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A kind of molecular sieve with multi-level pores and wide silicon-aluminum ratio euo structure and its synthesis method

A synthesis method and multi-stage pore technology, applied in molecular sieves and base exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of limited catalytic life of molecular sieves, prone to miscellaneous crystals, and product yields to be improved. Facilitate the implementation of industrialization, the effect of small grain size and wide feeding range

Active Publication Date: 2020-04-03
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The EUO structure molecular sieve preparation methods disclosed in the above documents mainly include traditional hydrothermal method and solid-phase in-situ method, but the molecular sieve structure is basically the same, its particle size is generally large, all in the micron level, and miscellaneous crystals are prone to appear. The lifespan is severely limited, and the product yield needs to be improved

Method used

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  • A kind of molecular sieve with multi-level pores and wide silicon-aluminum ratio euo structure and its synthesis method
  • A kind of molecular sieve with multi-level pores and wide silicon-aluminum ratio euo structure and its synthesis method
  • A kind of molecular sieve with multi-level pores and wide silicon-aluminum ratio euo structure and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A method for synthesizing a molecular sieve with hierarchical pores and a wide silicon-aluminum ratio EUO structure, comprising the following steps:

[0053] (1) Preparation of mixed sol: take quantitative cetyltrimethoxysilane and dissolve it in methanol to form a solution and stir to disperse to form a solution of cetyltrimethoxysilane; Add quantitative water glass, NaOH, 1,6-bis(N-methylpiperidinium) hexane and deionized water H to the silane solution 2 O, to obtain a silicon source mixed solution; under the condition of 60°C, put quantitative pseudo-boehmite into the silicon source mixed solution, stir vigorously for 90 minutes, and leave it at room temperature for 12 hours to obtain a mixed mixed sol, which is used as Crystallization precursor mixture, which consists of:

[0054] Na 2 O:SiO 2 :Al 2 o 3 :LCS:OSDA:H 2 O=0.072:1:0.0342:0.0247:0.12:45.

[0055] (2) Crystallization: The mixed sol obtained in step (1) is placed in a crystallization kettle, and cry...

Embodiment 2-8

[0066] Synthesize using the same synthesis method as in Example 1, the selected silicon source, aluminum source, long-chain organosilane, biquaternary ammonium salt template type and feeding ratio, heating rate, crystallization temperature, crystallization time and other parameters Selection, referring to Table 2; the physical and chemical properties of the products EUO-2~EUO-8 prepared in Example 2-8 are as shown in Table 3:

[0067] Table 2: Selection of parameters in the EU-1 molecular sieve synthesis method in the examples

[0068]

[0069]

[0070] Table 3: Physical and chemical properties of EU-1 molecular sieve products synthesized in Examples and Comparative Examples

[0071] Example / Comparative example Molecular sieve sample name EU-1 silicon aluminum ratio Mesopore average / nm Micropore volume / ml Mesopore volume / ml Specific surface area / (m 2 / g)

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Abstract

The invention discloses a EUO (Europium Oxide) structural molecular sieve with hierarchical pores and wide silica-alumina ratio and a synthetic method. The synthetic method comprises the following steps: performing crystallization synthesis by taking a long-chain silane compound as a crystallization assistant, taking double quaternary ammonium salt with an alkane structure being substituted by a double quinary heterocyclic group as an organic template, and heating silica-aluminum sol to a target temperature at the rate of 2 to 20 DEG C / h, wherein the target crystallization synthesis temperature is 150 to 200 DEG C; then performing separation, washing, drying and roasting to remove the organic template in order to obtain EUO structural molecular sieve raw powder with hierarchical pores andwide silica-alumina ratio, and performing ammonium ion exchange, drying and roasting in sequence to obtain an H-type EUO structural molecular sieve with hierarchical pores and wide silica-alumina ratio. The zeolite molecular sieve provided by the invention has the advantages of hierarchical pore structure, wide silica-alumina ratio range, small grain size, high relative crystallinity and high hydrothermal stability. Reaction evaluation shows high isomerization activity and selectivity of xylene, so that the EUO structural molecular sieve has a very good industrial application prospect.

Description

technical field [0001] The invention relates to a molecular sieve with multi-level pores and a wide silicon-aluminum ratio EUO structure and a synthesis method, belonging to the field of inorganic material synthesis. Background technique [0002] In the crystal structure of the EUO topological structure molecular sieve, there is a one-dimensional ten-membered ring 0.54nm×0.41nm channel in the [100] direction, and there are 0.81nm deep twelve-membered ring 0.68nm×0.58nm side pockets on both sides of the ten-membered ring channel. . EU-1, ZSM-50 and TPZ-3 molecular sieves all have EUO topology, among which EU-1 molecular sieve is a molecular sieve that has been widely studied in recent years. The bifunctional catalyst prepared by the acidic component of the structure catalyst shows good activity and selectivity in the catalytic reaction of C8 aromatics hydroisomerization and benzene isopropylation, and is known as a new generation of xylene isomerization preferred catalyst m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72C01P2004/03C01P2006/12C01P2006/14C01P2006/16
Inventor 王志光王建青王炳春李进
Owner CHINA CATALYST HLDG CO LTD
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