Process of preparing ZSM-5 molecular sieve of nano size and containing hetero atom

A nano-sized, ZSM-5 technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high toxicity of template agents, non-nano-sized, single synthesis conditions, etc. , to achieve the effect of controllable grain size, large crystallinity and uniform grain size

Inactive Publication Date: 2005-04-27
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystallite size of the heteroatom molecular sieves synthesized according to these documents belongs to the micron range and does not have a nanometer size
It can be seen that the methods for synthesizing

Method used

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  • Process of preparing ZSM-5 molecular sieve of nano size and containing hetero atom
  • Process of preparing ZSM-5 molecular sieve of nano size and containing hetero atom
  • Process of preparing ZSM-5 molecular sieve of nano size and containing hetero atom

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Mix the required amount of sodium hydroxide, sodium chloride, distilled water, aluminum sulfate and 22% tetrapropylammonium hydroxide solution evenly at room temperature, stir for 15 minutes and the mixed solution becomes clear, then add the required amount of concentration Add 25% silica sol dropwise to the above solution, stir for 30 minutes, put the above solution into a stainless steel reaction kettle, seal it and move it into an oven for static crystallization for 6 days, the crystallization temperature is 120°C. The relative molar content of each component in the reaction gel is: SiO 2 / Al 2 o 3 =65, NaOH / Al 2 o 3 =14, NaCl / Al 2 o 3 =130,H 2 O / Al 2 o 3 =2000,TPAOH / Al 2 o 3 =6, the product was suction filtered, washed, and dried at 120°C to obtain nanometer-sized ZSM-5 molecular sieves. The product is determined by XRD diffraction to be an MFI molecular sieve with a relative crystallinity of 90%, an average grain size of 40nm, and a specific surface area...

Embodiment 2

[0016] Mix the required amount of sodium hydroxide, sodium citrate, distilled water, sodium metaaluminate and 22% tetrapropylammonium hydroxide solution evenly at room temperature, stir for 15 minutes and the mixed solution becomes clear, then add the required amount Add white carbon black with a concentration of 85% dropwise to the above solution, stir for 30 minutes, put the above solution into a stainless steel reaction kettle, seal it and move it into an oven for static crystallization for 10 days, the crystallization temperature is 80°C . The relative molar content of each component in the reaction gel is: SiO 2 / Al 2 o 3 =85, NaOH / Al 2 o 3 =24, Na 3 C 6 h 5 o 7 / Al 2 o 3 =40,H 2 O / Al 2 o 3 =4000,TPAOH / Al 2 o 3 =15, the product was suction filtered, washed, and dried at 120°C to obtain nanometer-sized ZSM-5 molecular sieves. The product is determined by XRD diffraction to be an MFI structure molecular sieve, with a relative crystallinity of 90%, an average...

Embodiment 3

[0018] Mix the required amount of sodium hydroxide, sodium carbonate, distilled water, aluminum sulfate and tetrapropylammonium bromide uniformly at room temperature, and after stirring for 15 minutes, the mixed solution becomes clear, and then add the required amount of white carbon black with a concentration of 25%. Add it dropwise to the above solution, stir for 30 minutes, then put the above solution into a stainless steel stirring reaction kettle, seal it, stir and crystallize for 3 days, and the crystallization temperature is 110°C. The relative molar content of each component in the reaction gel is: SiO 2 / Al 2 o 3 =85, NaOH / Al 2 o 3 = 4, Na 2 CO 3 / Al 2 o 3 =55,H 2 O / Al 2 o 3 =10000, TPABr / Al 2 o 3 =20, the product was suction filtered, washed, and dried at 120°C to obtain nanometer-sized ZSM-5 molecular sieves. The product is determined by XRD diffraction to be an MFI molecular sieve with a relative crystallinity of 97%, an average grain size of 60nm, and...

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Abstract

The preparation process of ZSM-5 molecular sieve of nanometer size and containing hetero atom includes adding alkali metal salt; adding additive, template agent, one of Al and hetero atoms in certain order and at 60-120 deg.c for mixing with Si source; and crystallization statically or under stirring for 1-15 days. The molecular sieve has crystal grain size of 40-200 nm, and specific surface area of 300-600 sq m/g. The present invention has the advantages of optional static or dynamic synthesizing condition, no-toxic operation, controllable crystal grain size and skeleton hetero atom, various kinds of metal atom, low crystallization temperature and simple operation. The present invention provides some optional materials for developing catalyst with industrial application foreground and has great application value.

Description

technical field [0001] The invention relates to a method for preparing nanometer-sized heteroatom-containing ZSM-5 molecular sieves, belonging to the technical field of molecular sieve synthesis. Background technique [0002] Because of its unique pore / cage structure, ion exchange performance and potential acid performance, molecular sieves are extremely important in the hydrocarbon processing industry as catalyst active components or catalyst supports. Compared with large-grain molecular sieves, small-grain molecular sieves have many advantages, mainly in: (1) having a larger outer surface area and more active centers on the outer surface, which is conducive to the catalytic conversion of macromolecular reactants; ( 2) It has a higher intragranular diffusion rate, which is beneficial to make full use of the active sites on the inner surface to reduce the occurrence of side reactions; (3) has more pore entrances and exits, which is conducive to impr...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 程志林杨建国张欢燕何鸣元
Owner EAST CHINA NORMAL UNIVERSITY
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