Preparation method of low sodium and high silicon y-type molecular sieve

A molecular sieve and high-silicon technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of increased secondary pores of molecular sieves, low crystallinity retention, and lack of crystal lattice skeleton of molecular sieves issues of protection

Active Publication Date: 2022-08-05
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the method of combining ion exchange, hydrothermal treatment and chemical dealumination is generally used to prepare low-sodium high-silicon Y-type molecular sieves. The sodium ions in the zeolite are difficult to exchange with the ammonium ions, so the sodium oxide in the Y-type molecular sieve is generally still between 1.0% and 1.5% after double-cross-baking, and the conventional chemical dealumination method only relies on the Y-type molecular sieve. Molecular sieve framework silicon migration to replenish silicon, the lattice framework of molecular sieve is not protected, and the secondary pores of molecular sieve increase, and the relative crystallinity retention is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A method for preparing a low-sodium and high-silicon Y-type molecular sieve, the steps are as follows:

[0046] (1) adding NaY molecular sieve, ammonium solution and deionized water with a mass ratio of 1:0.1.0:6 into the exchange tank, warming up to 40-45 ° C under stirring, and reacting under 40-45 ° C for 1 hour, get the mixture;

[0047] (2) the mixed solution of step (1) is filtered, and the filter cake is washed with deionized water at 95°C;

[0048] (3) adding the filter cake and the silicon source of the step (2) with a mass ratio of 1:0.05 into the beating tank, stirring at normal temperature for 1 hour to obtain a mixed slurry, which is dried for subsequent use;

[0049] (4) the filter cake of step (3) was calcined for 4 hours in 50%-steam, 450 ℃ of calciners of furnace temperature, and the molecular sieve after calcination was obtained for subsequent use;

[0050] (5) deionized water is added to the molecular sieve after roasting, and the temperature is rai...

Embodiment 2

[0064] A method for preparing a low-sodium and high-silicon Y-type molecular sieve, the steps are as follows:

[0065] (1) adding the NaY molecular sieve, ammonium solution and deionized water with a mass ratio of 1:1.0:15 into the exchange tank, warming up to 95°C under stirring, and reacting under 95°C for 1 hour to obtain a mixed solution;

[0066] (2) the mixed solution of step (1) is filtered, and the filter cake is washed with deionized water at 95°C;

[0067] (3) adding the filter cake and the silicon source of the step (2) with a mass ratio of 1:0.05 into the beating tank, stirring at normal temperature for 1 hour to obtain a mixed slurry, which is dried for subsequent use;

[0068] (4) the filter cake of step (3) was calcined for 1 hour in 110% water vapor, 800 ℃ of calciners of furnace temperature, and the molecular sieve after calcination was obtained for subsequent use;

[0069] (5) deionized water is added to the molecular sieve after roasting, and the temperatur...

Embodiment 3

[0083] A method for preparing a low-sodium and high-silicon Y-type molecular sieve, the steps are as follows:

[0084] (1) adding NaY molecular sieve, ammonium solution and deionized water with mass ratio of 1:0.5:10 into the exchange tank, warming up to 55°C under stirring, and reacting under 55°C for 2 hours to obtain a mixed solution;

[0085] (2) the mixed solution of step (1) is filtered, and the filter cake is washed with deionized water at 70°C;

[0086] (3) adding the filter cake and the silicon source of the step (2) of mass ratio 1:0.03 into the beating tank, stirring at normal temperature for 2 hours to obtain a mixed slurry, and the mixed slurry is dried for subsequent use;

[0087] (4) the filter cake of step (3) was calcined for 3 hours in 80% water vapor, 600 ℃ of calciners of furnace temperature, and the molecular sieve after the calcination was obtained for subsequent use;

[0088] (5) deionized water is added to the molecular sieve after roasting, and the te...

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Abstract

The invention relates to a method for preparing a low-sodium and high-silicon Y-type molecular sieve, which belongs to the field of molecular sieve preparation. The raw materials are added into an exchange tank according to the mass ratio of NaY molecular sieve with a mass ratio of 1:0.1-1.0:6-15, ammonium solution and deionized water. By performing multiple exchanges and roasting, the sodium oxide in the Y-type molecular sieve can be reduced by reducing the pH of the exchange solution and increasing the number of exchanges, and at the same time, the lattice framework of the molecular sieve can be protected. The invention relies on the migration of the Y-type molecular sieve framework silicon to supplement silicon, and at the same time removes framework aluminum through external raw materials, ensures that the molar ratio of the silicon to aluminum ratio of the product is increased, and the molar silicon to aluminum ratio of the prepared product reaches 10-13.

Description

technical field [0001] The invention relates to a preparation method of a low-sodium and high-silicon Y-type molecular sieve, and belongs to the field of molecular sieve preparation. Background technique [0002] When used as a catalyst, Y-type molecular sieve should have higher catalytic activity and better hydrothermal stability. Therefore, Y-type molecular sieve is required to have a higher molar ratio of silicon to aluminum and a lower content of sodium. The synthesized NaY molecular sieve has a silicon-aluminum molar ratio below 5 and contains about 13% sodium oxide, so it needs to be treated to reduce the sodium content of the Y-type molecular sieve and increase the silicon-aluminum ratio. [0003] In the prior art, low-sodium and high-silicon Y-type molecular sieves are generally prepared by a combination of ion exchange, hydrothermal treatment and chemical dealumination. The sodium ions in the zeolite are difficult to exchange with ammonium ions, so after double-bak...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/24B01J29/08
CPCC01B39/24B01J29/084B01J2029/081B01J2229/16
Inventor 明曰信陈文勇刘环昌彭立苗植平王龙张国强
Owner SHANDONG QILU HUAXIN HIGH TECH
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