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Metal modified silica sol for synthesizing SAPO-34 molecular sieve and preparation method of metal modified silica sol

A metal modification, silica sol technology, applied in the field of metal modified silica sol, small particle size metal modified silica sol, can solve the problem of particle size reduction and specific surface area, to achieve increased specific surface area, large specific surface area, The effect of short production cycle

Active Publication Date: 2020-06-23
CHIA TAI ENERGY MATERIALS DALIAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the prior art, there is no disclosure related to the preparation process of several metal ion-modified silica sol products in the present invention, and the particle size of the SAPO-34 molecular sieve prepared by using the synthesized silica sol product of the present invention is reduced, The specific surface area increases accordingly, and the performance and life of the molecular sieve are significantly improved; the invention discloses a process that is simple and easy to operate, with mild conditions, short reaction time, small particle size of the product, uniform dispersion of metal ions, and adjustable ratio silica sol products

Method used

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  • Metal modified silica sol for synthesizing SAPO-34 molecular sieve and preparation method of metal modified silica sol
  • Metal modified silica sol for synthesizing SAPO-34 molecular sieve and preparation method of metal modified silica sol
  • Metal modified silica sol for synthesizing SAPO-34 molecular sieve and preparation method of metal modified silica sol

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preparation example Construction

[0037] A kind of metal-modified silica sol for synthesizing SAPO-34 molecular sieve, preparation method comprises the following steps:

[0038] S1. Mix silicon powder with a molar number of 3.5 to 6.5, a particle size of not higher than 50 μm, and a purity of not lower than 99%, and deionized water with a molar number of 14 to 52, stir, and activate at 45 to 65°C for 15 minutes to 1h;

[0039] S2, adding 0.025-0.30 moles of a basic catalyst, feeding at a temperature of 50-65°C, and reacting at 70-95°C for 5-8 hours to obtain a silica sol seed solution;

[0040] S3. Mix and stir the silica sol seed solution, deionized water, 0.025-0.05 moles of metal salt solution, and 0.025-0.05 moles of basic catalyst at 65-90°C, and react at 70-95°C for 2-5 hours After that, the modified silica sol solution is obtained;

[0041] S4. After stilling, precipitation and suction filtration, a metal-modified silica sol product with a particle size of 4-10 nm is obtained.

[0042] In the above p...

Embodiment 1

[0046] Add 500ml of deionized water to a 2L round bottom flask, add 100g of metal silicon powder under stirring, and activate at 45°C for 15min in a water bath. When the temperature rises to 65°C, slowly add an alkaline catalyst solution made of 1g of sodium hydroxide and 100ml of deionized water to the activated solution one by one. After the reaction exotherm is stable, rise to 80°C and react for 5h to obtain silica sol seeds solution.

[0047] Dissolve 1g of sodium hydroxide in 100ml of deionized water to make an alkaline catalyst solution, and heat it to 80°C, and dissolve 15g of Zn(NO 3 )·6H 2 O was dissolved in 100ml deionized water to make a metal salt solution; after mixing the two with the silica sol seed solution prepared in the previous step, react at 80°C for 2 hours under stirring.

[0048]After static precipitation and suction filtration to remove a small amount of unreacted metal silicon powder, a small particle size metal modified silica sol product is obtain...

Embodiment 2

[0050] Add 700ml of deionized water into a 2L round bottom flask, add 120g of metal silicon powder under stirring, and activate at 50°C for 15min in a water bath. When the temperature rises to 65°C, slowly add an alkaline catalyst solution made of 2g of sodium hydroxide and 100ml of deionized water to the activated solution one by one. After the reaction exotherm is stable, rise to 85°C and react for 5h to obtain silica sol seeds solution.

[0051] Dissolve 1g of sodium hydroxide in 100ml of deionized water to make an alkaline catalyst solution, and heat to 85°C, 15g of Zn(NO 3 )·6H 2 O was dissolved in 100ml of deionized water to make a metal salt solution; after mixing the two with the silica sol seed solution prepared in the previous step, react at 85°C for 3 hours under stirring.

[0052] After static precipitation and suction filtration to remove a small amount of unreacted metal silicon powder, a small particle size metal modified silica sol product is obtained.

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Abstract

The invention discloses metal modified silica sol for synthesizing an SAPO-34 molecular sieve and a preparation method of the metal modified silica sol. The preparation method comprises the followingsteps: activating silicon powder, adding an alkaline catalyst, reacting for a period of time to obtain a silica sol seed solution, continuously reacting with a metal salt solution and the alkaline catalyst under a stirring condition at a certain temperature, standing, precipitating, and carrying out suction filtration to finally obtain the metal modified silica sol product. The metal modified silica sol for synthesizing the SAPO-34 molecular sieve prepared by the method is simple in operation method, short in reaction time and mild in condition, and the obtained silica sol product has the characteristics of small particle size, large specific surface area, high activity and adjustable metal loading proportion. Meanwhile, the SAPO-34 molecular sieve prepared from the silica sol product obtained by the invention shows excellent performance in methanol-to-olefin reaction.

Description

technical field [0001] The invention relates to a metal-modified silica sol, in particular to a metal-modified silica sol for synthesizing SAPO-34 molecular sieves and a preparation method thereof, and belongs to the technical field of small-diameter metal-modified silica sol. Background technique [0002] SAPO-34 molecular sieve has attracted more and more attention from the industry because of its suitable acid center, good hydrothermal stability, excellent ethylene and propylene selectivity and long life. With the continuous demand for improving the performance of SAPO-34 molecular sieves, more optimization schemes have been proposed, including metal modification of molecular sieves and reduction of particle size of molecular sieves. [0003] The traditional metal modification of SAPO-34 molecular sieve is through molecular sieve impregnation, in situ synthesis and other methods, but these methods will cause metal ions to not enter the molecular sieve framework, but only ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/141C01B37/08C01B39/54B82Y30/00B01J29/85C07C1/20C07C11/04C07C11/06
CPCB01J29/85B82Y30/00C01B33/1412C01B37/08C01B39/54C01P2004/64C01P2006/12C07C1/20C07C2529/85C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 周君梦徐双刘禹王凤王闯袁龙
Owner CHIA TAI ENERGY MATERIALS DALIAN
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