Method for preparing phosphor modified ZSM-5 sieve

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of increasing manufacturing cost, difficulty in forming core/shell molecular sieve, long crystallization time, etc. problem, to achieve the effect of reducing manufacturing cost, improving stability of hydrothermal activity, and easy operation

Inactive Publication Date: 2007-02-21
北京盛大京泰化学研究所
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  • Summary
  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of its method is that if it is synthesized at high temperature, AlO 4 -5 grows well in the outer layer of ZSM-5, which easily leads to AlO 4 -5 independent crystallization, it is difficult to form a core/shell molecular sieve in the true sense; if synthesized at low temperature, AlO 4 -5 has a long crystallization time, resulting in excessive energy consumption
[0014] For ZSM-5 molecular sieve, due to the high ratio of silicon to aluminum in the framework and the unique

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0025] Example 1

[0026] Take 1.0 liter of water glass (Shandong Aluminum Factory, SiO 2 Content 250.4 g / L, Na 2 O 78.4 g / l, density (20℃) 1.259 g / ml); will be made from 76.5 ml of aluminum sulfate solution (produced by Shandong Aluminum Factory, Al 2 O 3 Content 92.7 g / L, d 4 20= 1.198) and 175.7 ml of dilute sulfuric acid (prepared with chemically pure reagents, Beijing Jihua Factory, concentration is 26% by weight, d 4 20 = 1.192) The acidified aluminum sulfate solution was added to the above-mentioned water glass with stirring to prepare a reaction mixture. The total volume of the materials obtained was 1260 ml. The reaction mixture was charged into the reaction kettle and stirred at 180°C for crystallization. After hours, the obtained product is filtered and washed to obtain the original ZSM-5 powder, and then the obtained product (ZSM-5 dry basis), ammonium sulfate and water are exchanged at 95°C for 1 hour at a weight ratio of 1:0.8:20. After the exchange, the content of...

Example Embodiment

[0035] Example 2

[0036] According to the preparation conditions of Example 1, take 150 grams of ZSM-5 raw powder, put the product into a fixed bed, weigh 7 grams of phosphorus pentoxide and evaporate and sublime under the action of 350°C to form a gas phase, and then dry it The air as the carrier is passed into the fixed bed and deposited on the ZSM-5 molecular sieve to form phosphorus-modified ZSM-5. The phosphorus content was determined to be 4.7% by X-ray fluorescence spectrometry, and the distribution of phosphorus oxides in the surface layer of any crystal particles was observed by transmission electron microscopy-energy dispersive spectroscopy TEM-EDS as shown in Table 3.

[0037] Measuring point

[0038] Determination of hydrothermal stability. After the obtained molecular sieve was hydrothermally aged at 800°C / 4 hours under 100% water vapor conditions, the aged sample was evaluated on the pulse micro-reverse chromatography device for its n-carbon tetradecane p...

Example Embodiment

[0039] Example 3

[0040] According to the preparation conditions of Example 1, the crystallization conditions were changed to crystallization at 170°C for 20 hours, and the rest were the same as in Example 1. 150g (dry basis) of the obtained ZSM-5 product was put into a fixed bed and weighed 5 Grams of phosphorus pentoxide evaporate and sublime under the action of 450℃ to form a gas phase, and then use dry air as a carrier to pass into the fixed bed and react with ZSM-5 to form a uniformly modified phosphorus oxide ZSM-5 molecular sieve. The phosphorus content was determined by X-ray fluorescence spectrometry to be 2.7%, and the distribution of phosphorus oxides in the surface layer of any crystal particles was observed by transmission electron microscopy-energy dispersive spectroscopy TEM-EDS as shown in Table 4.

[0041] Measuring point

[0042] Determination of hydrothermal stability. After the obtained molecular sieve was hydrothermally aged at 800°C / 4 hours under ...

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PUM

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Abstract

This invention relates to a method for preparing P-modified ZSM-5 molecular sieve. The method comprises: (1) performing heat-exchange on synthesized ZSM-5 molecular sieve with ammonium solution; (2) placing in a fixed bed reactor; (3) heating to evaporate and sublimate phosphorus oxide at 250-600 deg.C; (4) introducing air or inert gas into the fixed bed reactor as the carrier gas, and uniformly depositing phosphorus oxide onto ZSM-5 molecular sieve by chemical vapor deposition to obtain P-modified ZSM-5 molecular sieve. The method can uniformly deposit phosphorus oxide onto ZSM-5 molecular sieve, thus improving the hydrothermal activity and stability of ZSM-5 molecular sieve. The catalytic cracking catalysts with P-modified ZSM-5 molecular sieve as the active component have better catalytic activity and can bring higher olefin yields. The method has such advantages as easy operation, high controllability.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve preparation, and particularly relates to a method for preparing phosphorus-modified ZSM-5 molecular sieves. More precisely, phosphorus oxides are uniformly deposited on ZSM-5 molecular sieves by chemical vapor deposition for chemical modification. Background technique [0002] Since the Mobil Petroleum Company of the United States invented ZSM-5 molecular sieve (USP 3702886) in 1972, due to its high silicon-aluminum ratio, unique pore structure and excellent thermal and hydrothermal stability, ZSM-5 molecular sieve has been used in It has been widely used in petrochemical processes such as shape-selective cracking, alkylation, isomerization, disproportionation, catalytic dewaxing, and etherification of hydrocarbons. The synthesis method of ZSM-5 molecular sieve has been developed from the classic organic method using organic ammonium as a template to the synthesis method without ammonium. ...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 张周珺李朝利姜继东王华峰李桂英
Owner 北京盛大京泰化学研究所
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