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Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding

A solid-phase grinding and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, can solve the problems of complex template synthesis steps, low product yield, high price, etc., to improve the utilization rate of a single kettle and reduce waste discharge. , the effect of reducing production costs

Active Publication Date: 2015-06-17
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the preparation process causes a large amount of solvent waste, and the template synthesis steps are complicated and expensive
On the other hand, the solvent will cause high pressure in the kettle during heating, and the product yield is low

Method used

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  • Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding
  • Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding
  • Method for synthesizing SSZ-13 molecular sieve through solid-phase grinding

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation of embodiment 1 templating agent

[0021] According to the molar ratio of bromoethane and N,N-dimethylcyclohexylamine as 2.6:1, weigh 11.8g of bromoethane and 5g of N,N-dimethylcyclohexylamine and dissolve them in 10ml of ethanol, set the temperature as Reflux at 80°C and stir for 12 hours. After the reaction, add diethyl ether to the reaction product to produce a white solid precipitate, filter and dry to obtain the desired template.

Embodiment 2

[0022] The preparation of embodiment 2 templating agent

[0023] According to the molar ratio of bromoethane and N,N-dimethylcyclohexylamine as 0.5:1, weigh 2.15g of bromoethane and 5g of N,N-dimethylcyclohexylamine and dissolve them in 20ml of ethanol, set the temperature as Reflux at 80°C and stir for 18 hours. After the reaction, add diethyl ether to the reaction product to produce a white solid precipitate, filter and dry to obtain the desired template.

Embodiment 3

[0024] The preparation of embodiment 3 templating agent

[0025] According to the molar ratio of bromoethane and N,N-dimethylcyclohexylamine as 5:1, weigh 21.5g of bromoethane and 5g of N,N-dimethylcyclohexylamine and dissolve them in 20ml of ethanol, set the temperature at 80 Reflux at ℃ and stir for 24 hours. After the reaction, add diethyl ether to the reaction product to produce a white solid precipitate, filter and dry to obtain the desired template.

[0026] In Examples 1 to 3, ethyl bromide is replaced by ethyl iodide in an equimolar amount, and N, N-dimethylcyclohexylamine is subjected to the same operation reaction to obtain N, N-Dimethyl-N'-ethylcyclohexyl ammonium iodide.

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Abstract

The invention relates to the field of molecular sieve preparation, and aims to provide a method for synthesizing an SSZ-13 molecular sieve through solid-phase grinding. The method for synthesizing the SSZ-13 molecular sieve through solid-phase grinding comprises the following steps: weighing a silicon source, an aluminum source, an alkali source and a template agent for crystallization reaction so as to obtain a crystallization reaction product after the reaction is completed, cooling and washing till being neutral, drying to obtain crude molecular sieve powder, and roasting the crude molecular sieve powder for 5 hours in air of 550 DEG C, thereby obtaining a final product SSZ-13 molecular sieve. The SSZ-13 molecular sieve with relatively good crystallinity degree is synthesized through solid-phase raw material grinding under a solvent-free condition, so that the use of solvent water is reduced to the maximum extent, the synthesis route only involves mixing synthesis steps of primary raw materials, the method is greatly simplified when being compared with a conventional method, the yield and the utilization rate of a single kettle are both relatively increased, the production cost is greatly lowered, the pollution to the environment is greatly reduced, and great industrial application prospect can be achieved.

Description

technical field [0001] The invention relates to the field of molecular sieve preparation, in particular to a method for synthesizing SSZ-13 molecular sieves through solid phase grinding. Background technique [0002] Molecular sieves are characterized by their regular and orderly structure, adjustable skeleton composition, very high surface area and adsorption capacity, cation exchangeability, good shape selectivity of pores, high thermal stability and chemical stability, etc. Has been widely used in the field of catalytic industry. A new molecular sieve SSZ-13 was synthesized by the American chemist Zones S I through a hydrothermal method. SSZ-13 has good thermal stability and can be used as a carrier for adsorbents or catalysts, such as air purifiers, automobile exhaust catalysts, etc. At the same time, SSZ-13 also has cation exchange and acidity adjustable, so it has good catalytic performance for a variety of reaction processes, including methanol to light olefins (MTO...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 孟祥举吴勤明王雄肖丰收
Owner ZHEJIANG UNIV
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