Molecular sieve aggregate and its preparation method

A technology of molecular sieves and molecules, which is applied in the field of molecular sieve aggregates and their preparation, can solve problems such as difficult separation, achieve the effects of increasing specific surface area, solving pore blocking, and maintaining catalytic activity

Inactive Publication Date: 2013-01-16
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention overcomes the above-mentioned defects of the prior art, and provides a molecular sieve aggregate and a preparation method thereof. While the preparation method is simple and the performance of the molecular sieve is maintained, it solves the disadvantage of being difficult to separate in application, and is a useful material for the binder in molecular sieves. Applications in the

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  • Molecular sieve aggregate and its preparation method

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preparation example Construction

[0029] The preparation method of the molecular sieve aggregate of the present invention enables the molecular sieve to be easily separated and filtered, constructs multi-stage channels, and maintains the catalytic activity of the molecular sieve. The preparation steps are as follows:

[0030] (1) Synthesizing molecular sieves with crystal grains smaller than 300 nm according to a known method, and using the resulting synthetic slurry in step (3);

[0031] (2) Synthesize mesoporous silica sol according to a known method;

[0032](3) Add the mesoporous silica sol in step (2) directly into the synthetic slurry obtained in step (1), stir for 0.5-5 hours and then filter directly or continue heating at 50-195 °C before filtering, washing and drying Finally, molecular sieve aggregates are obtained.

[0033] Molecular sieves in step (1) can include Silicalite-1, Silicalite-2, ZSM-5, ZSM-11, TS-1, TS-2, Beta, Y-type molecular sieves, etc., more preferably TS-1, ZSM-5 and Beta Molecu...

Embodiment 1

[0034] Example 1 Preparation of mesoporous silica sol

[0035] Method 1: Refer to the synthesis method in the literature Kazuyuki Kuroda, Chem. Commun., 2009, 5094–5096 to synthesize mesoporous silica sol. Tetramethyl orthosilicate (TMOS) was used as the silicon source, and triethanolamine (TEAH 3 ) as the alkali source, and cetyltrimethylammonium bromide (CTAB) as the mesoporous directing agent. Dissolve CTAB in TEAH 3 In the aqueous solution, stir at 80 ℃ for 30 minutes to completely dissolve CTAB, add TMOS to the supernatant, and the ratio of the amount of substances in the final system is TMOS : TEA : CTAB : H 2 O = 1 : 0.25 : 0.5 : 1200, and continued stirring at 80°C for 2 hours to obtain a mesoporous silica sol.

[0036] Method 2: See the synthesis method in the literature Kun Zhang, Microporous and Mesoporous Materials, submitted, doi:10.1016 / j.micromeso: use tetramethylorthosilicate (TMOS) or tetraethylorthosilicate (TEOS) as the silicon source , with triethanolam...

Embodiment 2

[0038] Example 2 Preparation of TS-1 molecular sieve nanoparticles

[0039] Tetraethyl orthosilicate (TEOS) was used as the silicon source, tetrapropylammonium hydroxide (TPAOH) was used as the template, tetrabutyl titanate (TBOT) was used as the titanium source, and an appropriate amount of water and isopropanol was used as the Solvent; material molar ratio TPAOH: TEOS is 0.18, 0.27, 0.35; water: silicon source is 18, 30, 50; titanium source: silicon source is 0.025, 0.02; isopropanol: titanium source mass ratio is 10. First, dissolve TEOS in TPAOH. After TEOS is hydrolyzed, add TBOT dissolved in isopropanol in an ice-water bath, stir at room temperature for 30 minutes, and then distill alcohol in hot water at 70°C. Add an appropriate amount of water, continue to stir at room temperature for 30 minutes, and put it into a stainless steel self-generating pressure reactor with a polytetrafluoroethylene liner for crystallization. The crystallization temperature is 160-180 ℃, and ...

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Abstract

The invention belongs to the fields of the material chemistry and the catalytic chemistry, and discloses a molecular sieve aggregate. The molecular sieve aggregate comprises molecular sieve nanoparticles and mesoporous particles, wherein the surfaces of the molecular sieve nanoparticles have negative charges, the surfaces of the mesoporous particles have positive charges, and the molecular sieve aggregate is obtained by the combination of the molecular sieve nanoparticles with the mesoporous particles through an electrostatic action. The invention also discloses a preparation method of the molecular sieve aggregate. The preparation method comprises the following steps: respectively synthesizing the molecular sieve nanoparticles and the mesoporous particles, adding the mesoporous particles to the molecular sieve nanoparticles, stirring, and filtering to obtain the molecular sieve aggregate. The preparation method has the advantages of simple steps and easy operation; and the molecular sieve aggregate has the advantages of substantially improved molecular sieve specific surface area and maintenance of the catalytic performance of traditional molecular sieves.

Description

technical field [0001] The invention relates to the fields of inorganic chemistry, physical chemistry, material chemistry, catalytic chemistry and the like, and in particular relates to a molecular sieve aggregate and a preparation method thereof. Background technique [0002] In order to reduce the limitation of mass transfer in industrial applications, molecular sieves with small grains are often used. When the grain size of the molecular sieve is less than 300 nm, it is difficult to obtain the molecular sieve sample through simple filtration because the particles are too small, and it needs to be prepared by high-speed centrifugation or other means, which greatly increases the industrial cost and consumes more manpower and material resources . [0003] Many scientific researchers are committed to making the preparation process simpler and the molecular sieve easier to recycle while maintaining the performance of nano-TS-1 molecular sieves. Currently effective solutions ...

Claims

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Application Information

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IPC IPC(8): B01J29/89B01J29/70C07D301/03C07D303/04C07C39/06C07C37/11
Inventor 王一萌张颖张坤何鸣元
Owner EAST CHINA NORMAL UNIVERSITY
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