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Process for synthesizing core-shell structure compound molecular sieve and use thereof

A technology of composite molecular sieve and core-shell structure, which is applied in the synthesis field of core-shell structure composite molecular sieve, and can solve the problems of large particle diameter and inability to form core-shell structure composite molecular sieve, etc.

Active Publication Date: 2010-09-29
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle diameter of the synthesized composite molecular sieve is relatively large, about 10 μm, and there are many independently grown phosphorus-aluminum molecular sieves, which cannot form a real core-shell structure composite molecular sieve

Method used

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  • Process for synthesizing core-shell structure compound molecular sieve and use thereof
  • Process for synthesizing core-shell structure compound molecular sieve and use thereof
  • Process for synthesizing core-shell structure compound molecular sieve and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Mix 5.0 g of phosphorus pentoxide with 15 ml of deionized water, and load it onto the surface of 10.0 g of HZSM-5 raw powder by dipping (self-made, with a silicon-aluminum ratio of 76), and treat it at 180 ° C for 48 hours. P-ZSM-5 with the phosphorus source immobilized on the surface of ZSM-5 was obtained. P-ZSM-5 was added to 3.5 g of pseudoboehmite (w(Al 2 O 3 )=68%), 6.2g silica sol (w(SiO 2 ) 40%)) and 10 g of deionized water, after stirring, add 1.46 g of triethylamine.

[0025] The above gel was put into an autoclave, formed at room temperature for 10 hours, firstly crystallized at 120 °C for 7 hours, and then crystallized at 170 °C for 48 hours. The solid obtained by filtration of the product was washed with water, and dried at 160° C. for 24 h to obtain sample C.

[0026] The X powder diffraction of sample C is shown in Figure 1, and the scanning electron microscope is shown in Figure 4.

Embodiment 2

[0029] Example 2: Mix 7.8g of ammonium hydrogen phosphate and ammonium dihydrogen phosphate mixture with 15ml of deionized water, and add to 25.5g of HZSM-5 powder by ion exchange (self-made, silicon-aluminum ratio is 76), 300 ℃ for 4 hours to prepare P-ZSM-5 with phosphorus source immobilized on the surface of ZSM-5. P-ZSM-5 was added to 5.9g pseudo-boehmite (w(Al 2 o 3 )=68%), 11.2g silica sol (w(SiO 2 )=40%)) and 10 g of deionized water, after stirring, 1.35 g of triethylamine was added.

[0030] The above gel was placed in an autoclave, aged at room temperature for 5 hours, then crystallized at a constant temperature of 120°C for 7 hours, and then crystallized at a constant temperature of 180°C for 48 hours. The product was washed by filtration and dried at 160°C for 24h. The X powder diffraction spectrum of the obtained sample has the characteristics of accompanying drawing 1.

Embodiment 3

[0031] Example 3: Load 11.5g of phosphorus powder on the surface of 34.2g of HZSM-5 raw powder (self-made, with a silicon-aluminum ratio of 76) by vapor deposition, and keep the temperature at 600°C for 2 hours to obtain a phosphorus source fixed on the surface of ZSM-5 The P-ZSM-5. P-ZSM-5 was added to 4.6g pseudo-boehmite (w(Al 2 o 3 )=68%), 5.3g of ethyl orthosilicate and 10g of deionized water mixture, after stirring, add 5.43g of triethylamine.

[0032] The above gel was put into an autoclave, and crystallized at a constant temperature of 80°C for 10h, and at a constant temperature of 200°C for 24h. The product was filtered and washed, and dried at 160°C for 24 hours to obtain sample D. The X powder diffraction spectrum of the obtained sample has the characteristics of accompanying drawing 1.

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Abstract

The present invention relates to a synthesizing method for a core-shell structure compound molecular sieve. The method mainly adopts a location growing method to fix a loaded phosphor aluminum or silicon aluminum molecular sieve on the surface of a ZSM-5 molecular sieve to compose the raw materials and then prepare a gel in a primarily wet state and crystallize under a constant temperature, thus synthesizing the core-shell structure compound molecular sieve. The method overcomes the defects of the prior technology, thus reducing the independent growing number of the composed phosphor aluminumor silicon aluminum molecular sieves, further improving the distribution of the phosphor aluminum or silicon aluminum molecular sieve of the shell on the surfaced of the ZSM-5 and reducing the grain diameter of the compound molecular sieve. When the core-shell structure compound molecular sieve prepared by the method is used for heavy oil catalytic cracking, the heavy oil converting rate and the low carbon olefin yield are all higher than the molecular sieve synthesized by the prior technology. Compared with the catalyst which only adopts the ZSM-5 molecular sieve as the active component, theheavy oil converting rate is improved by 2 to 3 percent; the ethylene yield is increased by 1 to 1.5 percent and the liquid gas yield is enhanced by 1.5 to 3.5 percent.

Description

technical field [0001] The invention relates to a synthesis method of a core-shell structure composite molecular sieve. The method is a new method for synthesizing composite molecular sieves with core-shell structure in the petrochemical field - the positioning growth method. The method is mainly to fix one or several of the synthetic raw materials of phosphorus-aluminum or silicon-phosphorus-aluminum molecular sieve on the surface of ZSM-5 molecular sieve in advance before the crystallization of the composite molecular sieve, and enhance the force between the two by appropriate high temperature treatment. . Then, it is mixed with other raw materials for synthesizing the shell molecular sieve to form an incipient wet gel, and after aging at room temperature, the core-shell structure composite molecular sieve is synthesized by high temperature crystallization. The method overcomes the deficiencies of the prior art, reduces the particle diameter of the core-shell structure com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/85B01J29/83B01J29/40C07C4/06C07C11/06
CPCY02P20/52
Inventor 李春义张强杨朝合山红红
Owner PETROCHINA CO LTD
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