalyst, 36% by weight of ammonia (as NH 3 meter), 30% by weight of hydrogen peroxide (as H 2 o 2 ), tert-butanol and cyclohexanone by mass ratio = 1:7.5:10:7.5:10 and then stirred and reacted at 80°C under atmospheric pressure for 2h, filtered the reactant, and analyzed the obtained liquid phase by gas chromatography The composition of the catalyst is analyzed, and the conversion rate of cyclohexanone is calculated by the following formula and used as the activity of the catalyst,

[0066] The conversion rate (%) of cyclohexanone=[(the molar amount of cyclohexanone added−the molar amount of unreacted cyclohexanone) / the molar amount of cyclohexanone added]×100%.

[0067] In Examples 23 and 29, the pore volume and ultraviolet absorption peak of the titanium-silicon molecular sieve before and after modification were characterized by static nitrogen adsorption...

Embodiment 1

[0070] (1-1) Isopropanol and oxygen (provided in the form of a mixed gas of oxygen and nitrogen, based on the total amount of the mixed gas, the content of oxygen is 85% by volume) at a temperature of 120 ° C and a pressure of 1.5 MPa Under the conditions of contact reaction for 6 hours, a liquid mixture containing hydrogen peroxide and acetone was obtained, wherein the molar ratio of isopropanol to oxygen was 1:10. The composition of the liquid mixture was analyzed by gas chromatography, and it was determined that the total content of hydrogen peroxide and acetone was 28% by weight, and the molar ratio of hydrogen peroxide and acetone was 1:1.

[0071] (2) The liquid mixture obtained in step (1-1), dimethyl sulfide and titanium silicon molecular sieve TS-1 are placed in a high-pressure reactor for stirring reaction. Wherein, the mass ratio of dimethyl sulfide and titanium silicon molecular sieve TS-1 is 20:1, and the molar ratio of hydrogen peroxide and dimethyl sulfide in th...

Embodiment 2

[0073] The same method as in Example 1 is used to oxidize dimethyl sulfide, the difference is that step (1-2) is also carried out: the liquid mixture obtained in step (1-1) is mixed with hydrochloric acid (HCl concentration is 36.5% by weight) Mix in an autoclave, wherein the molar ratio of hydrogen peroxide to HCl in the liquid mixture obtained in step (1-1) is 1:0.005, the temperature in the autoclave is controlled at 40°C, and the The pressure is controlled as normal pressure (that is, 1 standard atmospheric pressure), and the mixing time is 2 hours to obtain the acid-treated liquid mixture, and the acid-treated liquid mixture obtained in step (1-2) is sent into step (2).

[0074]Table 1 lists the reaction results of titanium silicate molecular sieve TS-1 when it is used for the first time and for the 40th time.

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Abstract

The invention discloses a thioether oxidation method. The method comprises oxidizing isopropanol to obtain a liquid mixture containing hydrogen peroxide and acetone. Optionally, after mixing the liquid mixture with an inorganic acid, it is mixed with thioether and titanium The silicon molecular sieve is contacted to oxidize the thioether. The method according to the invention can greatly reduce the amount of solvent used for dispersion in the thioether oxidation reaction device, effectively improve the processing capacity and operating efficiency of the thioether oxidation reaction device, and reduce operating costs. Moreover, the method according to the invention can obtain higher conversion rate of sulfide, effective utilization rate of oxidant and selectivity of target oxidation product. When adopting the method of the present invention to oxidize thioether, a thioether oxidation reaction device can be directly installed at the material outlet end of the existing isopropanol oxidation device, which 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 high selective extraction ability and can be used as an extraction solvent for the separation of alkanes and aromatic hydrocarbons. At the same time, in the pharmaceutical industry, dimethyl sulfoxide can not only be directly used as the raw material and carrier of some drugs, but also play the role of anti-inflammatory, analgesic, diuretic, sedative, etc. middle. In addition, dimethyl sulfoxide can also be used as a capacitor medium, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C317/04C07C317/14C07C315/02
CPCY02P20/582
Inventor 史春风朱斌林民
Owner CHINA PETROLEUM & CHEM CORP
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