Preparation method of skeleton silicon-rich Y-shaped molecular sieve

A molecular sieve and framework technology, applied in the field of molecular sieves, to achieve the effects of high B acid content, increased secondary pore content, and high activity

Active Publication Date: 2010-06-09
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this material also has serious shortcomings: in the process of modifying and preparing molecular sieve materials, in order to maintain the crystallinity of the product, people deliberately choose moderate dealumination and silicon supplementation conditions, so that dealumination and silicon supplementation on Y molecular sieve The speed is roughly the same, and the position wh...

Method used

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  • Preparation method of skeleton silicon-rich Y-shaped molecular sieve
  • Preparation method of skeleton silicon-rich Y-shaped molecular sieve
  • Preparation method of skeleton silicon-rich Y-shaped molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 5 g of solid sodium hydroxide into 495 g of distilled water and stir to dissolve, then raise the temperature of the alkali solution to 65°C. Weigh 100g NaY molecular sieve (mass on dry basis, crystallinity 95%, silicon-aluminum ratio 6.2) into the above alkali solution, keep stirring and alkali treatment at 65°C for 2h. After the alkali treatment is completed, the slurry is filtered, and the obtained molecular sieve filter cake is washed until the pH of the filtrate=9.

[0029] The alkali-treated NaY molecular sieve filter cake (dry basis) was mixed with ammonium chloride and distilled water in a mass ratio of 1:1:10 for beating evenly, and after ammonium exchange was stirred at 90°C for 1 hour, filtered and the above ammonium exchange process was repeated Twice, NH 4 NaY molecular sieve.

[0030] Weigh 9.12 g of ammonium fluorosilicate solid and dissolve it in 250 g of distilled water to prepare an ammonium fluorosilicate solution with a concentration of about 0....

Embodiment 2

[0035] Put 10 g of solid sodium hydroxide into 490 g of distilled water and stir to dissolve, then raise the temperature of the alkali solution to 65°C. Weigh 100g NaY molecular sieve (mass on dry basis, crystallinity 95%, silicon-aluminum ratio 6.2) into the above alkali solution, stir evenly and maintain the reaction at 65°C for 3h to implement alkali treatment. After the alkali treatment is completed, the slurry is filtered, and the obtained molecular sieve filter cake is washed until the pH of the filtrate=9.

[0036] Mix the alkali-treated NaY molecular sieve filter cake (dry basis) with ammonium nitrate and distilled water at a ratio of 1:1:10 and beat evenly. After stirring for ammonium exchange at 90°C for 1 hour, filter and repeat the above exchange process twice to prepare Get NH 4 NaY molecular sieve.

[0037] Weigh 9.12 g of ammonium fluorosilicate solid and dissolve it in 250 g of distilled water to prepare an ammonium fluorosilicate solution with a concentratio...

Embodiment 3

[0039] Put 10 g of potassium hydroxide solid into 490 g of distilled water and stir to dissolve, then raise the temperature of the alkali solution to 45°C. Weigh 100g NaY molecular sieve (mass on dry basis, crystallinity 95%, silicon-aluminum ratio 6.2) into the above alkaline solution, stir evenly and maintain 45°C for reaction (alkali treatment) for 2h. After the alkali treatment is completed, the slurry is filtered, and the obtained molecular sieve filter cake is washed until the pH of the filtrate=9.

[0040] Mix the alkali-treated NaY molecular sieve filter cake (dry basis) with ammonium chloride and distilled water in a ratio of 1:1:10 and beat evenly. After stirring for ammonium exchange at 90°C for 1 hour, filter and repeat the above exchange process twice. Produce NH 4 KNaY molecular sieve.

[0041] Weigh 9.12 g of ammonium fluorosilicate solid and dissolve it in 250 g of distilled water to prepare an ammonium fluorosilicate solution with a concentration of about 0....

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Abstract

The invention discloses a preparation method of a skeleton silicon-rich Y-shaped molecular sieve, comprising the following steps of: firstly, carrying out desiliconizing pretreatment on a NaY molecular sieve with alkali lye and secondly carrying out ammonium exchange and dealumination and silicon reinsertion on the molecular sieve treated with alkali. The alkali treatment condition is to pulp and evenly mix the NaY molecular sieve and an alkali liquor in the mass ratio of NaY (dry basis): alkali: H2O being (0.1-2): (0.05-2): (4-15) and carry out alkali treatment at 0-120 DEG C for 0.1-24h. Compared with a product obtained by carrying out ammonium exchange and silicon-rich treatment on the NaY molecular sieve, the skeleton silicon-rich Y-shaped molecular sieve subject to the desiliconizing pretreatment has higher infrared acid quantity, B acid quantity and secondary pore content. A catalyst prepared from an active component which is the skeleton silicon-rich Y-shaped molecular sieve prepared by the method has stronger heavy oil transformation capability and higher light oil recovery rate when being used for a heavy oil cracking reaction.

Description

technical field [0001] The invention relates to a method for preparing a Y-type molecular sieve with a silicon-rich skeleton, and belongs to the technical field of molecular sieves. Background technique [0002] In the 1980s, the U.S. Union Carbon Company invented a method for preparing a skeleton silicon-rich Y-type molecular sieve (USP 4503023). In this method, the NaY molecular sieve was first subjected to ammonium ion exchange several times, and then the NH 4 A buffer solution such as ammonium oxalate is added to the NaY molecular sieve slurry to control the pH of the solution, and finally a certain concentration of ammonium fluorosilicate solution is slowly added, and the dealumination and silicon supplementation reaction is carried out at 70-90°C. During the reaction, the aluminum atoms in the molecular sieve framework structure are removed from the lattice under the action of ammonium fluorosilicate and dissolved into the solution, while the silicon source from ammoni...

Claims

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Application Information

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IPC IPC(8): C01B39/24
Inventor 申宝剑覃正兴庞新梅高雄厚王宝杰赵红娟刘从华林枫主明烨谢帅郭巧霞曾鹏晖孙国峰高晓慧王国峰申伟郭慧
Owner BC P INC CHINA NAT PETROLEUM CORP
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