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Integral-type heteroatom replacing hierarchical porous molecular sieve and synthesis method thereof

A technology of heteroatom and molecular sieve, which is applied in the field of monolithic heteroatom-substituted multi-stage porous molecular sieve and its one-step synthesis, achieving the effects of low temperature, short crystallization time and reduced water consumption.

Active Publication Date: 2013-06-26
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although in industrial applications, zeolite molecular sieve catalysts are usually in the form of monolithic columns or sheets, but there are no patents and literature reports on the substitution of monolithic heteroatoms for hierarchical pore molecular sieves.

Method used

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  • Integral-type heteroatom replacing hierarchical porous molecular sieve and synthesis method thereof
  • Integral-type heteroatom replacing hierarchical porous molecular sieve and synthesis method thereof
  • Integral-type heteroatom replacing hierarchical porous molecular sieve and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The sol (2.8 wt.% Al 2 o 3 ), 2g of water and 4g of tetrapropylammonium hydroxide mixed at 25 o After C was stirred for 3 hours, 3.5ml of 6% NaOH solution was added to it, and then 0.06g of Fe(NO 3 ) 3 .9H 2 O get the gel mixture, move the gel mixture into the stainless steel synthesis kettle and seal it at 155 o C crystallization for 24 hours, the product of monolithic molecular sieve was washed, dried and 550 o After C was calcined for 6 hours, the heteroatom substituted hierarchical porous Fe-ZSM-5 molecular sieve was obtained. Its chemical formula is Na + 0..073 [(Fe 0.006 al 0.067 Si 0.927 )O 2 ].60H 2 O.

[0018] figure 1 a is the XRD characterization result of the product, by figure 1 a It can be seen that the product has a typical MFI ZSM-5 molecular sieve structure, and the sample has a high degree of crystallinity, indicating that the product has good hydrothermal stability.

[0019] figure 2 and image 3 Respectively, the low-temperature ni...

Embodiment 2

[0023] The sol (2.8 wt.% Al 2 o 3 ), 2g of water and 4g of tetrapropylammonium hydroxide mixed at 25 o After C was stirred for 3 hours, 3.5ml of 6% NaOH solution was added to it, and then 0.06g of Fe(NO 3 ) 3 .9H 2 O get the gel mixture, move the gel mixture into the stainless steel synthesis kettle and seal it at 170 o C crystallized for 24 hours to obtain the product of the monolithic molecular sieve after washing, drying and 550 o After C is calcined for 6 hours, the whole body of Fe-ZSM-5 molecular sieve with heteroatoms and hierarchical pores can be obtained. Its chemical formula is Na + 0..073 [(Fe 0.006 al 0.067 Si 0.927 )O 2 ].60H 2 O.

Embodiment 3

[0025] The sol (2.8 wt.% Al2 o 3 ), 2g of water and 4g of tetrapropylammonium hydroxide mixed at 25 o After C was stirred for 3 hours, 3.5ml of 6% NaOH solution was added to it, and then 0.12g of Fe(NO 3 ) 3 .9H 2 O get the gel mixture, move the gel mixture into the stainless steel synthesis kettle and seal it at 170 o C crystallized for 24 hours to obtain the product of the monolithic molecular sieve after washing, drying and 550 o After C was calcined for 6 hours, the heteroatom substituted hierarchical porous Fe-ZSM-5 molecular sieve was obtained. Its chemical formula is Na + 0.067 [(Fe 0.023 al 0.044 Si 0.933 )O 2 ].60H 2 O.

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Abstract

The invention discloses an integral-type heteroatom replacing hierarchical porous molecular sieve. The chemical formula of the integral-type heteroatom replacing hierarchical porous molecular sieve is (M<n+>)(x+y) / n[(MexAlySil-(x+y))O2].wH2O, wherein M<n+> is one or a mixture of several of cations: Na<+>, K<+>, H<+>, Ca<2+> and Mg<2+>; Me which enters a molecular sieve framework is one or a mixture of several of the following metal atoms: Cu, Mo, Fe, Co, Ti, Ni, Mn, W, V, Zn, Mg, Sn, Pt, Pd, Ce, La and Y; x, y and 1-(x+y) respectively represent mole fractions of Me, Al and Si; x ranges from 0.001 to 0.05, and y ranges from 0 to 0.6; w represents the number of water molecules in each mole of (MexAlySil-(x+y))O2; and w ranges from 1 to 80, and n is equal to 1 or 2. The preparation process is simple, and is low in cost.

Description

technical field [0001] The invention relates to a monolithic heteroatom-substituted multi-stage pore molecular sieve and a one-step synthesis method thereof. Background technique [0002] Zeolite molecular sieves have regular channels, good shape selectivity, stability and adjustable catalytic performance, and are widely used in the fields of catalysis, ion exchange, adsorption and separation. The introduction of metal ions into molecular sieves can further improve the hydrothermal stability and catalytic performance of molecular sieves. At present, researchers often disperse metal elements on the surface or in the pores of molecular sieves by means of ion exchange, impregnation, and vapor deposition. However, in these three preparation processes, since the metal elements cannot completely enter the molecular sieve framework and partly disperse on the surface or in the pores of the molecular sieve, it is inevitable that they will be reduced to metals and lost under the hydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40C01B39/06
Inventor 程党国DO·孟辉陈丰秋金炜阳詹晓力
Owner ZHEJIANG UNIV
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