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Method for synthesizing low silica-alumina ratio beta zeolite

A technology with a low silicon-aluminum ratio and a synthetic method, which is applied in the field of synthesis of zeolite beta, can solve problems such as unseen synthesis, and achieve the effects of improving activity and activity stability, reducing diffusion resistance, and good repeatability

Active Publication Date: 2008-06-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] So far, there is no report on the synthesis of beta zeolite with low silicon-aluminum ratio and mesoporous structure

Method used

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  • Method for synthesizing low silica-alumina ratio beta zeolite
  • Method for synthesizing low silica-alumina ratio beta zeolite
  • Method for synthesizing low silica-alumina ratio beta zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 125ml of sodium metaaluminate solution (sodium oxide 139.5g / L, aluminum oxide 100.0g / L) and tetraethylammonium hydroxide (2.03N, Daxing Xingfu Fine Chemical Research Institute) 340ml into deionized water, stir well, Make a working solution, mix zeolite beta 500g in Comparative Example 1 with the above-mentioned working solution, make the surface of the solid particle wetted by the working solution, and obtain a reaction mixture, wherein the molar ratio of each component in the synthesis system SiO 2 / Al 2 o 3 =15,Na 2O / SiO 2 =0.06, TEAOH / SiO 2 =0.09,H 2 O / SiO 2 =6.5, then the reaction mixture was crystallized in a high-pressure reactor at 150° C. for 24 hours, and the solid product was separated after cooling to room temperature, washed and dried.

[0034] XRD crystal phase diagram as image 3 As shown, the relative crystallinity is 109.5%. Figure 10 for 27 Al MAS NMR spectrogram, this spectrogram result shows, this product has no non-skeleton aluminum, ...

Embodiment 2

[0037] Add 262ml of sodium metaaluminate solution (sodium oxide 139.5g / L, aluminum oxide 100.0g / L) and tetraethylammonium hydroxide (2.03N, Daxing Xingfu Institute of Fine Chemical Industry) 340ml into deionized water, stir well, Make a working solution, mix zeolite beta 500g in Comparative Example 1 with the above-mentioned working solution, make the surface of the solid particle wetted by the working solution, and obtain a reaction mixture, wherein the molar ratio of each component in the synthesis system SiO 2 / Al 2 o 3 =10, Na 2 O / SiO 2 =0.06, TEAOH / SiO 2 =0.09,H 2 O / SiO 2 =6.5, then the reaction mixture was crystallized in a high-pressure reactor at 150° C. for 24 hours, and the solid product was separated after cooling to room temperature, washed and dried.

[0038] Its XRD such as image 3 As shown, the relative crystallinity is 95.4%. 29 Si MAS NMR determined that its skeleton silicon aluminum ratio was 8.62.

Embodiment 3-8

[0040] Add sodium metaaluminate solution and tetraethylammonium hydroxide into deionized water, stir evenly to make a working solution, mix the β zeolite in Comparative Example 1 with the above working solution, and make the surface of the solid particles moistened by the working solution wet to obtain a reaction mixture, and then transferred to a crystallization tank for crystallization. The raw material composition, crystallization conditions and results are shown in Table 1.

[0041] Table 1

[0042] serial number

[0043] The result shows that the present invention provides the zeolite beta synthesized by the method, and the silicon-aluminum ratio of the sample is close to the feed ratio.

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Abstract

The invention discloses a method for compounding Beta zeolite with a low Si / Al ratio, which comprises the following steps: reaction mixture which is formed by mixing the Beta zeolite with a Si / Al molar ratio of 25 to 30 with aluminum source, positive ion source of tetraethylammonium and water, is crystallized for 0.5 to 2 days in a water temperature of 135 to 170 DEG C; wherein, the molar ratio of the reaction mixture is SiO2A12O3=4-15, TEAOH / SiO2=0 to 0.10, H2OSiO2=5.0 to 8.0.The Beta zeolite compounded by the method is characterized in that framework Si / Al ratio is 4 to 15, acid central density of the Beta zeolite is increased, thereby increasing activity and stability of the catalyst in a high space velocity.

Description

technical field [0001] The present invention relates to a synthesis method of zeolite, and more particularly relates to a synthesis method of beta zeolite with a low silicon-aluminum ratio. Background technique [0002] Beta zeolite was synthesized for the first time by the American Mobile Company in 1967 by the classic hydrothermal crystallization method (USP3308069). This zeolite is the only high-silica zeolite with a three-dimensional twelve-membered ring channel structure. Due to its unique topology and good thermal and hydrothermal stability, β zeolite can be used in alkylation, hydrocracking, hydroisomerization, and hydrogenation. Hydrogen refining, hydrocarbon cracking and other aspects have shown excellent catalytic performance, which has increasingly attracted people's attention. [0003] The acidity and pore structure of molecular sieves are important parameters of catalysts and play a decisive role in catalytic reactions. Therefore, controlling the acidity and po...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 贾晓梅慕旭宏王永睿舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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