Hierarchical porous ssz-13 molecular sieve with micropores and mesopores and its synthesis method and application

A synthesis method and molecular sieve technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of inapplicable porous structure synthesis, harsh control conditions of the synthesis process, etc., to reduce production costs, Wide application prospects, the effect of broad application prospects

Active Publication Date: 2019-08-06
CHINA CATALYST HLDG CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] 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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  • Hierarchical porous ssz-13 molecular sieve with micropores and mesopores and its synthesis method and application
  • Hierarchical porous ssz-13 molecular sieve with micropores and mesopores and its synthesis method and application
  • Hierarchical porous ssz-13 molecular sieve with micropores and mesopores and its synthesis method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] According to the list in Table 1, the reaction raw material ratio weighs quantitative polyquaternium salt and dissolves it in deionized water to form a solution, stirs and disperses, then adds silicon source and alkali source, and stirs at 40 ° C for 6 hours to obtain silicon source Mixed solution; at 60°C, add the aluminum source solution dropwise to the silicon source mixed solution according to the proportion of the reaction raw materials, stir vigorously for 90 minutes, and then stand and age for 12 hours to obtain the 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 hours, and roasting at 550°C for 4 hours to remove the organic t...

Embodiment 2

[0061] 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 micropores with a diameter of 0.3-0.5 nm, all of which contain mesoporous structures.

[0062] table 3

[0063]

[0064]

Embodiment 3

[0066] 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 image 3 ) 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.

[0067] Table 4

[0068] Characteristic pea...

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Abstract

The invention discloses a hierarchical-pore-structured SSZ-13 molecular sieve with micropores and mesoporouses as well as a synthetic method and application thereof. According to the synthetic method, polyquaternium is selected as a crystallization synthesis reaction aid, the molar ratio of an alkali source to a silicon source to an aluminum source to a template agent to polyquaternium to water is regulated, and a segmented dynamic / static crystallization manner is adopted. The synthetic method comprises the following specific steps: glue formation, ageing, crystallization, washing, template agent removal, activation, ion exchange, activation and the like. By virtue of the synthetic method, the high-crystallinity-degree hierarchical-pore SSZ-13 molecular sieve with uniformly-distributed micropores and mesoporous can be obtained. The obtained molecular sieve has two mesoporous size distribution in two size ranges of 2nm-5nm and 5nm-15nm, the volumes of micropores are more than 0.20cm<3> / g, the volumes of the mesoporouses are more than 0.35cm<3> / g, the specific surface area is more than 400m<2> / g, and the yield of a crystallized product can reach 85% or above. The SSZ-13 molecular sieve has the advantages of micropore zeolite and further has the advantages of macromolecule diffusivity in the mesoporouses and the like. The SSZ-13 molecular sieve has wide application prospects in the fields of petrochemical engineering, MTO (Methanol To Olefin) reaction, tail gas purification, fine chemical engineering and the like.

Description

technical field [0001] The invention provides a micropore-mesoporous hierarchical SSZ-13 molecular sieve and a synthesis method thereof, specifically relates to the introduction of polyquaternium salt ions as crystallization aids in the synthesis of silica-alumina sol mixtures, which are gradually formed during the crystallization reaction SSZ-13 molecular sieve with microporous-mesoporous hierarchical pore structure. 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 multi-stage pore molecular sieves has received extensiv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04B01J29/70B01J35/10
CPCB01J29/70B01J35/1019B01J35/1023B01J35/1038B01J35/1057B01J35/1061C01B39/04C01P2002/72C01P2004/03
Inventor 王志光刘国东王建青王贤彬李进王炳春刘宇婷史振宇
Owner CHINA CATALYST HLDG CO LTD
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