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Modification method of framework silicon-rich zeolite molecular sieve

A technology of silica-rich zeolite and molecular sieve, applied in the field of molecular sieve material preparation, can solve the problems of blocking molecular sieve channels and the like

Active Publication Date: 2021-06-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the platinum distributed on the molecular sieve aggregates during the reduction process, forming particles with a particle size of more than 1 nm, which block the pores of the molecular sieve.

Method used

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  • Modification method of framework silicon-rich zeolite molecular sieve
  • Modification method of framework silicon-rich zeolite molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0031] The ZSM-22 molecular sieve was prepared according to the procedure described in the literature Applied Catalysis A: General, 2017, 537:59, and the obtained zeolite molecular sieve powder was calcined at 550°C for 6 hours. X-ray fluorescence spectroscopic analysis results show that the silicon-aluminum ratio of the zeolite molecular sieve is 36, that is, the skeleton Si 4+ The number of ions accounts for 97% of the total number of skeleton cations.

[0032] Add 10 g copper nitrate (Cu(NO 3 ) 2 ·3H 2 (2) and 88g ethanol, after copper nitrate is completely dissolved, add ZSM-22 molecular sieve 5g wherein to carry out ion exchange. It can be observed that the zeolite molecular sieve quickly sinks and disperses in the solution after being put into the flask. Under the condition of 450rpm magnetic stirring, the above mixture was heated with an oil bath, and the temperature of the oil bath was kept at 78° C. for 36 hours. After the above mixture was cooled, it was suction...

Embodiment 2

[0035] Sn-Beta molecular sieves were prepared according to the procedures described in the literature Microporous and Mesoporous Materials, 2017, 247:158. The obtained zeolite molecular sieve raw powder was calcined at 550°C for 10 hours, pressed into tablets, crushed, and sieved to obtain 20-40 mesh particles. The results of inductively coupled plasma emission spectrometry analysis show that the silicon-tin ratio of the zeolite molecular sieve is 111, that is, the framework Si 4+ The number of ions accounts for 99% of the total number of skeleton cations.

[0036] 25g lanthanum nitrate (La(NO 3 ) 3 ·6H 2 O) be dissolved in 65g of methoxyethanol and make dipping liquid. Take 10 g of Sn-Beta molecular sieve particles for incipient wetness impregnation, and consume a total of 7 mL of impregnation solution. After impregnation, seal the zeolite molecular sieve and let it stand for 10 minutes. Dry at 150°C and bake at 550°C for 12 hours to obtain lanthanum-modified Sn-Beta mol...

Embodiment 3

[0039] According to the procedure described in the document Dalton Transactions, 2016, 45(15): 6634, the all-silicon Beta molecular sieve was prepared, and the obtained zeolite molecular sieve raw powder was calcined at 550°C for 5 hours. The framework Si in the zeolite molecular sieve 4+ The number of ions accounts for 100% of the total number of framework cations.

[0040] 8g zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 12g chromium nitrate (Cr(NO 3 ) 3 ) was dissolved in 80g of ethylene glycol to make an impregnation solution. Take 20g of all-silicon Beta molecular sieve for excessive impregnation, and consume a total of 36mL of impregnation solution. After impregnation, filter the zeolite molecular sieve under normal pressure and leave it open for 7 hours. Dried at 200°C and calcined at 550°C for 12 hours to obtain zinc-chromium-modified all-silicon Beta molecular sieve. The crystal structure of Beta molecular sieve can be clearly distinguished from the transmission electro...

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Abstract

The invention belongs to the technical field of molecular sieve material preparation, and relates to a modification method of a framework silicon-rich zeolite molecular sieve. The method is characterized by comprising the step of contacting an alcoholic solution of nitrate with a framework silicon-rich zeolite molecular sieve. Alcohol is used as a modifier solvent, so that the modifier is uniformly dispersed on the surface of the framework silicon-rich zeolite molecular sieve; nitrate is used as a modified species raw material, so that metal ions in the modifier are small in size and can enter zeolite molecular sieve pores. Alcohol and nitrate used in the method are cheap and easy to obtain, and the modification process is simple and convenient to operate. Metal species in the obtained modified framework silicon-rich zeolite molecular sieve are uniformly distributed.

Description

technical field [0001] The invention relates to a method for modifying a skeleton silicon-rich zeolite molecular sieve, and belongs to the technical field of molecular sieve material preparation. Background technique [0002] Zeolite molecular sieves have regular channels with high specific surface area and molecular size, and are widely used in catalysis, adsorption and separation processes. The zeolite molecular sieve framework consists of a central cation and four O 2- Tetrahedral connections of ions; the central cation is usually Si 4+ 、Al 3+ , can also be B 3+ , Sn 4+ Isomain group ions or Ti 4+ 、Cr 3+ , Fe 3+ 、Zr 4+ and other transition metal ions. With the increase of the silicon content of the framework, the heat resistance, water vapor resistance and acid resistance of the zeolite molecular sieve are correspondingly improved; moreover, the negative charge of the silicon-rich zeolite molecular sieve framework is less, making the surface of the pore channel h...

Claims

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Application Information

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IPC IPC(8): C01B39/02
CPCC01B39/026C01P2002/72C01P2004/04Y02P20/52
Inventor 刘浩田志坚王从新马怀军王琳陈欣
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI