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Composite pore molecular sieve and preparation method thereof

A molecular sieve and composite pore technology, applied in the direction of molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc. Poor adaptability and other issues

Active Publication Date: 2020-09-11
BAOTOU RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN107027805A prepares nano-scale molecular sieves through ultrasonic vibration and microwave ultraviolet treatment, but its universality is poor
The above-mentioned patent documents use an alkali treatment, which easily leads to the destruction of the molecular sieve structure, and cannot form a multi-level mesopore and microporous structure.

Method used

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  • Composite pore molecular sieve and preparation method thereof
  • Composite pore molecular sieve and preparation method thereof
  • Composite pore molecular sieve and preparation method thereof

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preparation example Construction

[0029] The composite pore molecular sieve of the present invention is a molecular sieve with mesoporous and microporous structures, and its preparation method includes the steps of pretreatment, primary lye treatment, secondary lye treatment and the like.

[0030] The molecular sieve is contacted with a reagent containing silicon tetrahalide or ammonium fluorosilicate to form a pretreated molecular sieve. During the contacting process, the molecular sieve reacts with silicon tetrahalide or ammonium fluorosilicate. The reaction temperature is 60-90°C, preferably 70-80°C. The contact time may be 1-3 h, preferably 1-2 h. According to one embodiment of the present invention, the molecular sieve is added into the reagent and fully stirred, and the pretreated molecular sieve is obtained after cooling, filtering, washing with water and drying. All of these can adopt conventional operations in the art, and will not be repeated here.

[0031] The molecular sieve of the present inven...

preparation example 1

[0047] The preparation of preparation example 1 Cu-SSZ-13 molecular sieve

[0048] 1) Al 2 o 3 , SiO 2 、Na 2 O and water are 1:50:30:1500 mixed evenly according to the mass ratio of substances to obtain a mixture, and then in the N,N,N-trimethyl-1-adamantyl ammonium hydroxide template (30wt% of the mixture mass) In the presence of the reaction at 40 ° C for 5 h.

[0049] 2) Transfer the product of step 1) to an autoclave, crystallize at 150° C. for 56 h, cool, filter to obtain the crystallized product, wash, dry and roast to obtain SSZ-13 molecular sieve.

[0050] 3) Disperse the SSZ-13 molecular sieve in step 2) in 0.5mol / L ammonium nitrate solution, stir at 80°C for 12h, cool, filter, wash, dry and roast to obtain H-SSZ13;

[0051] 4) Disperse H-SSZ13 in step 3) in 1mol / L copper nitrate solution, stir at 80°C for 12h, cool, filter, wash, dry and roast to obtain Cu-SSZ-13 molecular sieve.

Embodiment 1

[0053] (1) Add 28.58g of Cu-SSZ-13 molecular sieve (preparation example 1) to SiCl with a mass ratio of 1:20 4 In a mixture with ethyl orthosilicate (250ml), SiCl 4 The mass ratio to molecular sieve was 1:20, stirred at 80°C for 2 hours, cooled to room temperature, filtered, and the filter residue was washed with water and dried to obtain a pretreated molecular sieve.

[0054] (2) Add the pretreated molecular sieve into an aqueous solution of 12wt% tetrapropylammonium hydroxide (TPAOH), stir at 100° C. for 10 h, cool to room temperature, filter, wash the filter residue with water and dry to obtain a primary treated molecular sieve.

[0055] (3) Add the primary treated molecular sieve into 0.1mol / L NaOH solution, stir at 70°C for 3h, cool to room temperature, filter, wash the filter residue with 0.1mol / L hydrochloric acid solution, then wash with water, and then roast at 550°C for 8h , Composite pore molecular sieve A was prepared.

[0056] The properties of the obtained comp...

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Abstract

The invention discloses a composite hole molecular sieve and a preparation method thereof. The preparation method of the composite hole molecular sieve comprises the following steps: (1) making a molecular sieve be in contact with a reagent containing silicon tetraauragen or ammonium fluorosilicate to form a pretreatment molecular sieve; (2) making the pretreatment molecular sieve be in contact with a first alkali solution to form a primary treatment molecular sieve; (3) making the primary treatment molecular sieve be in contact with a second alkali solution, cleaning pore canals of a preparedproduct with an acid solution, and performing calcining to obtain the composite hole molecular sieve. By adopting the method, a part close to the surface of the molecular sieve can be formed into a mesoporous-microporous composite structure, and a part far away from the surface of the molecular sieve can be formed into a microporous structure.

Description

technical field [0001] The invention relates to a molecular sieve and a preparation method thereof, in particular to a composite pore molecular sieve which can be used for catalytic denitrification of motor vehicle tail gas and a preparation method thereof. Background technique [0002] As a porous material, microporous molecular sieves are widely used in industrial catalysis, but the direct use of microporous molecular sieves has great limitations, because the typical microporous molecular sieve channel size is less than 1nm, which is not conducive to the reaction of reactant molecules and products. The circulation and diffusion properties of molecules in the catalytic process greatly limit the application range of molecular sieves. The mesoporous structure is introduced into the synthesis system of traditional microporous molecular sieves to form composite pore molecular sieves, which can make the molecular sieves have high diffusion, anti-carbon deposition and anti-cloggi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02C01B39/14
CPCC01B39/02C01B39/026C01B39/14C01P2004/03C01P2004/04C01P2006/12C01P2006/14C01P2006/16
Inventor 赵文怡郭欣张舒乐张丞樊蓉蓉王荣王艳李兆强王雨丁智勇宋立华宋燕海
Owner BAOTOU RES INST OF RARE EARTHS
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