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Quick synthesis method for nano-scale ZSM-5 molecular sieve

A technology of ZSM-5 and synthesis method, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of unfavorable industrial production, expensive raw materials, and long time consumption, and achieve low cost and raw materials. Easy to get, prevent further growth effect

Active Publication Date: 2013-01-16
KAILUAN ENERGY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The existing ZSM-5 molecular sieve synthesis methods either take a long time (2-40 days), or use expensive raw materials (organic templates, tetrapropylammonium hydroxide, etc.), which are not conducive to industrial production

Method used

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  • Quick synthesis method for nano-scale ZSM-5 molecular sieve
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  • Quick synthesis method for nano-scale ZSM-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: The rapid synthesis method of this nano-scale ZSM-5 molecular sieve adopts the following process steps.

[0025] (1) Preparation of dry gel seed crystals: first mix 0.4085g of aluminum isopropoxide, 7.0180g of water and 14.6426g of tetrapropylammonium hydroxide (25%wt) to make solution A, then mix 12.4998g of orthosilicate Ethyl ester was added dropwise into solution A under vigorous stirring to obtain solution B, wherein the molar ratio of aluminum source, silicon source, tetrapropylammonium hydroxide and water was Al 2 o 3 :SiO2 2 :TPAOH:H 2 O=1:60:18:1000; continue to stir solution B until it is uniformly mixed and adjust the pH value to 12.5, then stir and age for 6 hours; then dry the aged sol-gel at 80°C to dry gel, Grinding the dry glue into powdery dry glue powder to obtain dry glue seeds;

[0026] (2) First mix 1.506g of aluminum nitrate (nine water) and 23.4g of water to make solution I, and then mix 53.263g of water glass (SiO 2 Content 27....

Embodiment 2

[0030] Embodiment 2: The rapid synthesis method of this nano-scale ZSM-5 molecular sieve adopts the following process steps.

[0031](1) The preparation method of dry rubber seed crystals is the same as in Example 1 except for the following differences: Stir solution B until it is uniformly mixed and adjust the pH value to 12; stir and age for 4 hours; the aged sol-gel is at 70 ℃ drying into dry glue;

[0032] (2) First mix 1.137g of aluminum chloride (hexahydrate) and 46.8g of water to make solution I, then mix 26.031g of water glass (SiO 2 Content 27.5wt%) was slowly added to solution I under vigorous stirring to obtain solution II, wherein the molar ratio of aluminum source, silicon source and water was Al 2 o 3 :SiO2 2 :H 2 O=1:30:1300; continue to stir solution II until uniformly mixed and adjust the pH value to 12, stirring for 1h;

[0033] (3) Add dry rubber seeds with a final ZSM-5 molecular sieve yield of 5% to the mixed solution, and stir for 1 hour to make it e...

Embodiment 3

[0036] Embodiment 3: The rapid synthesis method of this nano-scale ZSM-5 molecular sieve adopts the following process steps.

[0037] (1) The preparation method of dry rubber seed crystals is the same as in Example 1 except for the following differences: Stir solution B until it is uniformly mixed and adjust the pH value to 13; stir and age for 2 hours; the aged sol-gel is at 60 ℃ drying into dry glue;

[0038] (2) First mix 1.666g of aluminum sulfate (octadecane water) and 38.25g of water to form solution I, then mix 44.386g of water glass (SiO 2 Content 27.5wt%) was slowly added to solution I under vigorous stirring to obtain solution II, wherein the molar ratio of aluminum source, silicon source and water was Al 2 o 3 : 40 SiO 2 : 850H 2 O: Continue to stir solution II until it is evenly mixed and adjust the pH value to 12.5, stirring for 1 hour;

[0039] (3) Add dry rubber seeds with a final ZSM-5 molecular sieve yield of 3% to the mixed solution, and stir for 2 hours...

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Abstract

The invention discloses a quick synthesis method for a nano-scale ZSM-5 molecular sieve. The method includes process steps: (1), uniformly mixing aluminum isopropoxide, tetraethoxysilane, tetrapropylammonium hydroxide with water, stirring for ageing, drying aged sol-gel into dry gel, and grinding the dry gel into powdered dry gel powder to obtain dry gel seed crystal; (2), mixing water, silicon source and aluminum source into mixed solution, uniformly stirring, adding the mixed solution into the dry gel crystal seed, and uniformly stirring; (3), placing the mixed solution added with the dry gel crystal seed into a reaction kettle for static crystallization to obtain a crystallized product; and (4), taking out the crystallized product for washing, drying and roasting to obtain the nano-scale ZSM-5 molecular sieve. The dry gel serving as the crystal seed is added into ZSM-5 mixture, to induce quick formation of molecular sieve crystal during crystallization to realize quick synthesis of the ZSM-5 molecular sieve. The quick synthesis method for the nano-scale ZSM-5 molecular sieve has the advantage of simplicity, time saving, easiness to get raw materials, low cost, low pollution and high product crystallinity.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, in particular to a method for rapidly synthesizing nanometer ZSM-5 molecular sieves. Background technique [0002] ZSM series medium-porous high-silica zeolite is a new type of zeolite catalyst developed by Mobil in the 1970s to meet the needs of type-selective catalysis. ZSM-5 is one of the outstanding representatives with its unique crystal structure and three-dimensional intersecting channel system, and its high silicon-aluminum ratio makes it have ideal acid resistance, alkali resistance and hydrothermal stability. Therefore, it is widely used as a solid acid catalyst material in petroleum refining, such as catalytic cracking, non-hydrogen decondensation, etc., especially for increasing the octane number of FCC gasoline, and has received very good results. Nanomaterials are a new class of materials that emerged in the late 1980s and rose rapidly. Their small geometric size not on...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00
Inventor 王亚涛房承宣彭胜于泳王志彦
Owner KAILUAN ENERGY CHEM
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