Method for preparing mesoporous WO3/SBA-15 molecular sieve

A technology of molecular sieve and mesoporous, which is applied in the field of preparation of mesoporous WO3/SBA-15 molecular sieve, to achieve the effect of improving olefin disproportionation reaction performance, good technical effect and increasing specific surface area

Active Publication Date: 2008-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] So far, there is no report on using mesoporous WO3 / SBA-15 molecular sieve as olefin disproportionation catalyst

Method used

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  • Method for preparing mesoporous WO3/SBA-15 molecular sieve
  • Method for preparing mesoporous WO3/SBA-15 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of all-silicon SBA-15

[0025] With electromagnetic stirring, weigh 60 ml of concentrated hydrochloric acid (concentration 38%) and dissolve it in 312 ml of deionized water, and keep the temperature in a water bath at 40°C. Then add 12 grams of polyethylene glycol-polypropylene glycol-polyethylene glycol triblock polymer (Aldrich, molecular formula is H(-OCH 2 -CH 2 -) x [-OCH(CH 3 )CH 2 -] y (OCH 2 CH 2 -) z OH, the molar ratio of x:y:z is 20:70:20, the average molecular weight is 5800, referred to as P123), and stirred at constant temperature for 4 hours to obtain solution A. 25.6 g of tetraethyl orthosilicate (TEOS) was slowly added dropwise to A, and vigorously stirred at 40° C. for 24 hours to obtain milky white suspension B. The gel was transferred to a 200 ml autoclave with a Teflon liner and subjected to static crystallization at 95°C for 3 days. Filter, wash with deionized water three times, and bake in an oven at 120°C for 24 hours. The ob...

Embodiment 2～5

[0027] Synthetic samples S1, S2, S3 and S4

[0028] With electromagnetic stirring, weigh 60 ml of concentrated hydrochloric acid (concentration 38%) and dissolve it in 312 ml of deionized water, and keep the temperature in a water bath at 40°C. Then add 12 grams of polyethylene glycol-polypropylene glycol-polyethylene glycol triblock polymer P123 (Aldrich, molecular formula is H(-OCH 2 -CH 2 -) x [-OCH(CH 3 )CH 2 -] y (OCH 2 CH 2 -) z OH, the molar ratio of x:y:z is 20:70:20, and the average molecular weight is 5800) and 30 grams of polyethylene glycol-polypropylene glycol-polyethylene glycol triblock polymer F127 (Aldrich, molecular formula is H( -OCH 2 -CH 2 -) x [-OCH(CH 3 )CH 2 -] y (OCH 2 CH 2 -) zOH, the molar ratio of x:y:z is 106:70:106, and the average molecular weight is 14600), stirred at constant temperature for 4 hours to obtain solutions A and B. 25.6 grams of tetraethyl orthosilicate (TEOS) were slowly added dropwise to A and B respectively to ...

Embodiment 6～7

[0030] Synthetic samples S5 and S6

[0031] With electromagnetic stirring, weigh 300 ml of concentrated nitric acid (concentration 2 mol / L) and dissolve in 100 ml of deionized water, and keep the temperature in a water bath at 40°C. Then respectively add 12 grams of polyethylene glycol-polypropylene glycol-polyethylene glycol triblock polymer P123 (Aldrich, molecular formula is H(-OCH 2 -CH 2 -) x [-OCH(CH 3 )CH 2 -] y (OCH 2 CH 2 -) z OH, the molar ratio of x:y:z is 20:70:20, and the average molecular weight is 5800), stirred at constant temperature for 4 hours, slowly added dropwise 25.6 grams of tetraethyl orthosilicate (TEOS) and stirred at 40°C for 10 minutes; Add 5 ml of aqueous solutions containing 1.43 g of sodium tungstate and 5 ml of 1.18 g of sodium metatungstate dropwise, and stir vigorously at 40°C for 24 hours to obtain solutions G and H; transfer G and H to 200 ml Static crystallization at 80°C for 50 hours in an autoclave with a Teflon liner. Filter, ...

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Abstract

The invention relates to a preparation method of a meso-porous WO3SBA-15 molecular sieve, which mainly solves the problem of the former art that the synthetization of silica molecular sieve WO3SBA-15 including tungsten in the frame is not related. The invention adopts a three-block polymer of polyethylene-polypropylene glycol-polyethyleneglycol as template agent. Silica source selected from tetraethyl orthosilicate, silica sol, water glass or white carbon black is taken as a silica resource, ammonium metatungstate, ammonium paratungstate, sodium tungstate or tungsten hexachloride is taken as a tungsten source, the mole ratio of the raw materials is as follows: 1SiO2: 0.01 to 0.03M: 3 to 10H<+>:50 to 200H2O:0.03 to 0.25WO3, under the acidic condition, the crystallization temperature is 20 to 170 DEG C, and the WO3SBA-15 molecular sieve is obtained through hydrothermal crystallization for 6 to 120 hours. The invention can be used for the industrial production of olefin disproportionation.

Description

technical field [0001] The present invention relates to a mesoporous WO 3 / The preparation method of SBA-15 molecular sieve. Background technique [0002] Olefin disproportionation is a conversion process of olefins. Olefin disproportionation reaction can be used to convert relatively excess and low value-added olefins into high value-added olefin products. [0003] The key to the olefin disproportionation reaction is the catalyst, which can be a homogeneous catalyst or a heterogeneous catalyst. The heterogeneous olefin disproportionation catalyst is generally W, Mo, Re and other compounds supported on an inert carrier. The inert carrier is generally SiO 2 , Al 2 o 3 ,TiO 2 , SiO 2 -Al 2 o 3 , ZrO 2 Aluminophosphate. [0004] US5300718 has reported the process of producing propylene by disproportionation reaction of butene-2 ​​and ethylene, the catalysts used are MgO and WO 3 / SiO 2 mixed bed. [0005] EP0489585 has proposed the preparation method of butene d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03B01J23/30C07C6/10C07C11/02
CPCY02P20/52
Inventor 杨为民刘俊涛钟思青朱志焱刘红星
Owner CHINA PETROLEUM & CHEM CORP
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