Synthesis method of high-silicon b-oriented ZSM-5 nanosheets

A synthesis method, the technology of ZSM-5, applied in the directions of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of complex synthesis process, high synthesis cost, high cost and the like, and achieve synthesis High yield, strong hydrothermal stability, and the effect of reducing preparation costs

Inactive Publication Date: 2016-12-07
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Yingcai Long etc. (Micopor. Mesopor.Materials, 2006,95,234 and CN 1332114A), reported in the patent literature using dual-mode agent and the method of adding BETA seed crystals, can obtain the high-silicon MOR zeolite of b-axis orientation, but this This synthesis method needs to use two kinds of templates, the synthesis cost is expensive, and the obtained particles are also very thick strip-shaped MOR zeolite, and fluoride ions need to be added in the synthesis system, the synthesis process is complicated
[0005] The b-axis oriented high-silica zeolite prepared in the prior art requires the use of two templates, and the addition of fluoride ions to the synthesis system. The synthesis process is complex and expensive, and the obtained particles are also very thick long strip crystal grains.

Method used

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  • Synthesis method of high-silicon b-oriented ZSM-5 nanosheets
  • Synthesis method of high-silicon b-oriented ZSM-5 nanosheets

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Dissolve 0.03 g of ammonia water, 0.08 g of potassium chloride and 0.16 g of sodium metaaluminate in 25 ml of pure water, stir to clarify, add 20 g of silica sol with a concentration of 20 wt% dropwise under stirring, and stir the resulting solution for 20 minutes It is a silica-alumina sol-gel solution. Add 1.5 g of octylamine template dropwise to the above-prepared silica-alumina sol-gel solution, stir for 30 minutes, then add dropwise 0.2 g of silicate-1 seed solution with a concentration of 5wt%, and stir for 30 minutes to obtain a solution as a precursor solution. Mix the prepared precursor solution with 50ml polytetrafluoroethylene fluoride at 180 o C for 30 hours of crystallization reaction, washing and drying after the reaction to obtain high-silicon b-oriented ZSM-5 nanosheet zeolite.

[0013] See attached figure 1 , the product obtained in Example 1 was measured by XRD characterization, and its crystal phase only had characteristic X-ray diffraction peaks a...

Embodiment 2

[0016] Dissolve 0.02 g of ammonia water, 0.08 g of potassium chloride and 0.16 g of sodium metaaluminate in 20 ml of pure water, stir to clarify, then add 20 g of silica sol solution with a concentration of 20wt% dropwise under stirring, and stir the resulting solution for 20 minutes It is a silica-alumina sol-gel solution. Add 4.8g of octylamine template dropwise to the silica-alumina sol-gel solution prepared above, stir for 30 minutes, then add 0.2 g of 5wt% silicate-1 seed solution dropwise, and stir for 25 minutes to obtain the precursor solution . Mix the prepared precursor solution with 50 ml of polytetrafluoroethylene fluoride at 180 o The crystallization reaction was carried out at the temperature of C for 25 hours, and after the reaction was completed, it was washed and dried to obtain a high-silicon b-oriented ZSM-5 nanosheet zeolite.

Embodiment 3

[0018] Dissolve 0.05 g of ammonia water, 0.05 g of sodium chloride and 0.1 g of sodium metaaluminate in 50 ml of water, stir to clarify, then add dropwise 20 g of a silica sol solution with a concentration of 20 wt% under stirring, and stir for 20 minutes to obtain a solution that is silicon Aluminum sol gel solution. Add 2 g of hexylamine template dropwise to the above-prepared silica-alumina sol-gel solution, stir for 30 minutes, then add dropwise 0.2 g of 5 wt% silicate-1 seed solution, and stir for 25 minutes to obtain the precursor solution . Mix the prepared precursor solution with 50ml polytetrafluoroethylene fluoride at 180 o C crystallization reaction at temperature C for 30 hours, washing and drying after the reaction to obtain high-silicon b-oriented ZSM-5 nanosheet zeolite.

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Abstract

The invention discloses a synthesis method of high-silicon b-oriented ZSM-5 nanosheets. The method is characterized by comprising the following steps: mixing an aluminum source with ammonia water, inorganic salts and water, stirring, slowly and dropwisely adding a silicon source, adding a template and a crystal seed at a uniform speed, and carrying out crystallization reaction at 120-190 DEG C for 24-48 hours; and after the reaction finishes, filtering, and drying to obtain the high-silicon b-oriented ZSM-5 nanosheets. Compared with the prior art, the ZSM-5 nanosheets have the advantages of high activity, ultrathin crystal grains, high silicon b-orientation, adjustable silica-alumina ratio, controllable thickness, perfect crystals and high hydrothermal stability, well overcome the defect that the preparation of the nanosheet zeolite catalyst requires the use of the specific-structure high-price structure guide agent or secondary template, have the characteristics of lower preparation cost and high synthesis yield, and have certain industrialized application prospects and obvious economic value.

Description

technical field [0001] The invention relates to the technical field of zeolite molecular sieve synthesis, in particular to a method for synthesizing high-silicon b-orientation ZSM-5 nanosheets. Background technique [0002] Mobil Corporation of the United States first reported the synthesis of ZSM-5 molecular sieve in 1972 (USP3702886). Due to the unique intersecting pore structure, high hydrothermal stability and shape selectivity, adjustable silicon-aluminum ratio, and strong acidity, MFI zeolite has gradually developed into the preferred catalytic material in the field of petrochemical industry. It is widely used in ether to propylene, alkylation reaction, methanol conversion to gasoline, toluene disproportionation and other devices. In recent years, the preparation of hierarchically porous ZSM-5 molecular sieves with nanosheet structure has become one of the hotspots in the field of catalytic materials research. In the prior art, Ryong Ryoo et al. (J. Am.Chem. Soc., 20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2004/03C01P2004/20
Inventor 陈丽丁键施宗波吴海虹何鸣元
Owner EAST CHINA NORMAL UNIV
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