Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size

A zeolite molecular sieve, all-silicon technology, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve the problems of poor product quality, low repetition rate and high cost, achieve high quality and reduce synthesis energy. consumption and shortening the crystallization time

Inactive Publication Date: 2012-11-21
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method with simple process and low cost for the shortcomings of the above-mentioned complex process, high cost, low repetition rate, poor product quality and difficulty in industrial produ

Method used

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  • Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size
  • Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size
  • Method for preparing full-silicon DD3R zeolite molecular sieve with pure phase and uniform crystal morphology and size

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0021] Dissolve 3 mL of silicon source in 30 mL of deionized water, stir vigorously, and add 1.6 g of amantadine. After stirring for a while, add 1.3 g of KF to obtain a mixed solution. Add 0.036g of seed crystals to the mixed system obtained in the above steps, mix and stir for 2 hours, transfer to a 50mL hydrothermal reaction kettle, and place it at 170°C for crystallization for 1 day; filter the obtained sample with deionized water Wash, dry at 110°C for 12 hours, and then bake in a muffle furnace at 700°C for 8 hours to obtain a sample. The XRD spectrum of the sample is shown in figure 1 -Example 1, as can be seen from the characterization diagram, the characteristic diffraction peaks of DD3R molecular sieves appeared at 2θ=7.68°, 15.39° and 17.13°, indicating that the synthesized sample is DD3R molecular sieve; the SEM photo is shown in figure 2 -Example 1, the DD3R molecular sieve crystal in the figure has a clear outline, regular shape, parallelepiped, and a grain siz...

Embodiment 2

[0023] Dissolve 3 mL of silicon source in 30 mL of deionized water, stir vigorously, and add 0.8 g of amantadine. After stirring for a while, add 2.6 g of KF to obtain a mixed solution. Add 0.036g of seed crystals to the mixed system obtained in the above steps, mix and stir for 2 hours, transfer to a 50mL hydrothermal reaction kettle, and place it at 170°C for crystallization for 1 day; filter the obtained sample with deionized water Wash, dry at 110°C for 12 hours, and then bake in a muffle furnace at 700°C for 8 hours to obtain a sample. The XRD spectrum of the sample is shown in figure 1 -Example 2, it can be seen from the characterization diagram that the characteristic diffraction peaks of DD3R molecular sieve appear at 2θ=7.68°, 15.39° and 17.13°, indicating that the synthesized sample is DD3R molecular sieve. SEM photo see figure 2 -Example 2, the DD3R molecular sieve crystals in the figure have clear outlines, regular shapes, parallelepipeds, and a grain size of ab...

Embodiment 3

[0025] Dissolve 3 mL of silicon source in 25 mL of deionized water, stir vigorously, and add 1.6 g of amantadine. After stirring for a while, add 1.3 g of KF to obtain a mixed solution. Add 0.036g of seed crystals to the mixed system obtained in the above steps, mix and stir for 2 hours, then transfer to a 50mL hydrothermal reaction kettle, and crystallize at 170°C for 3 days; filter the obtained samples with deionized water Wash, dry at 110°C for 12 hours, and then bake in a muffle furnace at 700°C for 8 hours to obtain a sample. The XRD spectrum of the sample is shown in figure 1-Example 3, it can be seen from the characterization diagram that the characteristic diffraction peaks of DD3R molecular sieve appear at 2θ=7.68°, 15.39° and 17.13°, indicating that the synthesized sample is DD3R molecular sieve. SEM photo see figure 2 -Example 3, the DD3R molecular sieve crystal in the figure has a clear outline, regular shape, regular octahedron, and a grain size of about 8 μm; ...

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Abstract

The invention discloses a method for preparing a full-silicon DD3R zeolite molecular sieve with a pure phase and uniform crystal morphology and size. The purpose of the invention is to provide the method for preparing the full-silicon DD3R zeolite molecular sieve with the pure phase and uniform crystal morphology and size. The method is simple in process, low in cost, good in repeatability and excellent in product quality. The method for preparing the full-silicon DD3R zeolite molecular sieve comprises the following steps: (1) adding an organic structure directingagent, a silicon source and a mineralizer into deionized water to mix and agitate; (2) adding a crystal seed to a mixing system obtained from the step (1); after mixing, agitating and aging, transferring the mixture into a hydrothermal reaction kettle to crystallize; (3), filtering and washing a sample obtained from the step (2), and obtaining the pure-phase DD3R zeolite molecular sieve with uniform crystal morphology and size after drying and baking the sample. The method has the characteristics that the crystallization time is short, the synthetic energy consumption is low, and the obtained pure-phase DD3R zeolite molecular sieve has excellent quality.

Description

technical field [0001] The invention belongs to the technical field of microporous materials, in particular to a method for preparing all-silicon DD3R zeolite molecular sieves with pure phase, uniform crystal shape and size. Background technique [0002] The skeleton structure of all-silica zeolite molecular sieve DD3R (Gies, Z. Kristallogr. 1986, 175, 93-104) is composed of decahedron [4 3 5 6 6 1 ], dodecahedron[5 12 ] and the nineteen-sided [4 3 5 12 6 1 8 3 ] Three basic structures, the unit cell structure is hexagonal. Common angle [SiO 4 ] 4- A five-sided dodecahedron coplanar with [5 12 ] The fake six-sided layer composed of ] is connected. These toppings are stacked in the order ABCABC. between the layers by additional [SiO 4 ] 4- The six-membered rings are connected. The larger nineteen-sided structural units communicate through the eight-membered rings, forming a two-dimensional channel structure between the planes formed by the dodecahedrons. Among...

Claims

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Application Information

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IPC IPC(8): C01B39/46
Inventor 朱伟东彭安娜
Owner ZHEJIANG NORMAL UNIVERSITY
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