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Synthesis method for ZSM-11 molecular sieve with nano multi-stage pores

A technology for ZSM-11 and synthesis methods, applied in the direction of molecular sieves and base exchange compounds, nanotechnology, chemical instruments and methods, etc., can solve the problems of increasing the synthesis cost of ZSM-11 molecular sieves, increasing synthesis costs, unfavorable industrial applications, etc., to achieve Enrich micropores and mesoporous channels, reduce waste liquid discharge, and have good hydrothermal stability

Active Publication Date: 2017-02-22
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) Most of the synthetic raw materials use expensive chemical reagents, which greatly increases the synthesis cost of ZSM-11 molecular sieve, which is not conducive to large-scale industrial application
[0007] (2) The post-treatment of hydrothermal synthesis needs to be filtered, and the crystallization product can only be obtained after the crystallization wastewater is filtered out, resulting in a large amount of wastewater pollution
[0008] (3) The preparation of nano-hierarchical ZSM-11 is not only cumbersome, but the yield is low, and it is necessary to add a mesoporous directing agent, which greatly increases the synthesis cost

Method used

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  • Synthesis method for ZSM-11 molecular sieve with nano multi-stage pores
  • Synthesis method for ZSM-11 molecular sieve with nano multi-stage pores
  • Synthesis method for ZSM-11 molecular sieve with nano multi-stage pores

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The synthesis of embodiment 1 ZSM-11 molecular sieve

[0059] (1) Roast 40 g of kaolin at 850° C. for 1 h to obtain roasted kaolin, mix the roasted kaolin with 200 mL of hydrochloric acid solution with a concentration of 6 mol / L (liquid-solid ratio is 5 mL / g), then heat and stir at 90° C. for 6 h, Afterwards, filter cake was obtained by filtration, and the filter cake was dried at 100° C. for 6 hours to obtain modified kaolin. The active silica content in the modified kaolin was determined to be 96.37%, and the active alumina content was 2.28%.

[0060] (2) Add 12.68g of white carbon black, 18.88g of tetrabutylammonium hydroxide (TBAOH) solution (40%, mass concentration), 66.86g of deionized water, 0.89g of sodium hydroxide, 34.23g of ethanol and 10.00g of g modified kaolin, the molar ratio of each raw material in the slurry after mixing is as follows: 1SiO 2 :0.006Al 2 o 3 :0.03Na 2 O:0.1TBAOH:10H 2 O:2EtOH. It is calculated that the active silicon oxide in the ...

Embodiment 2

[0064] The synthesis of embodiment 2 ZSM-11 molecular sieves

[0065] (1) Roast 60 g of kaolin at 750° C. for 3 h to obtain roasted kaolin, mix the roasted kaolin with 480 mL of nitric acid solution with a concentration of 6 mol / L (liquid-solid ratio is 8 mL / g), then heat and stir at 80° C. for 3 h, Afterwards, filter cake was obtained by filtration, and the filter cake was dried at 120° C. for 12 hours to obtain modified kaolin. The active silica content in the modified kaolin was determined to be 95.26%, and the active alumina content was 3.66%.

[0066] (2) Add 13.47g ethyl orthosilicate, 29.78g tetrabutylphosphorus hydroxide (TBPOH) solution (40%, mass concentration), 193.83g deionized water, 0.86g sodium hydroxide and 30.00g modified kaolin, the molar ratio of each raw material in the slurry after mixing evenly is as follows: 1SiO 2 :0.02Al 2 o 3 :0.02Na 2 O:0.08TBPOH:20H 2 O. It is calculated that the active silicon oxide in the above-mentioned modified kaolin acc...

Embodiment 3

[0070] The synthesis of embodiment 3 ZSM-11 molecular sieves

[0071] (1) Roast 30 g of kaolin at 900° C. for 4 h to obtain roasted kaolin, mix the roasted kaolin with 180 ml of hydrochloric acid solution with a concentration of 8 mol / L (liquid-solid ratio is 6 mL / g), then heat and stir at 90° C. for 2 h, Afterwards, filter cake was obtained by filtration, and the filter cake was dried at 120° C. for 24 hours to obtain modified kaolin. The active silica content in the modified kaolin was determined to be 90.31%, and the active alumina content was 6.13%.

[0072] (2) 30.57g of tetrabutylammonium hydroxide (TBAOH) solution (40%, mass concentration), 54.11g of deionized water, 55.40g of ethanol and 20.00g of modified kaolin were added successively under stirring, and each raw material in the slurry was mixed uniformly The molar ratio is as follows: 1SiO 2 :0.04Al 2 o 3 :0.2TBAOH:10H 2 O:4EtOH. It is calculated that the active silicon oxide in the above-mentioned modified ka...

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Abstract

The invention discloses a synthesis method for a ZSM-11 molecular sieve with nano multi-stage pores. The synthesis method comprises the following steps of (1) carrying out acid treatment on calcined kaolin to obtain modified kaolin; (2) mixing the modified kaolin with an additional silicon source, an organic template agent, inorganic base, alcohol and water and stirring uniformly; (3) drying slurry prepared in the step (2) to form xerogel; and (4) crystallizing the xerogel under the assistance of water vapor, calcining crystallization products obtained at high temperature to obtain the ZSM-11 molecular sieve. The synthesis method disclosed by the invention has the advantages that the ZSM-11 molecular sieve with the nano multi-stage pores is high in degree of crystallinity, small in grain and good in hydrothermal stability, and has large specific surface area and rich microporous and mesoporous channels; simultaneously, the synthesis cost of the ZSM-11 molecular sieve is greatly reduced, and a product does not need to be filtered, so that the environment-friendly effect in the synthesis process is obviously improved.

Description

technical field [0001] The invention belongs to the field of synthesis of molecular sieves, and in particular relates to a synthesis method of nanometer hierarchical porous ZSM-11 molecular sieves. Background technique [0002] ZSM-11 molecular sieve is a new structure molecular sieve first developed by Mobil in the early 1970s. ZSM-11 belongs to the MEL structure configuration and belongs to the Pentasil type molecular sieve, which has a very unique lattice structure, and the ratio of silicon to aluminum in the crystal structure is high. The surface of its crystal has obvious hydrophobic effect and strong surface acidity. It is an important adsorbent and a good shape-selective catalyst. It has excellent performance in heavy oil catalytic cracking, methanol conversion to gasoline, hydrocracking and catalytic dewaxing reactions. catalytic performance. [0003] In recent years, the research on the catalytic performance of ZSM-11 molecular sieve has become increasingly active...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36B82Y40/00
CPCC01B39/365C01P2002/72C01P2004/03C01P2004/61C01P2006/12C01P2006/14C01P2006/80
Inventor 朱学栋魏振浩邢蓝吁闻振浩何暄杨帆徐亚荣
Owner PETROCHINA CO LTD
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