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Method for synthesizing rare-earth containing MFI zeolite

A synthesis method and rare earth technology, applied in the field of synthesis of MFI zeolite, can solve the problem of low rare earth content

Active Publication Date: 2016-04-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is the problem of low rare earth content in MFI zeolite crystals in the prior art

Method used

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  • Method for synthesizing rare-earth containing MFI zeolite
  • Method for synthesizing rare-earth containing MFI zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 2 grams of Magadiite with a silicon-aluminum ratio of 200 (molar ratio) are mixed with 30 milliliters of 1mol / L La(NO 3 ) 3 solution, the mixture is stirred at room temperature for 18 hours, then washed, separated and dried to obtain a mixture containing La Magadiite material.

[0030]Mix 1.8 grams of the above-mentioned Magadiite material containing La with 0.0074 grams of sodium metaaluminate, 0.27 grams of NaOH, 1.04 grams of tetrapropylammonium bromide and 10 ml of water. After crystallization in the system for 48 hours, the crystallized product obtained becomes MFI zeolite containing rare earth after washing, separation, drying and roasting. Its XRD spectrum is as follows: figure 1 As shown, the La in the zeolite 2 o 3 The content is 24.5%.

Embodiment 2

[0032] 2 grams of Magadiite with a silicon-aluminum ratio of 200 (molar ratio) are mixed with 30 milliliters of 1mol / L La(NO 3 ) 3 solution, the mixture is stirred at room temperature for 18 hours, then washed, separated and dried to obtain a mixture containing La Magadiite material.

[0033] Mix 1.8 grams of the above-mentioned Magadiite material containing La with 0.0074 grams of sodium metaaluminate, 0.27 grams of NaOH, 1.04 grams of tetrapropylammonium bromide and 10 ml of water. After crystallization in the system for 96 hours, the obtained crystallized product becomes a rare earth-containing MFI zeolite after washing, separation, drying and roasting, and the La in the zeolite 2 o 3 The content is 22.8%.

Embodiment 3

[0035] 2 grams of Magadiite with a silicon-aluminum ratio of 200 (molar ratio) are mixed with 30 milliliters of 1mol / L La(NO 3 ) 3 solution, the mixture is stirred at room temperature for 18 hours, then washed, separated and dried to obtain a mixture containing La Magadiite material.

[0036] 1.8 grams of the above-mentioned Magadiite material containing La were uniformly mixed with 0.23 grams of NaOH, 1.04 grams of tetrapropylammonium bromide and 10 ml of water, and the resulting mixture was crystallized in a closed system at a temperature of 170 ° C for 48 hours to obtain After washing, separating, drying and roasting, the crystallized product becomes the rare earth-containing MFI zeolite, and the La in the zeolite 2 o 3 The content is 23.5%.

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Abstract

The invention relates to a method for synthesizing rare-earth containing MFI zeolite. The method is mainly used for solving the problem in the prior art that the content of rare earths in MFI zeolite crystals is low. According to the method for synthesizing the rare-earth containing MFI zeolite, by adopting the technical scheme that the rare-earth containing MFI zeolite is obtained through mixing a rare-earth containing sheet silicate material, an aluminum source, a template agent and an alkali in water in accordance with that the mole ratio of SiO2 in the sheet silicate material to Al2O3 in the aluminum source to M2O in an alkali source to the template agent to H2O is 1: (0-0.05): (0.05-0.25): (0.01-0.5): (10-100) so as to obtain initial sol, then, crystallizing the initial sol for 20-120 hours in a closed system at the temperature of 130-200 DEG C so as to obtain a product, and subjecting the product to washing, drying and roasting according to conventional methods, the technical problem is better solved, and the rare-earth containing MFI zeolite can be applied to water vapor accompanied high-temperature catalytic reaction.

Description

technical field [0001] The invention relates to a synthesis method of MFI type zeolite containing rare earth. Background technique [0002] The MFI zeolite represented by ZSM-5 has a unique pore structure and easy-to-regulate solid acid properties, so it is used in petrochemical processes such as catalytic cracking, alkylation, isomerization, disproportionation, dewaxing and etherification of hydrocarbons. has been widely applied. The earliest MFI-type zeolite (ZSM-5) was invented by the original Mobil company in the early 1970s [USP3702886]. They used expensive tetrapropylammonium hydroxide as a template to synthesize a lower silicon-alumina than the product. After decades of development, the synthesis method of MFI zeolite has been greatly improved [Cracking, 1997, 16, 53], such as the use of cheap alkylamines, cheap alcohols, and even without the use of organic The template agent also synthesized MFI zeolites [USP4151189, USP4175114, EP0042225, GB1553209, CN85100463, C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 袁志庆陶伟川滕加伟
Owner CHINA PETROLEUM & CHEM CORP
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