SSZ-13 molecular sieve having micropore-mesopore multi-level pore channel structure, synthesis method and applications thereof

A synthesis method and pore structure technology, applied in the direction of molecular sieves and base exchange compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of inapplicable porous structure synthesis, harsh control conditions of the synthesis process, etc., to shorten the diffusion distance, The effect of improving the adsorption capacity and wide application prospects

Active Publication Date: 2017-06-30
CHINA CATALYST HLDG CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The above-mentioned patents describe the synthesis method of Beta molecular sieve and ZSM-5 molecular sieve with multi-level pore structure. The control conditions of the synthesis process are relatively harsh, and cannot be applied to the synthesis of small-pore SSZ-13 molecular sieve with 8-membered ring CHA type porous structure.

Method used

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  • SSZ-13 molecular sieve having micropore-mesopore multi-level pore channel structure, synthesis method and applications thereof
  • SSZ-13 molecular sieve having micropore-mesopore multi-level pore channel structure, synthesis method and applications thereof
  • SSZ-13 molecular sieve having micropore-mesopore multi-level pore channel structure, synthesis method and applications thereof

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Experimental program
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Effect test

Embodiment 1

[0033] According to the listed in Table 1, the proportion of reaction raw materials weighed quantitative long-chain diquaternary ammonium salt surfactant and dissolved in methanol to form a solution and stirred to disperse, then added silicon source and alkali source, and stirred at 40°C for 6 hours , to obtain a silicon source mixed solution; at 60 ° C, according to the proportion of the reaction raw materials, the aluminum source solution was added dropwise to the silicon source mixed solution, after vigorous stirring for 90 minutes, it was left to stand and aged for 12 hours to obtain a mixture gel. Place the mixture gel in a hydrothermal synthesis kettle at 120-190°C for crystallization in two stages, the temperature of the second stage is 20°C higher than that of the first stage, after the crystallization is complete, centrifuge to separate the solid product, and then use the solid product Repeated washing with deionized water until neutral, then drying at 120°C for 24 hou...

Embodiment 2

[0041] The SSZ-13 molecular sieve samples 1-20 synthesized in Example 1 were characterized and analyzed using a Micromeritics ASAP 2020 nitrogen physical adsorption instrument. The pretreatment method of the sample before analysis is as follows: vacuumize the molecular sieve sample at room temperature, and when the vacuum condition is reached, treat it at 130°C for 2h; then treat it at 350°C for 2h. The nitrogen physical adsorption results show that samples 1-20 have a micropore diameter of 0.3-0.5nm and all contain mesoporous structures.

[0042] table 3

[0043]

[0044]

Embodiment 3

[0046] Samples 1-20 prepared in Example 1 were characterized by XRD to confirm that they were SSZ-13 molecular sieves. The instrument used is a PANalytical X’Pert X-ray diffractometer, a copper target, and a Kα radiation source. The operating voltage of the instrument is 40kv, and the operating current is 40mA. The obtained XRD spectrum of samples 1-20 and the characteristic spectrum of standard SSZ-13 molecular sieve Figure 1 Sincerely. Typical XRD patterns (such as figure 2 ) is represented by sample 1, and the positions and peak intensities of the main diffraction peaks at 2θ between 5° and 50° are shown in Table 4. Compared with sample 1, other sample data results have the same diffraction peak position and shape, and the relative peak intensity fluctuates within ±5% according to the change of synthesis conditions, indicating that the synthesized product has the characteristics of SSZ-13 molecular sieve structure.

[0047] Table 4

[0048] Characteristic pe...

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Abstract

The invention discloses a SSZ-13 molecular sieve having micropore-mesopore multi-level pore channel structure, a synthesis method and applications thereof. The synthesis method selects a long-chain double quaternary ammonium salt surfactant as a crystallization synthesis aid, and specially comprises: gelation and aging, crystallization, washing, template agent removing and activating, ion exchange and activation, and other steps so as to obtain the micropore-mesopore ordered-distribution high-crystallinity multi-level pore SSZ-13 molecular sieve. According to the present invention, the obtained molecular sieve has two sizes such as the mesopore pore size distribution of 2-5 nm and the mesopore pore size distribution of 5-15 nm, wherein the micro-pore volume is more than 0.20 cm<3> / g, the mesopore volume is more than 0.35 cm<3> / g, the specific surface area is more than 400 m<2> / g, and the yield of the crystallized product can achieve more than 85%; and the SSZ-13 molecular sieve has the advantages of the micropore zeolite, the macromolecule diffusion and the other advantages of the mesopore middle-macromolecules, and has wide application prospects in the fields of MTO reactions, tail gas catalytic reduction (SCR) reactions, and the like.

Description

technical field [0001] The present invention relates to a kind of microporous-mesoporous hierarchical porous SSZ-13 molecular sieve and its synthesis method, in particular to the introduction of long-chain diquaternary ammonium salt surfactant ions into the synthesized silica-alumina sol mixture as a crystallization aid, crystallization The SSZ-13 molecular sieve with a microporous-mesoporous hierarchical channel structure is gradually formed in the chemical reaction. Background technique [0002] The particle size of the molecular sieve obtained by the traditional preparation method is relatively large, which has a serious limitation on the catalytic life of the molecular sieve. The introduction of the concept of multi-stage pore molecular sieve shortens the molecular diffusion distance, makes it easier for the reaction product to diffuse from the active site to the outer surface, inhibits the formation of coke, and increases the life of the catalyst. The synthesis of mult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48B01J29/70C07C1/20C07C11/06C07C11/04
CPCB01J29/70C01B39/48C01P2002/72C01P2004/03C01P2006/12C01P2006/14C01P2006/17C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 王志光李进王炳春王建青刘国东刘宇婷史振宇张旭旺
Owner CHINA CATALYST HLDG CO LTD
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