Method for preparing vanadium-silicon molecular sieve

A silicon molecular sieve, vanadium source technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite and other directions, can solve the problems of high product cost, affect product activity, complex preparation process, etc., achieve good desulfurization effect, The effect of reducing the production cost

Active Publication Date: 2006-10-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] To sum up, in the preparation method of vanadium-silicon molecular sieve provided by the prior art, either the preparation process is relatively complicated, or the cost of the product is very high due to the use of expensive organic ammonium as a template; or the prepared The molecular sieve contains a certain amount of non-framework vanadium, which affects the product activity

Method used

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  • Method for preparing vanadium-silicon molecular sieve
  • Method for preparing vanadium-silicon molecular sieve
  • Method for preparing vanadium-silicon molecular sieve

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0039] With 10.6g silica gel (Lanzhou Catalyst Factory, burning loss 3% by weight, alumina content 1% by weight), 1.36g vanadyl sulfate, 1.33gNaOH and 36gH 2 O mixed, then added 2.46g n-butylamine, stirred evenly, the molar composition of the resulting reaction mixture was: SiO 2 : 0.05VO 2 : 0.2CH 3 (CH 2 ) 3 NH 2 :0.2NaOH:12H 2 O. Put this reaction mixture into a closed crystallization tank for crystallization at 120°C for 1 day, then at 150°C for 1 day, filter, wash, and dry at 120°C to obtain sample Z1.

[0040] The XRD spectrum of Z1 is shown in figure 1 , showing that Z1 has a typical MFI structure, and its relative crystallinity is 91.2% (relative to Silicate-1 with good crystallinity, the same below, Silicate-1 is according to Stud.Surf.Sci.Catal., 18, (1984) P159 synthesized by the method described above).

[0041] NH for Z1 4 After Cl was exchanged several times, the molar composition of its anhydrous oxide was analyzed by fluorescence: 0.024V 2 o 5 : SiO...

Embodiment 2

[0045] 15.9g silica gel, 6.12g vanadyl sulfate, 4gNaOH and 54gH 2 O mixed, then added 4.94g n-butylamine, stirred evenly, the molar composition of the resulting reaction mixture was: SiO 2 : 0.15VO 2 : 0.25CH 3 (CH 2 ) 3 NH 2 :0.4NaOH:12H 2 O. The reaction mixture was crystallized at 150° C. for 4 days, filtered, washed, and dried at 120° C. for two hours to obtain sample Z2.

[0046] The XRD spectrum of Z2 is shown in figure 2 , indicating that Z2 has a typical MFI structure with a relative crystallinity of 83%.

[0047] NH for Z2 4 After Cl was exchanged several times, the molar composition of its anhydrous oxide was analyzed by fluorescence: 0.07V 2 o 5 : SiO 2 : 0.008Al 2 o 3 .

[0048] IR skeleton analysis spectrum see image 3 The B curve also appears 970cm -1 The characteristic absorption peak of , indicating that V enters the molecular sieve framework.

[0049] 51 V MAS NMR spectrum see Figure 4 The resonance peak of the chemical shift -868.5ppm f...

Embodiment 3

[0051] With the method and step of embodiment 1, the difference is that V 2 o 5 and the amount of NaOH, the molar composition of the prepared reaction mixture: SiO 2 : 0.02VO 2 : 0.2CH 3 (CH 2 ) 3 NH 2 : 0.1NaOH: 12H 2 O.

[0052] The above reaction mixture was crystallized at 150°C for 5 days, and the crystallized product was filtered, washed, and dried to obtain sample Z3, whose XRD pattern had figure 1 characteristics, the relative crystallinity is 94.7%.

[0053] use NH 4 After Cl was exchanged several times, the molar composition of its anhydrous oxide was analyzed by fluorescence to be 0.009V 2 o 5 : SiO 2 : 0.01Al 2 o 3 .

[0054] The IR spectrum of sample Z3 has image 3 A characteristic of the curve, 51 The V MAS NMR spectrum has Figure 4 A characteristic of the curve.

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Abstract

The preparation method for V-Si molecular sieve with MFI structure comprises: mixing Si source, V source, the template agent by n-butyl amine and / or triethylamine with mole ratio to SiO2 as 0.04-0.5:1, the inorganic alkali, and water; crystallizing in sealed kettle to obtain the product.

Description

technical field [0001] The invention relates to a preparation method of a vanadium-silicon molecular sieve, in particular to a preparation method of a vanadium-silicon molecular sieve (VS-1) with an MFI structure. Background technique [0002] The introduction of transition element vanadium with coordination and valence characteristics into molecular sieves can combine the performance of molecular sieves with the catalytic performance of transition metals to produce unique catalytic effects. Experiments have shown that vanadium-silicon zeolites have good catalytic performance in many organic oxidation reactions. It shows good catalytic performance in redox reaction, especially shows good reaction selectivity, and has good application prospect. [0003] Vanadium can be introduced into silicalite by impregnation or ion exchange, for example, F.Cavani and F.Trifiro (Zeolites, 1988, Vol 8, January) reported the use of NH 4 VO 3 Vanadium-containing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/00
Inventor 林民焦永东朱斌郑金玉汝迎春刘郁东舒兴田宗保宁罗一斌
Owner CHINA PETROLEUM & CHEM CORP
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