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Vanadium-titanium-silicon molecular sieve, preparation method and application thereof, and sulfide oxidation method

A technology of titanium silicon molecular sieve and silicon molecular sieve, applied in the field of molecular sieve, can solve the problems of occupying land resources and inventory space, and achieve the effect of good catalytic effect

Active Publication Date: 2020-06-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this way, valuable land resources and storage space are taken up, and the recovery and utilization technology development of deactivated ammoximation catalysts is urgently needed

Method used

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  • Vanadium-titanium-silicon molecular sieve, preparation method and application thereof, and sulfide oxidation method
  • Vanadium-titanium-silicon molecular sieve, preparation method and application thereof, and sulfide oxidation method
  • Vanadium-titanium-silicon molecular sieve, preparation method and application thereof, and sulfide oxidation method

Examples

Experimental program
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Embodiment approach

[0025] According to a preferred embodiment of the present invention, the molecular sieve satisfies nV / nTi=A, I 960 / I 800 =B, B=i(A+1)nTi, wherein 0.1960 Infrared absorption spectrum of molecular sieve at 960cm -1 Absorption intensity in the vicinity, I 800 Infrared absorption spectrum of molecular sieve at 800cm -1 The absorption intensity at the vicinity is preferably 0.2<A<5, 0.3<B<0.8. In this way, it can be more beneficial to the diffusion of reactants and product molecules in the catalytic oxidation reaction, not only can further improve the conversion rate of the oxidant, but also can more effectively adjust the selectivity of the target product. For example, when used in a thioether oxidation reaction, the conversion rate of the oxidant peroxide can be further improved, and the selectivity of the target product sulfone can be more effectively adjusted.

[0026] In the present invention, the absorption intensity of the infrared absorption spectrum of the molecular s...

Embodiment 1

[0125] This example illustrates the methods and products provided by the invention.

[0126] At normal temperature (20°C, the rest of the comparative examples are the same as the examples) and normal pressure (0.1MPa, the rest of the comparative examples are the same as the examples), the deactivated cyclohexanone oximation catalyst SH-2 and 1mol / L hydrochloric acid The aqueous solution was mixed and beaten, and then the mixed slurry was mixed and stirred at 80°C for 12 hours; after solid-liquid separation, the solid, vanadium source ammonium metavanadate, titanium source titanium sulfate and sodium hydroxide aqueous solution (pH 12) were mixed and the mixed solution was Put it into a stainless steel sealed reaction kettle, and treat it at 170°C for 12 hours, wherein, the mass composition of the material is an inactivated cyclohexanone oximation catalyst: titanium source: vanadium source: acid: alkali: water = 100: 1: 1: 10: 5:250, deactivated cyclohexanone oximation catalyst ...

Embodiment 2

[0131] This example illustrates the methods and products provided by the invention.

[0132] At normal temperature and pressure, first mix the deactivated cyclohexanone oximation catalyst SH-3 with 5mol / L hydrochloric acid solution for beating, then mix and stir the mixed slurry at 60°C for 1 hour; after solid-liquid separation, separate the solid, Vanadium tetrachloride as a source of vanadium, tetrabutyl titanate as a source of titanium, and tetrapropylammonium hydroxide aqueous solution (pH 10) are mixed, and the mixture is put into a stainless steel sealed reaction kettle, and treated at 150°C for 12 hours. Composed of deactivated cyclohexanone oximation catalyst: titanium source: vanadium source: acid: alkali: water = 100:2:0.5:15:15:200, the deactivated cyclohexanone oximation catalyst is SiO 2 In terms of acid, H + In terms of alkali in OH - In terms of titanium source as TiO 2 count. Then the product was recovered according to the method of Example 1 to obtain a mo...

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Abstract

The invention relates to the field of molecular sieves, and discloses a vanadium-titanium-silicon molecular sieve, a preparation method and application thereof as well as a thioether oxidizing method.The molecular sieve is made from elements of vanadium, titanium, silicon and oxygen, wherein the molecular sieve satisfies that X(<1-1.8)> / X(<0.4-0.9)>=C; C is larger than 0.2 and less than 1; X(<0.4-0.9)> is a proportion of the distribution of micropores which are 0.4 to 0.9 nm in the aperture to the distribution of total micropores; X(<1-1.8)> is a proportion of the distribution of micropores which are 1 to 1.8 nm in the aperture to the distribution of total micropores. The molecular sieve with a special physical-chemical property structure has the micropore aperture distribution of 1 to 1.8 nm, X(<1-1.8)> / X(<0.4-0.9)>=C, C is larger than 0.2 and less than 1; in a catalytic reaction, diffusion of reactants and product molecules is facilitated, the oxidization reaction of thioether is facilitated, and the selectivity of a target product can be effectively regulated and changed.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a vanadium-titanium-silicon molecular sieve, a preparation method of the vanadium-titanium-silicon molecular sieve, an application of the vanadium-titanium-silicon molecular sieve in a thioether oxidation reaction and a thioether oxidation method. Background technique [0002] Titanium-silicon molecular sieve is a molecular sieve whose skeleton is composed of silicon, titanium and oxygen elements, and has broad application prospects in petroleum refining and petrochemical industry. Among them, TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. [0003] TS-1 not only has the catalytic oxidation of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89C07C315/02C07C317/04
CPCB01J29/89B01J2229/183C01B39/08C01P2006/17C07C315/02C07C317/04
Inventor 史春风林民朱斌
Owner CHINA PETROLEUM & CHEM CORP
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