Preparation method for dimethyl sulfone

A technology of dimethyl sulfone and dimethyl sulfide, applied in the field of preparation of dimethyl sulfone, can solve the problems of serious equipment corrosion, need to be further improved, unfavorable environmental protection and the like, and achieves low corrosion degree and high oxidant effect. Utilization, high conversion rates and the effectiveness of

Active Publication Date: 2016-04-27
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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Problems solved by technology

However, the dimethyl sulfone yield of this method needs to be further improved; and, this method uses nitric acid as an oxidant, which seriously corrodes the

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  • Preparation method for dimethyl sulfone
  • Preparation method for dimethyl sulfone
  • Preparation method for dimethyl sulfone

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[0009] The invention provides a method for preparing dimethyl sulfone, which comprises the steps of passing a liquid mixture through a catalyst bed filled with at least one titanium-silicon molecular sieve in a fixed-bed reactor under oxidation reaction conditions to obtain A mixture comprising dimethyl sulfone, the liquid mixture comprising dimethyl sulfide and at least one peroxide.

[0010] According to the method of the present invention, the peroxide refers to a compound containing -O-O-bonds in its molecular structure, which may be hydrogen peroxide and / or organic peroxides (such as hydroperoxides and peracids). Specific examples of the peroxide may include, but are not limited to, hydrogen peroxide, t-butyl hydroperoxide, cumene peroxide, cyclohexyl hydroperoxide, peracetic acid, and peroxypropionic acid. Preferably, the oxidizing agent is hydrogen peroxide, which can further reduce the separation cost. The hydrogen peroxide may be hydrogen peroxide commonly used in th...

Embodiment 13、14 and 16-18

[0049] Embodiment 13, 14 and 16-18 adopt the following method to measure the activity of catalyst:

[0050] Catalyst, 36% by weight of ammonia water (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,

[0051] The conversion rate (%) of cyclohexanone=[(the molar amount of cyclohexanone added−the molar amount of unreacted cyclohexanone) / the molar amount of cyclohexanone added]×100%.

Embodiment 1

[0054] (1) Mix titanium-silicon molecular sieve TS-1 with silica sol (silicon oxide content is 30% by weight) and water, wherein the weight ratio of titanium-silicon molecular sieve TS-1, silica sol in terms of silicon oxide and water is 1 :0.2:1.5. The obtained mixture was granulated by rolling balls, and the obtained wet granules were calcined at 550° C. for 5 hours to obtain a catalyst (referred to as C1) with a volume average particle diameter of 200 μm. Wherein, in the catalyst, the content of titanium-silicon molecular sieve TS-1 is 80% by weight.

[0055] (2) Packing the catalyst prepared in step (1) in an equal-diameter fixed-bed reactor to form a catalyst bed. Dimethyl sulfide, hydrogen peroxide (as 30% by weight hydrogen peroxide), and methanol were mixed to form a liquid mixture. The liquid mixture is then fed into a fixed bed reactor and passed through a catalyst bed. Among them, in the liquid mixture, the molar ratio of dimethyl sulfide to hydrogen peroxide is ...

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Abstract

The invention provides a preparation method for dimethyl sulfone. The method comprises the step of subjecting a liquid mixture to passing through a catalyst bed filled with at least one titanium-silicon molecular sieve in a fixed bed reactor under the condition of oxidation reaction so as to obtain a mixture containing dimethyl sulfone, wherein the liquid mixture comprises dimethyl sulfide and at least one peroxide; and the mol ratio of the peroxide to the dimethyl sulfide is more than 2: 1. According to the invention, with peroxide as an oxidant, the method has low corrosiveness to equipment, releases few environmental pollutants, can obtain high conversion rate of dimethyl sulfide and selectivity of dimethyl sulfone, and has high effective utilization rate of the oxidant at the same time.

Description

technical field [0001] The invention relates to a preparation method of dimethyl sulfone. Background technique [0002] Dimethyl sulfone is white crystalline powder, easily soluble in water, ethanol, benzene, methanol and acetone, 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 the human body to produce insulin, and at the same time, it can ...

Claims

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Application Information

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