A synthetic method of an SSZ-13 molecular sieve

A molecular sieve and seed crystal technology, which is applied in the direction of crystalline aluminosilicate zeolite, etc., achieves the effects of easy preparation, reduced usage, and easy popularization and application.

Active Publication Date: 2016-06-08
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can reduce the use of N,N,N-trimethyl-1-adamantanamine (TMAA+) cations an

Method used

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  • A synthetic method of an SSZ-13 molecular sieve
  • A synthetic method of an SSZ-13 molecular sieve
  • A synthetic method of an SSZ-13 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Synthesis of template N,N,N-trimethyl-1,3,5,7-tetraazatricyclo[3.3.1.1]decane-2-ammonium hydroxide.

[0039] This example introduces a synthesis of N,N,N-trimethyl-1,3,5, A method for 7-tetraazatricyclo[3.3.1.1]decane-2-ammonium hydroxide, which comprises four steps of ①nitration, ②hydrogenation, ③quaternization and ④electrolysis.

[0040] ①In a cold bath at -15°C, put 663.2 grams of 95% nitric acid in a 2-liter three-necked flask, and slowly add 140.2 grams of urotropine under stirring conditions, and react for 90 minutes after the addition. The cold bath was removed, and 900 g of water was added, stirred for 30 minutes, and white crystals were precipitated. Filter and wash with water until neutral, then place the filter cake in a vacuum oven at 50°C and dry for 5-6 hours to obtain about 138.9 grams of white powdery solid A, namely 2-nitro-1,3,5 , 7-tetraazatricyclo[3.3.1.1]decane, yield 75.1%.

[0041] ② Dissolve 120 grams of solid A in 300 milliliters of ethanol, ...

Embodiment 2

[0046] First, 4.210 grams of sodium hydroxide was dissolved in 21 grams of deionized water, and then 0.656 grams of sodium metaaluminate (aluminum source) was added to the above sodium hydroxide solution, and stirred vigorously to dissolve it. Next, add 7.230 grams of N,N,N-trimethyl-1,3,5,7-tetraazatricyclo[3.3.1.1]decane-2-hydrogen obtained in Example 1 to the above solution The ammonium oxide solution was used as the template agent R, which was dissolved by strong stirring, and 42.062 grams of 40%wt silica sol (silicon source) was slowly added under strong stirring conditions.

[0047] The molar ratio of each material of the synthetic mixture consists of:

[0048]

[0049] Stir the above mixture at room temperature for one hour, then divide it into two parts (Part A and Part B), and transfer Part A and Part B to a stainless steel autoclave with a Teflon liner, and place it at 150°C Oven and keep for 4 days (for Part A) and 6 days (for Part B).

[0050] The product was ...

Embodiment 3

[0053] First, 2.880 g of sodium hydroxide was dissolved in 21 g of deionized water, and then 0.656 g of sodium metaaluminate (aluminum source) was added to the above sodium hydroxide solution, and stirred vigorously to dissolve it. Next, add 3.443 grams of N,N,N-trimethyl-1,3,5,7-tetraazatricyclo[3.3.1.1]decane-2-hydrogen obtained in Example 1 to the above solution The ammonium oxide solution was used as the template agent R, which was dissolved by vigorous stirring, and 24.033 grams of 40%wt silica sol (silicon source) was slowly added under the condition of strong stirring.

[0054] The molar ratio of each material of the synthetic mixture consists of:

[0055]

[0056] The above mixture was stirred at room temperature for one hour, and then it was divided into two parts (Part A and Part B), and Part A and Part B were respectively transferred to a stainless steel autoclave with a Teflon liner, and placed in 140°C oven and 160°C oven for 6 days.

[0057] The product was ...

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Abstract

A synthetic method of an SSZ-13 zeolite molecular sieve is disclosed. The method includes preparing SSZ-13 crystals under crystallization conditions from raw materials comprising an oxide of at least one quadrivalent element or a quadrivalent element mixture, an oxide of at least one trivalent element and a trivalent element mixture, at least one alkali metal compound, N,N,N-trimethyl-1,3,5,7-tetraazatricyclo[3.3.1.1]decane-2-ammonium hydroxide or a mixture of the N,N,N-trimethyl-1,3,5,7-tetraazatricyclo[3.3.1.1]decane-2-ammonium hydroxide and the SSZ-13 molecular sieve crystal seeds, hydroxyl ions and water. The method is a method of synthesizing the SSZ-13 molecular sieve by adopting a novel and cheap template. The method avoids adoption of traditional expensive N,N,N-trimethyladamantan-1-ammonium cations or benzyl trimethyl quaternary ammonium cations as templates to synthesize the SSZ-13 molecular sieve, thus significantly reducing the cost of synthesizing the SSZ-13 zeolite molecular sieve.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis and relates to a method for synthesizing SSZ-13 molecular sieves by using a cheap template agent. Background technique [0002] Molecular sieve refers to a class of substances with uniform micropores whose pore size is equivalent to that of ordinary molecules. Molecular sieves are widely used and can be used as high-efficiency desiccants, selective adsorbents, catalysts, ion exchangers, etc. Commonly used molecular sieves are crystalline silicates or aluminosilicates, which are connected by silicon-oxygen tetrahedrons or aluminum-oxygen tetrahedrons through oxygen bridges to form a molecular-sized pore and cavity system. [0003] The International Molecular Sieve Association (IZA) defines different types of zeolite molecular sieves as different structural codes, such as MFI, BEA, CHA, etc. SSZ-13 molecular sieve is a molecular sieve with CHA topology, and its structure is composed of AlO...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 李进李永宾王建青张旭旺
Owner CHINA CATALYST HLDG CO LTD
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