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Phosphorus-containing hierarchical pore ZSM-5 molecular sieve and preparation method thereof

A technology of ZSM-5 and molecular sieves, which is applied in the direction of molecular sieve catalysts, molecular sieve catalysts, chemical instruments and methods, and can solve problems such as unsatisfactory hydrothermal stability

Active Publication Date: 2021-10-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Therefore, one of the purposes of the present invention is to provide a phosphorus-containing hierarchically porous ZSM-5 molecular sieve that is different from the physicochemical characteristics of the prior art for problems such as unsatisfactory hydrothermal stability in the prior art; the second purpose It is to provide the preparation method of the phosphorus-containing hierarchical porous ZSM-5 molecular sieve

Method used

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  • Phosphorus-containing hierarchical pore ZSM-5 molecular sieve and preparation method thereof
  • Phosphorus-containing hierarchical pore ZSM-5 molecular sieve and preparation method thereof
  • Phosphorus-containing hierarchical pore ZSM-5 molecular sieve and preparation method thereof

Examples

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Embodiment 1A

[0036] Example 1A illustrates the phosphorus-containing hierarchically porous ZSM-5 molecular sieve and process of the present invention.

[0037] 18.5g diammonium hydrogen phosphate was dissolved in 60g deionized water, stirred for 0.5h to obtain a phosphorus-containing aqueous solution, added 108g hydrogen-type multi-stage porous ZSM-5 molecular sieves (provided by Qilu branch of Sinopec catalyst company, relative crystallinity is 88.6%, The silica / alumina molar ratio is 20.8, Na 2 The O content is 0.017% by weight, and the specific surface area is 373m 2 / g, the total pore volume is 0.256ml / g, the mesopore volume is 0.119ml / g, and the average pore diameter is 5.8nm, the same below), using the impregnation method, after immersing at 20°C for 2 hours and drying in an oven at 110°C, Apply external pressure and add water, and treat for 0.5h at 450°C, 0.4Mpa, 60% water vapor atmosphere to obtain a phosphorus-containing hierarchical porous ZSM-5 molecular sieve sample, which is ...

Embodiment 1B

[0039] Example 1B illustrates the phosphorus-containing hierarchically porous ZSM-5 molecular sieve and process of the present invention.

[0040] The materials, proportioning, drying and roasting are the same as those in Example 1A, except that diammonium hydrogen phosphate, hydrogen-type hierarchical porous ZSM-5 molecular sieve and water are mixed to form a slurry, and the temperature is raised to 100° C. for 2 hours. The obtained phosphorus-containing hierarchically porous ZSM-5 molecular sieve sample is denoted as PBZ-1.

Embodiment 2A

[0063] Example 2A illustrates the phosphorus-containing hierarchically porous ZSM-5 molecular sieve and process of the present invention.

[0064] Dissolve 18.5g of diammonium hydrogen phosphate in 120g of deionized water, stir for 0.5h to obtain a phosphorus-containing aqueous solution, then add 108g of hydrogen-type multi-stage porous ZSM-5 molecular sieves, and use the impregnation method to soak at 20°C for 2 hours and then at 110°C After drying in an oven, apply external pressure and add water, and treat for 2 hours at 600°C, 0.4Mpa, and 50% water vapor atmosphere to obtain a phosphorus-containing hierarchically porous ZSM-5 molecular sieve sample, which is designated as PAZ-2.

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Abstract

The invention discloses a phosphorus-containing hierarchical pore ZSM-5 molecular sieve, which is characterized in that in surface XPS elemental analysis, n1 / n2 is less than or equal to 0.08, n1 represents the mole number of phosphorus, and n2 represents the total mole number of silicon and aluminum. Based on an NH3-TPD atlas after 17h of hydrothermal aging under the conditions of 800 DEG C and 100% water vapor, the proportion of the central peak area of the strong acid at the desorption temperature of 200 DEG C or above to the central peak area of the total acid is greater than or equal to 45%, and the strong acid center retention degree is relatively high. The molecular sieve is capable of increasing the yield of low-carbon olefins and increasing the yield of high-added-value products in liquefied gas production.

Description

technical field [0001] The invention relates to a phosphorus-containing ZSM-5 molecular sieve and a preparation method thereof, more specifically the invention relates to a phosphorus-containing multi-level porous ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve is a widely used catalytic material developed by Mobil Company 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. The pores of ZSM-5 molecular sieve are composed of ten-membered rings, and its size is between small-pore zeolite and large-pore zeolite, so it has a unique shape-selective catalytic effect. ZSM-5 molecular sieve has a unique pore structure, good shape-selective cat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38B01J29/40C07C4/06C07C11/06C07C11/08
CPCC01B39/38B01J29/40C07C4/06C01P2002/86C01P2006/12C01P2006/14C01P2006/17C01P2002/72C07C2529/40C07C11/06C07C11/08Y02P20/52
Inventor 罗一斌王成强欧阳颖邢恩会舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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