Method for fast synthesizing ZSM-5 molecular sieves

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of increasing the cost of molecular sieve, consumption of organic template agents, environmental pollution, etc., and achieve crystallization The effect of good degree, low cost and low pollution

Inactive Publication Date: 2012-09-19
KAILUAN ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At present, the existing ZSM-5 molecular sieve synthesis method generally takes 2 to 7 days, which is a long time; in addition, a large amount of o

Method used

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  • Method for fast synthesizing ZSM-5 molecular sieves
  • Method for fast synthesizing ZSM-5 molecular sieves
  • Method for fast synthesizing ZSM-5 molecular sieves

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0030] Example 1: The method for rapidly synthesizing ZSM-5 molecular sieve adopts the following process steps.

[0031] (1) First, 0.61g aluminum isopropoxide, 16.09g deionized water and 0.20g NaOH are mixed to form solution A, then 12.48g ethyl orthosilicate and 9.75g tetrapropylammonium hydroxide solution (25%wt Solution) mixed to form solution B (where SiO 2 / Al 2 O 3 , OH - / SiO 2 , R / SiO 2 And H 2 O / SiO 2 The molar ratio of the sol-gel is 40, 0.28, 0.2 and 21.7), the solution B is dropped into the solution A under vigorous stirring to obtain a uniformly mixed sol-gel, and the mixture is stirred and aged for 4h at room temperature.

[0032] (2) Take out the aged sol-gel and put it in an oven at 80°C for 2.5 hours and grind it into a powdery dry glue powder.

[0033] (3) Put the dry glue powder into a stainless steel crystallization kettle with PTFE lining, add water, and crystallize at 150℃ for 24h.

[0034] (4) The precipitate (crystallized product) is washed to neutrality by ce...

Example Embodiment

[0035] Example 2: The method for rapidly synthesizing ZSM-5 molecular sieve adopts the following process steps.

[0036] (1) First mix 1.50g aluminum nitrate, 34.94g deionized water and 1.20g NaOH to form solution A, then mix 12.48g ethyl orthosilicate, 10g deionized water and 4.88g tetrapropylammonium hydroxide solution (25 %wt aqueous solution) mixed to form solution B (where SiO 2 / Al 2 O 3 , OH - / SiO 2 , R / SiO 2 And H 2 O / SiO 2 The molar ratio of the solution B is 30, 0.6, 0.1 and 45), the solution B is dropped into the solution A under vigorous stirring to obtain a uniformly mixed sol-gel, and the mixture is stirred and aged for 4 hours at room temperature.

[0037] (2) Take out the aged sol-gel and put it in an oven at 70°C for 3 hours and grind it into a powdery dry glue powder.

[0038] (3) Put the dry glue powder into a stainless steel crystallization kettle with PTFE lining, add water, and crystallize at 150℃ for 24h.

[0039] (4) The precipitate (crystallized product) is w...

Example Embodiment

[0040] Example 3: The method for rapidly synthesizing ZSM-5 molecular sieve adopts the following process steps.

[0041] (1) First mix 0.82g aluminum isopropoxide, 17.78g deionized water and 0.80g NaOH to form solution A, then mix 24.96g ethyl orthosilicate and 19.50g tetrapropylammonium hydroxide solution (25%wt Aqueous solution) mixed to form solution B (where SiO 2 / Al 2 O 3 , OH - / SiO 2 , R / SiO 2 And H 2 O / SiO 2 The molar ratio of the solution B is 60, 0.37, 0.2 and 15). Under vigorous stirring, drop solution B into solution A to obtain a uniformly mixed sol-gel, and stir and age at room temperature for 4 hours.

[0042] (2) Take out the aged sol-gel and put it in an oven at 80°C for 2h, and grind it into a powdery dry glue powder.

[0043] (3) Put the dry glue powder into a stainless steel crystallization kettle with PTFE lining, add water, and crystallize at 160℃ for 20h.

[0044] (4) The precipitate (crystallized product) is washed to neutrality by centrifugation and dried at ...

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Abstract

The invention discloses a method for fast synthesizing ZSM-5 molecular sieves. The method comprises the synthesis steps that (1) firstly, aluminum sources, silicon sources, template agents, water and alkali are uniformly mixed according to the following mol ratios: SiO2/Al2O3 equals to 10 to 60, OH<->/SiO2 equals to 0.1 to 0.8, R/SiO2 equals to 0 to 0.2, and H2O/SiO2 equals to 10 to 200, then, the stirring aging is carried out for 2 to 4 hours, and aged sol-gel is obtained, wherein R is template agents; (2) the aged sol-gel is baked into dry glue under the condition being 60 to 90 DEG C, and then, the dry glue is ground into powder dry glue powder; (3) the dry glue powder is placed into a reaction kettle with a polytetrafluoroethylene inner liner, water is added, and the static crystallization is carried out for 12 to 40 hours under the condition being 150 to 180 DEG C; (4) the crystallization products are taken out to be washed by water and baked, then, the temperature is raised to 450 to 650 DEG C, and the products are roasted for 4 to 6 hours to obtain the ZSM-5 molecular sieves. The method has the advantages that the supersaturation degree of the sol-gel system can be enhanced when the sol-gel is baked into dry glue so that the system fast forms crystal nucleus, and the ZSM-5 zeolite molecular sieves are fast synthesized. The method has the characteristics that the simplicity is realized, the time is saved, the cost is low, and the pollution is low.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, in particular to a method for quickly synthesizing ZSM-5 molecular sieves. Background technique [0002] After the 1970s, with the in-depth research on type-selective catalysis, Mobil Corporation developed the ZSM series of high-silica zeolites. The high silicon-aluminum ratio of ZSM series high-silica zeolites makes them have ideal acid resistance, alkali resistance and hydrothermal stability, and their unique crystal structure makes them have a uniform pore system. The ZSM-5 zeolite is its outstanding representative. Its skeleton structure is characterized by the formation of five-silicon chains parallel to the c-axis by 8 five-membered rings through common edges, and then the mirror-symmetric connection of the five-silicon chains to obtain ten-membered ring holes. The wavy network layer, and finally the network layer is further connected to form a three-dimensional cross-channel s...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 房承宣王亚涛于泳彭胜
Owner KAILUAN ENERGY CHEM
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