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A kind of ZSM-5 molecular sieve and its preparation method and application

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of easy agglomeration, large grain size, cannot exceed 40, etc., and achieve dispersibility. Good, particle dispersion, large aspect ratio effect

Active Publication Date: 2019-05-31
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But for ZSM-5 molecular sieves, it is usually easy to synthesize aluminum-rich and low-silicon molecular sieves under the condition of no template, and the molar silicon-aluminum ratio usually cannot exceed 40, and the product size is generally larger than the seed crystal molecular sieve, and the crystal grains are larger and easy to agglomerate;

Method used

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  • A kind of ZSM-5 molecular sieve and its preparation method and application
  • A kind of ZSM-5 molecular sieve and its preparation method and application
  • A kind of ZSM-5 molecular sieve and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Dissolve 8.61g of ethanol in 17.36g of deionized water, add 0.84g of concentrated sulfuric acid to form a uniform mixed solution A; mix and stir for 10min at 60°C and then add 0.216g of aluminum sulfate (Al 2 (SO 4 ) 3 18H 2 (0), then add 0.19g seed crystals (silicon-aluminum ratio 90, particle size is 5 μm, average flake size 30nm, as figure 2 , Figure 6 shown). Continue to stir for 1h, finally add 10g water glass (19wt.%SiO 2 , Si / Na=1.11) and 10g deionized water. After aging for 6h, the mixed gel SiO 2 :Al 2 o 3 :Seed:Na 2 O:Alcohol:SO 4 2- :H 2 O=100:1:1.2:40:500:25:7000, crystallized at 140°C for 200h, filtered, washed and dried the crude product to obtain the original ZSM-5 molecular sieve powder (the average length of the sheet is 2μm, The average thickness is 340nm). Related spectra such as figure 1 , 3 and 5. The silica-alumina ratio of the prepared molecular sieve is shown in Table 1.

Embodiment 2

[0065] Dissolve 8.61g of ethanol in 17.36g of deionized water, add 0.76g of concentrated sulfuric acid to form a uniform mixed solution A; mix and stir for 10min at 60°C and then add 0.072g of aluminum sulfate (Al 2 (SO 4 ) 3 18H 2 O), then add 0.19g seed crystals (silicon-aluminum ratio 120, average particle size 4μm, average flake size 20nm). Continue to stir for 1h, finally add 10g water glass (19wt.%SiO 2 , Si / Na=1.11) and 10g deionized water. After 6h of stirring, the mixed gel SiO 2 :Al 2 o 3 :Seed:Na 2 O:Alcohol:SO 4 2- :H 2 O=100:0.5:1.5:30:300:15:5000, crystallized at 140°C for 120h, filtered, washed and dried the crude product to obtain ZSM-5 molecular sieve powder (the average length of the sheet is 1.5μm , with an average thickness of 280nm).

Embodiment 3

[0067] Dissolve 8.61g of ethanol in 17.36g of deionized water, add 0.84g of concentrated sulfuric acid to form a uniform mixed solution A; mix and stir for 10min under the condition of 60°C, and then add 0.043g of aluminum sulfate (Al 2 (SO 4 ) 3 18H 2 O), and then add 0.19g seed crystals (silicon to aluminum ratio 154, average particle size of 3 μm, average flake size of 15 nm). Continue to stir for 1h, finally add 10g water glass (19wt.%SiO 2 , Si / Na=1.11) and 10g deionized water. After 6h of stirring, the mixed gel SiO 2 :Al 2 o 3:Seed:Na 2 O:Alcohol:SO 4 2- :H 2 O=100:0.3:2:40:700:30:7000, crystallize at 140°C for 72h, filter, wash and dry the crude product to obtain ZSM-5 molecular sieve powder (the average length of the sheet is 1.2μm , with an average thickness of 220nm).

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Abstract

A ZSM-5 molecular sieve, a preparing method thereof and applications of the molecular sieve are provided. The ZSM-5 molecular sieve is prepared through an amine-free system. A silica-alumina ratio of the ZSM-5 molecular sieve is 40-200. The ZSM-5 molecular sieve is prepared by adopting a nanometer thin-layer ZSM-5 molecular sieve having a high silica-alumina ratio as a crystal seed with the mole ratio of raw materials meeting a condition that the mole ratio of SiO2 to Al2O3 is 100:(0.04-2). Compared with molecular sieves synthesized under traditional template-free conditions, the ZSM-5 molecular sieve synthesized by the method is a molecular sieve having a high silica-alumina ratio (higher than 40). The silica-alumina ratio of the prepared flake ZSM-5 molecular sieve is adjustable in a large range (40-200).

Description

technical field [0001] The invention relates to the field of molecular sieve preparation, in particular to a ZSM-5 molecular sieve and its preparation method and application. Background technique [0002] Among porous materials, ZSM-5 zeolite molecular sieves are widely used in ion exchange, adsorption, And separation, petrochemical and fine chemical synthesis and other fields. Patents CN1699173, CN1247457C, CN101723405A, etc. have adopted different organic amine (ammonium) templates to synthesize ZSM-5 molecular sieves, but generally synthesized silica-alumina zeolite molecular sieves, the price of organic templates is more expensive, which increases the synthesis cost of zeolite; The open pore structure can only be obtained after high-temperature calcination to remove the organic template. Generally, high-temperature calcination at 500-600 ° C consumes a lot of energy and destroys the crystal structure of zeolite molecular sieves to a certain extent (such as framework dea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38
CPCC01B39/38C01P2002/72C01P2004/03C01P2004/04C01P2004/60C01P2004/62
Inventor 巩雁军李佳蓉闵媛媛尚蕴山
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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