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A kind of molecular sieve with hierarchical pores and wide silicon-aluminum ratio eu-1 and its preparation method

An EU-1, molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of molecular sieve catalytic life limitation, prone to miscellaneous crystals, product yield to be improved, etc. Cost and environmental protection, small grain size, wide range of feeding effects

Active Publication Date: 2020-08-21
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 hierarchical pores and wide silicon-aluminum ratio eu-1 and its preparation method
  • A kind of molecular sieve with hierarchical pores and wide silicon-aluminum ratio eu-1 and its preparation method
  • A kind of molecular sieve with hierarchical pores and wide silicon-aluminum ratio eu-1 and its preparation method

Examples

Experimental program
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Embodiment 1

[0047] A preparation method of EU-1 molecular sieve with multiple pores and wide silicon-to-aluminum ratio, which is proud of its characteristics and includes the following steps:

[0048] (1) Preparation of mixed sol: deionized water H 2 O, NaOH particles, 1,6-bis(N-methylpiperidinium) hexane organic template are uniformly mixed into a solution and mixed into a solution, and then silica sol (SiO2: 26.49wt%), pseudo-boehmite (Al2O3: 66wt%) and boric acid were gradually added to the above solution in batches under thorough stirring and vigorously shaken at room temperature for 1 hour to obtain a mixed sol. The molar ratio of each material in the mixed sol: Na 2 O: SiO 2 : Al 2 O 3 : B 2 O 3 : OSDA: H 2 O=0.07:1:0.04098:0.036:0.14:40;

[0049] (2) Crystallization: Place the mixed sol obtained in step (1) in a crystallization kettle and crystallize at 170°C for 72 hours. The crystalline product is filtered and the solid product is separated. The solid product is subjected to deionized ...

Embodiment 2~8

[0053] The types of silicon source, alkali source, aluminum source, boron source, double quaternary ammonium salt template OSDA, acid and ammonium salt selected in Examples 2-8 are shown in Table 1, and the same process method as in Example 1 is used. Preparation, the obtained molecular sieve crystallization precursor mixture slurry molar composition is shown in Table 1, the process parameters are shown in Table 2, and the physical and chemical characterization parameters of the obtained product are shown in Table 3:

[0054] Table 1: Types of materials in Examples 1-8

[0055] Example Silicon source Aluminum source Boron source Types of organic template Acid type Types of ammonium salt Example 1 Water glass Pseudo-boehmite Boric acid 1,6-bis(N-methylpiperidinium)hexane Nitric acid Ammonium Chloride Example 2 Silica sol Aluminum Nitrate Sodium borate 1,6-bis(N-methylpiperazinium)hexane hydrochloric acid Ammonium Sulfate Example 3 Ethyl silicate Aluminum sulfate Boron oxide 1...

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Abstract

The invention discloses an EU-1 molecular sieve with multi-stage pores and a wide silicon-aluminum ratio and a preparation method thereof. The preparation method comprises: uniformly mixing a siliconsource, an alkali source, an aluminum source, a boron source, a double quaternary ammonium salt template agent OSDA and deionized water to obtain mixed sol, crystallizing the mixed sol at 160-200 DEGC, carrying out separation, washing, drying and roasting to remove the organic template and to obtain an EU-1 molecular sieve with a skeleton containing boron, carrying out reflux washing through an acid solution to remove boron, carrying out separation, washing and drying on the product to obtain an EU-1 molecular sieve with a skeleton without boron, and orderly carrying out aluminum ion exchange, drying and roasting to obtain the EU-1 molecular sieve with multi-stage pores and a wide silicon-aluminum ratio. The zeolite molecular sieve has a multi-stage pore structure, and has a wide range ofa silicon-aluminum ratio, small crystal grain sizes, high relative crystallinity and high hydrothermal stability. The reaction evaluation result shows that the EU-1 molecular sieve has good xylene isomerization activity and selectivity and has a good industrial application prospect.

Description

Technical field [0001] The invention relates to an EU-1 molecular sieve with multiple pores and wide silicon-to-aluminum ratio and a preparation method thereof, belonging to the field of inorganic material synthesis. Background technique [0002] The crystal structure of EUO type topological structure molecular sieve has a one-dimensional 10-membered ring 0.54nm×0.41nm pores in the [100] direction, and a 0.81nm deep twelve-membered ring 0.68nm×0.58nm side pockets on both sides of the 10-membered ring pores . EU-1, ZSM-50 and TPZ-3 molecular sieves all have EUO-type topological structures. EU-1 molecular sieves are widely studied in recent years. Due to their special pore structure and acidic characteristics, they are regarded as carbon eight aromatic hydrocarbons. The bifunctional catalyst prepared by the acid component of the structured catalyst shows good activity and selectivity in the hydroisomerization of carbon eight aromatics and the isopropylation of benzene. It is known...

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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