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A kind of preparation method of nano zsm-5 molecular sieve and phosphorus modified zsm-5 molecular sieve

A technology of ZSM-5 and molecular sieve, which is applied in the direction of nanotechnology, crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of low crystallinity, uneven particle size, The silicon-aluminum ratio cannot be adjusted, etc., to achieve the effects of large-scale industrialization and application, good dispersion, and regular crystal shape

Active Publication Date: 2018-03-23
山东泓泰恒瑞新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many reports related to this aspect, the process is long, complicated and difficult to control
Moreover, the obtained ZSM-5 molecular sieve has low crystallinity, uneven particle size, uncontrollable silicon-aluminum ratio, and obvious crystal agglomeration after high-temperature heat treatment.

Method used

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  • A kind of preparation method of nano zsm-5 molecular sieve and phosphorus modified zsm-5 molecular sieve
  • A kind of preparation method of nano zsm-5 molecular sieve and phosphorus modified zsm-5 molecular sieve
  • A kind of preparation method of nano zsm-5 molecular sieve and phosphorus modified zsm-5 molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Mix the required pseudo-boehmite, tetraethylorthosilicate, tetrapropylammonium hydroxide and water according to the molar ratio of 0.025:1:0.25:12.5, and adjust the pH to 11-12 with ammonia water. After mixing evenly, crystallize at 120°C for 12 hours, crystallize at 170°C for 12 hours, cool to room temperature, and then evaporate through thin film to obtain nano ZSM-5 molecular sieve powder.

Embodiment 2

[0036] Mix the required pseudo-boehmite, tetraethylorthosilicate, tetrapropylammonium hydroxide and water according to the molar ratio of 0.020:1:0.25:10, and adjust the pH to 11-12 with ammonia water. After mixing evenly, crystallize at 120°C for 12 hours, crystallize at 170°C for 12 hours, and cool to room temperature to obtain the ZSM-5 molecular sieve mother liquor; then add ammonium dihydrogen phosphate accounting for 0.1% of the obtained ZSM-5 molecular sieve mother liquor by weight, and After centrifugal separation and drying (120°C), the phosphorus-modified nano ZSM-5 molecular sieve raw powder was obtained.

Embodiment 3

[0038] Mix the required pseudo-boehmite, tetraethylorthosilicate, tetrapropylammonium hydroxide and water according to the molar ratio of 0.0167:1:0.3:10, and adjust the pH to 11-12 with ammonia water. After mixing evenly, crystallize at 120°C for 12 hours, crystallize at 170°C for 12 hours, and cool to room temperature to obtain the ZSM-5 molecular sieve mother liquor; then add ammonium dihydrogen phosphate accounting for 5% of the obtained ZSM-5 molecular sieve mother liquor by weight. After centrifugal separation and drying (120°C), the phosphorus-modified nano ZSM-5 molecular sieve raw powder was obtained.

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Abstract

The invention discloses a nano ZSM-5 molecular sieve and a preparation method of a phosphorus-modified ZSM-5 molecular sieve thereof and mainly solves the problems that the nano molecular sieve of the prior art of preparation has large grain size and poor uniformity and has low degree of crystallinity; a required aluminum source, a silicon source, a template agent and water are mixed well to obtain a material mixed transparent sol with material composition: (0.01-0.1):1:(0.01-0.6):(3-20), crystallizing is performed at 100-175 DEG C for 24-48 hours, and the prepared molecule sieve sol is subjected to alkali neutralization and membrane evaporative concentration, and nano ZSM-5 molecular sieve raw powder is obtained by rake drying; the preparation of the phosphorus-modified molecular sieve includes adding ammonium dihydrogen phosphate modifying agent directly into the product sol, coagulating by means of salting-out effect and great adsorption effect of the nano molecular sieve, and a centrifugal separation product is dried to obtain the phosphorus-modified ZSM-5 molecular sieve. The ZSM-5 molecular sieve synthesized herein has cake shaped grain shape under an electron microscope, and grains are uniform and disperse and are nano-sized without agglomeration.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves and their preparation. Specifically, it relates to a preparation method of a small crystal-scale nanometer ZSM-5 molecular sieve and the phosphorus-modified ZSM-5 molecular sieve. Background technique [0002] ZSM-5 molecular sieve is a widely used zeolite molecular sieve catalytic material developed by Mobil Corporation of the United States in 1972. ZSM-5 molecular sieve has a three-dimensional intersecting channel structure. The channel along the a-axis is a straight hole with a cross-sectional size of 0.54×0.56nm, which is approximately circular. The channel along the b-axis is a zigzag hole with a cross-sectional size of 0.51 ×0.56nm, oval shape. Its orifice is composed of ten-membered rings, and its size is between small-pore zeolite and large-pore zeolite, so this type of molecular sieve has unique shape-selective catalysis (reactant selectivity, product shape selectivity, transit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38B82Y40/00
CPCC01B39/38C01P2002/74C01P2004/03C01P2004/62C01P2004/64
Inventor 柳云骐刘智潘龙君潘原马殿民
Owner 山东泓泰恒瑞新材料有限公司
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