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Modified vanadium-silicon molecular sieve, preparation method thereof and thioether oxidation method

A silicon molecular sieve and molecular sieve technology, applied in the field of molecular sieves, can solve problems such as poor catalytic performance and limited application

Active Publication Date: 2020-06-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although the prior art can prepare vanadium-silicon molecular sieves, its catalytic performance is poor, which limits its application

Method used

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  • Modified vanadium-silicon molecular sieve, preparation method thereof and thioether oxidation method
  • Modified vanadium-silicon molecular sieve, preparation method thereof and thioether oxidation method
  • Modified vanadium-silicon molecular sieve, preparation method thereof and thioether oxidation method

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preparation example Construction

[0047] In the preparation method of the modified vanadium-silicon molecular sieve provided by the present disclosure, the micropore size distribution of the prepared modified vanadium-silicon molecular sieve can be adjusted by adjusting the addition amount of the silicon source in step (2). 2 Calculated, when the mol ratio of the vanadium silicon molecular sieve in the step (1) and the silicon source in the step (2) is 100: (10-50), the modified vanadium silicon molecular sieve can be made to satisfy X 1-1.8 / X 0.4-0.9 =A, 0.2

[0048] According to the present disclosure, the type of the modified vanadium-silicon molecular sieve prepared is jointly determined by factors such as the type of the initial vanadium-silicon molecular sieve, the type of alkali source, and the ratio of materials. The vanadium-silicon molecular sieve refers to unmodified vanadium-silicon molecular sieve, which can be fresh vanadium-silicon molecular sieve or deactivated vanadium-silicon molecul...

Embodiment 1

[0095] At normal temperature (20°C, the rest of the examples are the same as the comparative examples) and normal pressure (0.1MPa, the rest of the examples are the same as the comparative examples), first vanadium silicon molecular sieves are mixed with 1mol / L aqueous hydrochloric acid for beating, and then the mixed slurry is mixed in Mix and stir at 80°C for 12 hours; after solid-liquid separation, mix the solid, vanadium source ammonium metavanadate, organosilicon source tetraethyl orthosilicate and sodium hydroxide aqueous solution (pH 12), and treat tetraethyl orthosilicate After hydrolysis (the hydrolysis rate is 80%), transfer the mixture into a stainless steel sealed reaction kettle, and treat it at 170°C for 12 hours, wherein the molar ratio of vanadium silicon molecular sieve: vanadium source: organic silicon source: acid: alkali: water is 100:0.5 :15:10:15:450, vanadium silicon molecular sieve and organosilicon source with SiO 2 In terms of acid, H + In terms of a...

Embodiment 2

[0097] At normal temperature and pressure, first mix the vanadium silicon molecular sieve with 5mol / L hydrochloric acid solution for beating, then mix and stir the mixed slurry at 60°C for 2 hours; The source methyl orthosilicate is mixed with aqueous solution of tetrapropylammonium hydroxide (pH 10). After the methyl orthosilicate is hydrolyzed (the hydrolysis rate is 90%), the mixture is transferred to a stainless steel sealed reaction kettle and treated at 150°C. 12h, wherein, the molar ratio of vanadium silicon molecular sieve: vanadium source: organosilicon source: acid: alkali: water is 100:1:10:15:25:600, vanadium silicon molecular sieve and organosilicon source are SiO 2 In terms of acid, H + In terms of base, in N. The obtained product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain modified vanadium-silicon molecular sieve S-2, whose XRD crystal phase diagram showed that it was a molecular sieve with ...

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Abstract

The invention relates to a modified vanadium-silicon molecular sieve, a preparation method thereof and a thioether oxidation method. The modified vanadium silicalite molecular sieve comprises: vanadium element, silicon element and oxygen element, wherein the modified vanadium-silicon molecular sieve meets the condition that X<1-1.8> / X<0.4-0.9>=A; wherein 0.2 < A < 0.5, preferably 0.25 < A < 0.45,X<1-1.8> is the ratio of the micropore diameter of the molecular sieve in the range of 1-1.8 nm to the total micropore diameter distribution amount, and X<0.4-0.9> is the ratio of the micropore diameter of the molecular sieve in the range of 0.4-0.9 nm to the total micropore diameter distribution amount. The modified vanadium-silicon molecular sieve provided by the invention has a special physicochemical characteristic structure, is used for thioether oxidation reaction, is beneficial to improving the thioether conversion rate, and is beneficial to modulating the selectivity of a target product sulfone.

Description

technical field [0001] The disclosure relates to the field of molecular sieves, in particular, to a modified vanadium-silicon molecular sieve, a preparation method thereof, and a sulfide oxidation method. Background technique [0002] Vanadium-silicon molecular sieve is a molecular sieve whose skeleton is composed of silicon, vanadium and oxygen. Vanadium-silicon molecular sieves have broad application prospects in petroleum refining and petrochemical industry. [0003] CN1500729A discloses a kind of preparation method of vanadium silicon molecular sieve, vanadium silicon molecular sieve has following general formula: (SiO 4 )n·(VO 4 )m, n / m is 30-200, it uses ammonium vanadate as the vanadium source, silica sol as the silicon source, tetraethylammonium hydroxide or tetrapropylammonium hydroxide as the template, wherein each of the molecular sieve precursors The molar ratio of the material is: SiO 2 : VO 3 :OH-:H 2 O=1: x: y: 10~100, wherein the value range of x is 0.0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/00C07C315/02C07C317/04C07C317/14
CPCB01J29/00C07C315/02C07C317/04C07C317/14
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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