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Has multi-level porous ssz-13 molecular sieve catalyst and its synthesis method and application

A synthesis method and molecular sieve technology, which are applied to molecular sieve catalysts, including molecular sieve catalysts, molecular sieves and alkali exchange compounds, etc., can solve the problems of molecular sieve catalytic life limitation and large molecular sieve particle size.

Active Publication Date: 2019-03-19
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The SSZ-13 molecular sieve obtained by the traditional preparation method has a relatively large particle size, which has a serious limitation on the catalytic life of the molecular sieve

Method used

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  • Has multi-level porous ssz-13 molecular sieve catalyst and its synthesis method and application
  • Has multi-level porous ssz-13 molecular sieve catalyst and its synthesis method and application
  • Has multi-level porous ssz-13 molecular sieve catalyst and its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] According to the ratio listed in Table 1, the ratio of the reaction raw materials was weighed and the quantitative long-chain organosilane was dissolved in methanol to form a solution and stirred to disperse, then the silicon source and the alkali source were added, and stirred at 40°C for 6 hours.

[0029] A silicon source mixed solution was obtained; at 60° C., the aluminum source solution was added dropwise to the silicon source mixed solution according to the ratio of the reaction raw materials, and after vigorous stirring for 90 minutes, the mixture was left to age 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°...

Embodiment 2

[0037]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 0.3-0.5 nm, and all contain mesopore diameter distribution, mesopore average pore diameter, mesopore volume and specific surface area as shown in Table 3.

[0038] table 3

[0039]

[0040]

Embodiment 3

[0042] 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 1 ) 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.

[0043] Table 4

[0044]

[0045]

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Abstract

The invention discloses a hierarchical porous SSZ-13 molecular sieve catalyst, a method for synthesizing the same and application of the hierarchical porous SSZ-13 molecular sieve catalyst. The method includes that long-chain silane is selected to be used as an auxiliary for crystallization synthesis reaction, molar ratios of alkali sources, silicon sources, aluminum sources, template agents, the long-chain silane and water are regulated, and segmented dynamic / static crystallization modes are adopted. Synthesizing procedures include steps of gel forming and aging, crystallizing, washing, template agent removing and activating, ion exchanging and activating and the like. High-crystallinity hierarchical porous SSZ-13 molecular sieves with micropore-mesopore ordered distribution can be obtained by the aid of the method. The obtained molecular sieves have distribution of two types of pore sizes in a 2-5 nm range and a 5-15 nm range, the volumes of micropores are larger than 0.20 cm<3> / g, the volumes of mesopores are larger than 0.35 cm<3> / g, the specific surface areas are larger than 400 m<2> / g, and the yield of crystallization products can reach 85% at least. The hierarchical porous SSZ-13 molecular sieve catalyst, the method and the application have the advantages that the SSZ-13 molecular sieves not only have merits of micropore zeolite, but also have merits of mesopore materials which have large pore sizes and are favorable for macromolecule diffusion, the hierarchical porous SSZ-13 molecular sieve catalyst has a broad application prospect in the fields of petrochemical engineering, MTO (methanol to olefin) reaction, tail gas purification and fine chemical engineering, and the like.

Description

technical field [0001] The present invention relates to a kind of SSZ-13 molecular sieve catalyst with microporous-mesoporous multi-level channels and its synthesis method and application, specifically relates to the addition of long-chain organosilane in the initial silica-alumina gel mixture as a crystallization aid, during the crystallization process The SSZ-13 molecular sieve gradually formed a microporous-mesoporous hierarchical channel 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 mol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70C01B39/48C07C1/20C07C11/06C07C11/04
CPCB01J29/70C01B39/48C01P2002/72C01P2004/03C07C1/20C07C2529/70C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 王志光王建青王贤彬刘国东李进王炳春史振宇刘宇婷
Owner CHINA CATALYST HLDG CO LTD
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