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Phosphorus-modified ZSM-5 molecular sieve and preparation method thereof

A technology of ZSM-5 and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., 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

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Problems solved by technology

[0009] Therefore, one of the purposes of the present invention is to provide a phosphorus-modified ZSM-5 molecular sieve that is different from the prior art for problems such as unsatisfactory hydrothermal stability existing in the prior art; two purposes of the present invention are to provide the Preparation method of phosphorus modified ZSM-5 molecular sieve

Method used

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  • Phosphorus-modified ZSM-5 molecular sieve and preparation method thereof
  • Phosphorus-modified ZSM-5 molecular sieve and preparation method thereof
  • Phosphorus-modified ZSM-5 molecular sieve and preparation method thereof

Examples

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Embodiment 1-1

[0033] Example 1-1 illustrates the phosphorus-modified ZSM-5 molecular sieve and process of the present invention.

[0034] Get 16.2g diammonium hydrogen phosphate (Tianjin Guangfu Science and Technology Development Co., Ltd., analytically pure, the same below) and dissolve it in 60g deionized water, stir for 0.5h to obtain a phosphorus-containing aqueous solution, add 113g HZSM-5 molecular sieve (Sinopec catalyst company Qilu Provided by the branch company, the relative crystallinity is 91.1%, the silica / alumina molar ratio is 24.1, and the Na 2 The O content is 0.039% by weight and the specific surface area is 353m 2 / g, the total pore volume is 0.177ml / g, the same below), modified by impregnation, impregnated at 20°C for 2 hours, dried in an oven at 110°C, applied external pressure and added water, at 500°C, The phosphorus-modified ZSM-5 molecular sieve sample obtained by treating under 0.5Mpa and 50% water vapor atmosphere for 0.5h is designated as PSZ1-1.

Embodiment 1-2

[0036] Examples 1-2 illustrate the phosphorus-modified ZSM-5 molecular sieves and methods of the present invention.

[0037] The materials, proportioning, drying and roasting are the same as those in Example 1-1, except that diammonium hydrogen phosphate, HZSM-5 molecular sieve and water are mixed and beaten into a slurry, and the temperature is raised to 100° C. for 2 hours. The obtained phosphorus-modified ZSM-5 molecular sieve sample is denoted as PSZ1-2.

Embodiment 2-1

[0061] Example 2-1 illustrates the phosphorus-modified ZSM-5 molecular sieve and process of the present invention.

[0062] Dissolve 16.2g of diammonium hydrogen phosphate in 120g of deionized water at 50°C, stir for 0.5h to obtain a phosphorus-containing aqueous solution, add 113g of HZSM-5 molecular sieve, modify it by impregnation, soak it at 20°C for 2 hours, and then soak it at 110°C Dry it in a lower oven, apply external pressure and add water, pressurize hydrothermal calcination at 600°C, 0.5Mpa, and 30% water vapor atmosphere for 2 hours, and obtain a phosphorus-modified ZSM-5 molecular sieve sample, which is designated as PSZ-2.

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Abstract

The invention discloses a phosphorus modified ZSM-5 molecular sieve. In 27Al MAS-NMR, the ratio of the resonance signal peak area with the chemical shift of 39 + / - 3 ppm to the resonance signal peak area with the chemical shift of 54 + / - 3 ppm is greater than or equal to 1. The phosphorus-modified ZSM-5 molecular sieve is prepared by carrying out phosphorus modification treatment on a hydrogen type ZSM-5 molecular sieve by adopting a phosphorus-containing compound solution through an impregnation method; and carrying out hydrothermal roasting treatment under the atmosphere environment of externally applying pressure and externally adding water. Phosphorus in the molecular sieve is fully coordinated with framework aluminum, and the framework aluminum is fully protected, so that the molecular sieve has good hydrothermal and active stability and meanwhile has more excellent cracking conversion rate and higher low-carbon olefin yield.

Description

technical field [0001] The invention relates to a modified ZSM-5 molecular sieve and a preparation method thereof, and further the invention relates to a phosphorus-modified 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 catalysis and isomerization performance, hi...

Claims

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Application Information

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