Method for synthesizing aluminum-containing ITQ-13 molecular sieve with one-step method by linearpoly quaternary ammonium base organic template

An organic template, polyquaternium technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of limiting the wide application of zeolite molecular sieves, unfavorable hydrothermal stability, introduction of aluminum elements, etc. problems, to achieve good catalytic activity, good crystallinity and purity, and reduce the cost of preparation.

Active Publication Date: 2017-05-24
ZHEJIANG UNIV
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  • Application Information

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Problems solved by technology

However, since it was reported by the Corma research group in 2002, it has been difficult for researchers to directly introduce aluminum into its framework.
The existing methods of introducing aluminum either need to prepare silicon boron ITQ-13 first and then replace boron with aluminum, or need to introduce germanium species that are expensive and unfavorable to hydrothermal stability in the system, which limits ITQ-13 Wide range of applications of this potential zeolite molecular sieve with good properties

Method used

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  • Method for synthesizing aluminum-containing ITQ-13 molecular sieve with one-step method by linearpoly quaternary ammonium base organic template
  • Method for synthesizing aluminum-containing ITQ-13 molecular sieve with one-step method by linearpoly quaternary ammonium base organic template
  • Method for synthesizing aluminum-containing ITQ-13 molecular sieve with one-step method by linearpoly quaternary ammonium base organic template

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Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1: the synthesis of linear cheap polyquaternium organic template

[0022] According to the molar ratio of 1,4-dibromobutane and N,N,N,N-tetramethyl-1,6-hexanediamine as 1:1, weigh 10g of 1,4-dibromobutane and 12.5 Dissolve g N,N,N,N-tetramethyl-1,6-hexanediamine in 50ml of ethanol, set the temperature to reflux at 80°C, and stir for 12 hours; after the reaction, add enough ether to remove the crystal from the solvent Precipitate in; produce white solid precipitate after filtration, drying, obtain the quaternary ammonium salt corresponding to the linear polyquaternium base organic template agent T; this quaternary ammonium salt is dissolved in appropriate amount of water, with strong basic anion exchange resin The bromide ion in the quaternary ammonium salt is completely exchanged for hydroxide; the exchange resin is filtered off to obtain a linear polyquaternary ammonium base organic template agent T solution.

[0023] Strong basic anion exchange resin refer...

Embodiment 2

[0024] Embodiment 2: Synthesis of ITQ-13 zeolite by linear cheap polyquaternium base organic template

[0025] Put the solution containing the equivalent of 0.72mmol of quaternary ammonium base template (T), 0.96g of white carbon black, 0.024g of boehmite and 0.19g of 40% HF in a beaker and stir evenly, and evaporate the water to the expected ratio at room temperature , and then the gel was added to a polytetrafluoroethylene stainless steel reaction kettle, crystallized at 160°C for 10 days and then completely crystallized, and the product was filtered with suction and dried to obtain the product. The proportioning of reaction raw material is as follows:

[0026] 7H 2 O:SiO 2 :0.01Al 2 o 3 :0.23HF:0.045T

[0027] Through X-ray diffraction analysis, its structure is ITQ-13 zeolite molecular sieve belonging to ITH ( figure 1 ), and it can be seen from the scanning electron microscope that the synthesized product particles are round cakes with longitudinal protrusions in th...

Embodiment 3

[0028] Example 3: Synthesis of ITQ-13 zeolite at high temperature by linear cheap polyquaternium base organic template

[0029] Put a solution containing 0.5mmol of quaternary ammonium base template (T), 1g of solid silica gel and 0.15g of HF in a beaker and stir evenly, evaporate the water to a predetermined ratio at room temperature, and then add the gel to the polytetrafluoroethylene In an ethylene stainless steel reaction kettle, crystallize at 200°C for 2 days to complete crystallization, and the product is filtered with suction and dried to obtain the product. The proportioning of reaction raw material is as follows:

[0030] 10H 2 O:SiO 2 :0Al 2 o 3 :0.18HF:0.03T

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Abstract

The invention relates to a preparation technology of a zeolite molecular sieve and aims at providing a method for synthesizing an aluminum-containing ITQ-13 molecular sieve with a one-step method by a linearpoly quaternary ammonium base organic template. The method comprises the following steps: mixing a silicon source, an aluminum source, the linearpoly quaternary ammonium base organic template T and hydrofluoric acid or ammonium fluoride, uniformly stirring the mixture, placing the mixture in a reaction kettle for a crystallization reaction, and performing extraction filtration and drying on a product, so as to obtain raw powder of the ITQ-13 zeolite molecular sieve. The novel method for synthesizing the ITQ-13 zeolite molecular sieve by the linearpoly quaternary ammonium base organic template not only can greatly lower the using cost of the organic template, but also can broaden a synthesis phase region of the organic template to a great range. Aluminum is introduced into a framework of the ITQ-13 zeolite molecular sieve by one step without germanium, therefore, the operation complexity and the preparation cost are reduced; in addition, the product maintains good crystallinity and purity and has good catalysis reactivity.

Description

technical field [0001] The invention belongs to a molecular sieve preparation method, in particular to a novel linear polyquaternary ammonium base organic template agent to synthesize an aluminum-containing ITQ-13 zeolite molecular sieve in one step. Background technique [0002] Molecular sieves are widely used in catalysis, ion exchange, adsorption and separation due to their open structure and large surface area. In the synthesis of modern zeolite molecular sieves, mesoporous zeolite molecular sieves have attracted the attention of many researchers because of their good shape-selective properties. ITQ-13 is a molecular sieve with a 9×10×10-membered ring three-dimensional channel system. Due to its unique nine-membered ring structure, it has been proven to have unique performance in many catalytic reactions. However, since it was reported by Corma's research group in 2002, it has been difficult for researchers to directly introduce aluminum into its framework. The existi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04B01J29/70
CPCB01J29/70C01B39/04C01P2002/72C01P2002/86C01P2004/03
Inventor 孟祥举吴勤明肖丰收陈芳
Owner ZHEJIANG UNIV
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