Preparation method for small-crystal-grain Y molecular sieve with high specific surface area and high silicon-aluminium ratio

A technology with high silicon-aluminum ratio and high specific surface area is applied in the field of molecular sieves and achieves the effects of good industrial application prospect, simple preparation method, good hydrothermal stability and catalytic activity

Inactive Publication Date: 2014-12-24
天津神能科技有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

The document {Chem.J.Chinese Universities (Chemical Journal of Universities) [J], 2007, 28(9):1634~1636) reported the synthesis of Y-type zeolite with a silicon-aluminum ratio of nearly 6 by high-temperature crystallization using a directing agent as a silicon source. , this method proposes a new idea for the synthesis of high silicon Y, but the particle size of the synthesized product is about 1000nm

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  • Preparation method for small-crystal-grain Y molecular sieve with high specific surface area and high silicon-aluminium ratio

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take water glass 47.20g (specific gravity 1.259, SiO 2 Content 250.5g / L, modulus 3.21) into a three-necked bottle, add sodium metaaluminate (Al 2 o 3 Content 2.9534mol / L,Na 2 (05.0000mol / L) 2.65ml, NaOH solid (produced by Tianjin Chemical Factory, purity 96%) 4.60g, water 10g, after mixing evenly, stir vigorously at room temperature (30°C) for 12h to obtain the desired transparent gel guide Agent, its molar ratio is Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=16:1:20:360.

[0026] NaY is synthesized according to Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=2.73:1:8.4:209 ratio synthesis: put 30.7448g of water glass in a three-neck flask, control the temperature in the flask to 60°C, add 7.0002g of sodium metaaluminate and aluminum sulfate (Al 2 (SO4) 3 Specific gravity 1.273Al 2 o 3 89.6g / L) 10.5565g and water 8.384g, directing agent 6g, stir evenly, aging for 6h, then add water glass 2.4107g, NaOH solution (3.4275mol / L) 0.15ml, make the feeding ratio become Na 2 O: Al 2 o 3 ...

Embodiment 2

[0028] Raw material and directing agent are identical with embodiment 1.

[0029] NaY is synthesized according to Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=2.73:1:8.4:209 Proportion Synthesis: Place 30.7448g of water glass in a three-neck flask, control the temperature in the flask to 80°C, add 7.0002g of sodium metaaluminate and aluminum sulfate (Al 2 (SO4) 3 Specific gravity 1.273Al 2 o 3 89.6g / L) 10.5565g and water 8.384g, directing agent 3.85g, stir evenly, aging for 4h, then add water glass 2.4107g, NaOH solution (3.4275mol / L) 0.15ml, make the feeding ratio become Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=2.93:1:9.0:217 Vigorously stir evenly, then raise the temperature to 120°C for dynamic crystallization for 10h, add raw material water glass 8.0356g, NaOH solution 1.8215ml and H 2 O3.2875g, make final gel proportioning be Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=3.73:1:11:258. Continue static crystallization at 120°C for 25h, then filter, wash, and dry to obtain NaY molecular sieve...

Embodiment 3

[0031] Take water glass 43.08g (specific gravity 1.259, SiO 2 Content 250.5g / L, modulus 3.21) into a three-necked bottle, add sodium metaaluminate (Al 2 o 3 Content 2.9534mol / L,Na 2 (05.0000mol / L) 4.79ml, NaOH solid (produced by Tianjin Chemical Factory, purity 96%) 9.770g, water 9.70g, after mixing evenly, stir vigorously at room temperature (30°C) for 12h to obtain the required transparent gel Directing agent, its molar ratio is Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=13:1:10:180.

[0032] NaY is synthesized according to Na 2 O: Al 2 o 3 :SiO2 2 :H 2 O=1:1:5:180 ratio synthesis: put 24.90g of water glass in a three-neck flask, control the temperature in the flask to 80°C, add 2.52ml of sodium metaaluminate, aluminum sulfate (Al 2 (SO4) 3 Specific gravity 1.273Al 2 o 3 89.6g / L) 14.00g and water 24g, guiding agent 6.0g, stir evenly, aging for 4h, then add water glass 11.10g, aluminum sulfate (Al 2 (SO4) 3 Specific gravity 1.273Al 2 o 3 89.6g / L) 5.00g. Change the f...

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Abstract

A provided preparation method for a small-crystal-grain Y molecular sieve with high specific surface area and high silicon-aluminium ratio comprises the concrete synthetic steps: firstly aging at 15-60 DEG C for 0.5-48 h to prepare a high-silicon crystallization guiding agent; then utilizing a silicon source, an aluminium source, an alkali source, water and the guiding agent and employing a segmented three-step method to prepare a finale crystallized mixture, standing and crystallizing at a certain temperature for a certain period, and performing filtering, washing and drying on the product to prepare the small-crystal-grain Y molecular sieve with high specific surface area, high silicon-aluminium ratio and the relative crystallization degree larger than 85%. The product prepared by utilizing the method has good hydro-thermal stability and catalytic activity. The product is obtained by employing a template-free direct synthesis method, the preparation method is simple, the raw materials are easy to obtain, environment pollution does not exist, and good industrial application prospect is provided.

Description

technical field [0001] The invention relates to the field of molecular sieves, in particular to a method for preparing a Y molecular sieve with high specific surface area, high silicon-aluminum ratio and small grain size. Background technique [0002] Y-type molecular sieves with a faujasite crystal structure are widely used in catalytic cracking and other chemical reactions as catalyst active components or catalyst supports. Due to the constraints of chemical conditions in the synthesis process, the NaY molecular sieve produced in conventional industry currently has a skeleton silicon-aluminum ratio of about 5.0, and generally has a grain size of about 1000nm. Because the directly synthesized NaY molecular sieve framework has a low silicon-aluminum ratio and poor stability, it is difficult to adapt to the harsh reaction and aging conditions of the FCC device. At the same time, due to its high intracrystalline diffusion rate and external specific surface area, the molecular...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/24
Inventor 袁忠勇王震宇李晓文王宝义
Owner 天津神能科技有限公司
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