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Preparation method of nano Silicalite-1 molecular sieve

A molecular sieve and nanotechnology, applied in the field of preparation of nano-Silicalite-1 molecular sieve, can solve problems such as easy aggregation of crystal nuclei, and achieve the effects of simple and easy operation, production cost saving and dosage saving.

Inactive Publication Date: 2019-02-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, when using the steam-assisted crystallization method to synthesize Silicalite-1 molecular sieve, it is often limited by the water content in the system. During the crystallization process, the crystal nuclei are easy to aggregate and obtain larger-sized Silicalite-1 molecular sieve crystals.

Method used

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  • Preparation method of nano Silicalite-1 molecular sieve
  • Preparation method of nano Silicalite-1 molecular sieve

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preparation example Construction

[0026] The present invention uses mesoporous silica as a precursor for the preparation of nano-Silicalite-1 molecular sieves by steam-assisted crystallization. The specific steps are:

[0027] Step 1, the material ratio required for the synthesis of nano Silicalite-1 molecular sieve is SiO 2 :yR:mH 2 O, wherein: R is template, y=0.05~0.5, m=0.1~5, calculate the amount of corresponding material according to need;

[0028] Step 2, weigh the required template agent (organic amine) and a certain amount of water, stir and dissolve at room temperature evenly. The templating agent is at least one of tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrapropylammonium bromide and tetrapropylammonium chloride;

[0029] Step 3, impregnating the mesoporous silica with the above mixed solution, and then drying at room temperature to volatilize part of the water until the material composition ratio in the raw material is reached to obtain the initial synthesis mixture. The s...

Embodiment 1

[0033] Example 1: Mesoporous silica

[0034] The average particle size parameters of spherical mesoporous silica used are shown in Table 1, and the scanning electron microscope images of mesoporous silica are shown in figure 1 .

[0035] Table 1 Spherical mesoporous silica particle size parameter table

[0036] mark

Embodiment 2

[0037] Embodiment 2: the preparation of nano Silicalite-1

[0038]First, tetrapropylammonium hydroxide was added into deionized water, stirred and dissolved to obtain a mixed solution. A certain amount of the above solution was taken to impregnate the mesoporous silica, and dried at room temperature for a period of time to obtain a solid mixture. The above solid mixture was transferred to the upper plate of the stainless steel autoclave, and water was added to the bottom of the autoclave. Seal the stainless steel reaction kettle, put it in an oven, and crystallize at 100-200°C for 12-150 hours. Cool rapidly after the reaction, separate the solid product, wash with deionized water, dry at 110°C in air atmosphere and bake at 550°C for 6 hours to obtain nano-Silicalite-1 molecular sieve.

[0039] The preparation process of using other templates is the same as the preparation process of tetrapropylammonium hydroxide as the template.

[0040] The samples prepared for each reacti...

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Abstract

The invention discloses a preparation method of a nano Silicalite-1 molecular sieve. The molecular sieve is provided with an MFI topological structure, and the grain size of the molecular sieve can beregulated and controlled within a wide nanometer range. Through aA synthesis method of the nano Silicalite-1 molecular sieve, is used for preparing the nano Silicalite-1 molecular sieve is prepared by utilizing spherical mesoporous silica as a precursor through a steam-assisted crystallization method. and with spherical mesoporous silica as a precursor. Compared with the prior art, the synthesismethod is simple and feasible, the synthesized molecular sieve is high in crystal crystallinity, and the grain size of the molecular sieve is uniform and can be regulated and controlled within the wide nanometer range.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a preparation method of nano Silicalite-1 molecular sieve. Background technique [0002] Zeolite molecular sieves are a class of microporous crystal materials with regular pore structures, and are widely used in chemical fields such as homogeneous catalysis, adsorption, separation, ion exchange, and host-guest assembly [Chem.Rev., 1997,97,2373-2419; Chem. Eng., 2011, 118, 16-20]. MFI type zeolite molecular sieve has become the object of many researchers' attention because of its pore size is similar to the kinetic diameter of many commonly used chemical raw material molecules, and has excellent catalytic and separation performance. In 1978, Flanigen first synthesized the all-silicon MFI molecular sieve, Silicalite-1 molecular sieve [Nature, 1978, 271, 512-516]. The molecular sieve has good heat-resistant stability and acid-resistant stability. At t...

Claims

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Application Information

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IPC IPC(8): C01B37/02
CPCC01B37/02C01P2002/72C01P2004/03C01P2004/62
Inventor 张晓敏许磊张艳飞卢鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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