A kind of preparation method of sulfone
A catalyst bed and logistics technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problem of increasing system energy consumption, affecting the stability and safety of reactor operation, and reducing catalyst bed pressure. It can reduce the energy consumption of the system, prolong the stable operation time, and suppress the increase of pressure drop.
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preparation example Construction
[0012] The present invention provides a method for the preparation of sulfones, the method comprising providing a reaction feed comprising at least one thioether, at least one oxidizing agent and optionally at least one solvent.
[0013] The thioether refers to a compound containing an -S- bond in the molecular structure. Preferably, the thioether is selected from thioethers with 2-18 carbon atoms, more preferably dimethyl sulfide and / or benzyl Thioether.
[0014] The oxidizing agent can be various substances sufficient to oxidize thioethers to sulfones. The method of the present invention is especially suitable for the occasion of preparing sulfone by oxidizing thioether with peroxide as an oxidizing agent. The peroxide refers to a compound containing -O-O-bonds in its molecular structure, which can be selected from hydrogen peroxide, organic peroxides and peracids. The organic peroxide refers to a substance obtained by replacing one hydrogen atom or two hydrogen atoms in a...
preparation Embodiment 1
[0106] In this preparation example, a vanadium-free titanium-silicon molecular sieve was prepared by hydrothermal crystallization.
[0107] Mix ethyl orthosilicate, titanium isopropoxide and tetrapropyl ammonium hydroxide, and add an appropriate amount of distilled water to stir and mix. The molar ratio of ethyl orthosilicate: titanium isopropoxide: tetrapropyl ammonium hydroxide: water is 100:3:20:2000, among them, ethyl orthosilicate with SiO 2 In terms of titanium isopropoxide as TiO 2 hydrolyze at normal pressure and 60°C for 1 hour, then stir at 75°C for 3 hours, then put the mixed solution into a stainless steel sealed reaction kettle, and place it at a constant temperature of 170°C for 72 hours to obtain a mixture of crystallized products; The mixture was filtered, and the solid phase was collected, washed with water, and dried at 110° C. for 60 minutes to obtain a molecular sieve powder. The raw molecular sieve powder was roasted in an air atmosphere at 550°C for 3 h...
preparation Embodiment 2
[0109] In this preparation example, a vanadium-titanium-silicon molecular sieve was prepared by a hydrothermal crystallization method.
[0110] Mix ethyl orthosilicate, ammonium metavanadate, titanium isopropoxide and tetrapropyl ammonium hydroxide, and add an appropriate amount of distilled water to stir and mix, ethyl orthosilicate: titanium isopropoxide: ammonium metavanadate: tetrapropyl The molar ratio of ammonium hydroxide: water is 100:3:1:20:2000, wherein, ethyl orthosilicate is SiO 2 In terms of titanium isopropoxide as TiO 2 In terms of ammonium metavanadate in V 2 o 5 Meter; hydrolyze at normal pressure and 60°C for 1 hour, then stir at 75°C for 3 hours, then put the mixed solution into a stainless steel sealed reaction kettle, and place it at a constant temperature of 170°C for 72 hours to obtain a mixture of crystallized products; filter the mixture , the solid phase was collected, washed with water, and dried at 110° C. for 60 minutes to obtain a molecular sie...
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Abstract
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