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Molecular sieve and preparation method thereof

A molecular sieve and quality technology, applied in the direction of molecular sieve catalysts, molecular sieves and base exchange compounds, chemical instruments and methods, etc., can solve the problems of weak catalytic ability of molecular sieves, and achieve excellent hydrothermal aging resistance and good catalytic activity.

Active Publication Date: 2020-10-13
BAOTOU RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all adopt a one-step hydrothermal method to synthesize molecular sieves. The crystal structure of the molecular sieves obtained is non-football type, and the catalytic ability of molecular sieves at high and low temperatures is relatively weak.

Method used

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  • Molecular sieve and preparation method thereof
  • Molecular sieve and preparation method thereof
  • Molecular sieve and preparation method thereof

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preparation example Construction

[0055]

[0056] The preparation method of the molecular sieve of the present invention comprises the following steps: (1) the step of the first hydrothermal synthesis reaction; (2) the step of the second hydrothermal synthesis reaction; (3) the step of the third hydrothermal synthesis reaction; (4) The step of roasting. The composition and properties of the resulting molecular sieves are as described above. Detailed description will be given below.

[0057] Steps of the first hydrothermal synthesis reaction

[0058] The template agent, the alkali metal inorganic base, the silicon source, the aluminum source and water form the first mixture, and the first hydrothermal synthesis reaction is carried out.

[0059] The aluminum source of the present invention may be selected from one or more of pseudoboehmite, aluminum hydroxide, aluminum sol or sodium metaaluminate. Preferably, the aluminum source is selected from one or more of aluminum sol or sodium metaaluminate. More p...

Embodiment 1

[0082](1) 28.4g N, N, N-trimethyladamantyl ammonium (TMAda-OH) aqueous solution (concentration is 25wt%), 4.8g sodium hydroxide and 85g water are heated and refluxed at 60 ℃ and mixed uniformly, and then mixed with 32.9 g silica sol (solid content is 20wt%, pH is 3.2, density is 1.2g / cm 3 , with a particle size of 11 nm) and 1.17 g of sodium metaaluminate were stirred and mixed for 2 hours to form a first mixture, which was subjected to the first hydrothermal synthesis reaction at a reaction temperature of 110° C. and a reaction time of 2 days.

[0083] (2) The reaction product of step (1) was cooled to 30°C, then stirred and mixed with 3.43g ammonium nitrate for 8h, then added 8.9g chelated copper glutamic acid and stirred for 3h to form a second mixture, and the second mixture was carried out For the second hydrothermal synthesis reaction, the reaction temperature is 80° C. and the reaction time is 10 h.

[0084] (3) Stir and mix the reaction product obtained in step (2) wi...

Embodiment 2

[0087] (1) 34.4g N, N, N-trimethyladamantyl ammonium (TMAda-OH) aqueous solution (concentration is 25wt%), 6.72g potassium hydroxide and 85g water are heated and refluxed at 50 ℃ and mixed uniformly, and then mixed with 28.5 g silica sol (solid content is 20wt%, pH is 5.6, density is 1.5g / cm 3 , particle size is 11nm) and 7.28g aluminum sol (solid content is 10wt%, pH is 4, viscosity is 43mPa·s, particle size is 10nm) stirring and mixing 3h, forms the first mixture, the first mixture is carried out the first time For the hydrothermal synthesis reaction, the reaction temperature is 130° C., and the reaction time is 3 days.

[0088] (2) Cool the reaction product of step (1) to 25°C, then stir and mix with 4.57g of ammonium nitrate for 8h, then add 8.6g of copper acetate and stir and mix for 3h to form a second mixture, which is subjected to the second water Thermal synthesis reaction, the reaction temperature is 70°C, and the reaction time is 13h.

[0089] (3) Stir and mix the...

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Abstract

The invention discloses a molecular sieve and a preparation method thereof. The molecular sieve has a football-shaped microstructure and is composed of a molecular sieve framework and active elements,the molecular sieve framework comprises a silicon element and an aluminum element, the active elements comprise a copper element and a rare earth element(s), and the rare earth element(s) are selected from one or more of La, Ce, Pr, Nd, Pm, Sm, Eu, Sc and Y. The mass ratio of the silicon element to the aluminum element is (3-9): 1, the content of the copper element in the molecular sieve is 1.5-3.2 wt%, and the mass of the rare earth element(s) is 50ppm-2wt% of the molecular sieve framework. The mass of the silicon element is metered by silicon dioxide, the mass of the aluminum element is metered by aluminum oxide, the mass of the copper element is metered by copper oxide, and the mass of the rare earth element(s) is metered by rare earth oxide. The molecular sieve has good catalytic activity at the temperature of 175-550 DEG C, and has excellent hydrothermal aging resistance.

Description

technical field [0001] The invention relates to a molecular sieve and a preparation method thereof. Background technique [0002] Zeolite molecular sieve materials are widely used in the fields of adsorption, separation and catalysis due to their high stability, regular and uniform pores, and adjustable acidity and alkalinity. The selective catalytic reduction technology of molecular sieves loaded with transition metals such as Cu for the elimination of nitrogen oxides has been developed rapidly. Rare earth elements can further improve the catalytic activity of molecular sieve catalysts. [0003] CN110102337A discloses a method for preparing a composite copper-based SCR molecular sieve catalyst. Mix N,N,N-trimethyladamantane ammonium with water, stir, then add aluminum sulfate, stir, adjust the pH value with alkali, then add silica sol, stir to obtain the initial gel mixture; the initial gel mixture Crystallization at constant temperature, cooling, washing, drying, and ro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/03C01P2004/32C01B39/48C01B39/026B01J29/7065B01J35/1023B01J35/1028B01J35/1038B01J35/1042B01J35/1057B01J37/06B01J37/10B01J37/346B01J2219/1948F01N3/0842F01N3/2066F01N2370/04
Inventor 王艳李兆强丁智勇樊蓉蓉张丞王雨郭欣康娜刘威王荣宋静
Owner BAOTOU RES INST OF RARE EARTHS
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