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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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

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

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[0026] The present invention uses mesoporous silica as a precursor to synthesize nano Silicalite-1 molecular sieve by steam assisted crystallization method, and the specific steps are as follows:

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

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

[0029] In step 3, the mesoporous silica is impregnated with the above-mentioned mixed solution, and then dried at room temperature to volatilize a part of the water until the material composition ratio in the raw materials is reached to obtain the initial synthesi...

Example Embodiment

[0033] Example 1: Mesoporous silica

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

[0035] Table 1 Particle size parameter table of spherical mesoporous silica

[0036] Mark

Example Embodiment

[0037] Example 2: Preparation of Nano Silicalite-1

[0038] First, tetrapropylammonium hydroxide is added to deionized water, stirred and dissolved to obtain a mixed solution. A certain amount of the above-mentioned solution is impregnated with mesoporous silica and dried for a period of time at room temperature to obtain a solid mixture. Transfer the above solid mixture to the upper flat plate of the stainless steel autoclave, and add water to the bottom of the reactor. The stainless steel reactor is sealed, put in an oven, and crystallized at 100-200°C for 12-150 hours. After the reaction is completed, the solid product is rapidly cooled, the solid product is separated, washed with deionized water, dried in an air atmosphere at 110°C and calcined at 550°C for 6 hours to obtain nano Silicalite-1 molecular sieve.

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

[0040] The s...

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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...

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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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