Method for preparing low-silicon NaX zeolite by applying activated silicon source

A technology for activating silicon and silicon sources, applied in the direction of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., which can solve problems such as increased cost, troublesome operation, and slow exchange rate of potassium ions

Inactive Publication Date: 2012-04-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the slow exchange rate of potassium ions, potassium ions need to be exchanged for sodium ions

Method used

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  • Method for preparing low-silicon NaX zeolite by applying activated silicon source
  • Method for preparing low-silicon NaX zeolite by applying activated silicon source
  • Method for preparing low-silicon NaX zeolite by applying activated silicon source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The main raw material used: water glass (wherein the active ingredient content is SiO 2 26.79wt%, Na 2 O10.62wt%), sodium aluminate ((wherein the content of active ingredient is Al 2 o 3 43.3 wt%, Na 2 O 40.35wt%), sodium hydroxide (analytically pure, purity 98wt%)

[0017] First prepare the activated silicon source, weigh 1.61 grams of sodium aluminate, add 21.29 grams of deionized water, stir to dissolve, then add 4.55 grams of sodium hydroxide, continue to stir and dissolve. Then this alkaline sodium aluminate solution is slowly added in 26.89 grams of water glass, stirs while adding dropwise, stirs again 30 minutes after finishing adding. It was used after standing and aging at room temperature (25°C) for 1 day. The activated silicon originates from being stored at room temperature for 1 to 7 days and is in a liquid state and is effective. If left for too long, gel will be formed, and the activity will decrease when the gel is formed. If the aging temperature...

Embodiment 2

[0021] The raw materials used are the same as in Example 1, and the preparation and molar composition of the activated silicon source are the same as in Example 1.

[0022] When synthesizing low-silicon NaX zeolite, weigh 2.09 grams of sodium aluminate, add 45.96 grams of water, stir and dissolve, add 0.46 grams of sodium hydroxide, continue to stir and dissolve, and slowly add the prepared alkaline sodium aluminate solution to 10.86 In the above-mentioned activated silicon source, stir while adding, and stir for 30 minutes after adding. Then the reaction mixture was placed in a reaction kettle, statically crystallized at 60°C for 24h, then filtered, washed with deionized water to be close to neutral, and dried at 100°C. The molar ratio of each component in the reaction mixture is Na 2 O:Al 2 o 3 : SiO 2 :H 2 O=4.2:1:2.4:300.

[0023] The product was analyzed as zeolite X using X-ray powder diffraction, solid using magic angle rotation 29 Si-NMR analysis of SiO in the p...

Embodiment 3

[0025] The raw materials used are the same as in Example 1, and the preparation and molar composition of the activated silicon source are the same as in Example 1. The molar ratio and preparation method of the synthetic low-silicon NaX reaction mixture are the same as in Example 2, but the crystallization temperature is different, specifically crystallization at 60°C for 7h, and then crystallization at 95°C for 5h. The molar ratio of each component in the reaction mixture is Na 2 O:Al 2 o 3 : SiO 2 :H 2 O=4.2:1:2.4:300.

[0026] The product was analyzed as zeolite X using X-ray powder diffraction, solid using magic angle rotation 29 Si-NMR analysis of SiO in the product 2 / Al 2 o 3 The molar ratio is 2.08, and the average particle size is 210nm by scanning electron microscope analysis.

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Abstract

The invention belongs to the technical field of zeolite molecular sieve synthesis and particularly relates to a method for preparing low-silicon NaX zeolite by applying an activated silicon source. The product nano (100nm-500nm) NaX zeolite, the SiO2/Al2O3 ratio of which is less than 2.1, is synthesized in a sodium-containing silicoaluminate system by using the method provided by the invention. The method comprises the following steps: firstly, preparing the activated silicon source, wherein the activated silicon source is obtained by adding a certain amount of alkaline aluminum source solution to a common silicon source so that the high-polymerized silicate is depolymerized to form low-polymerized silicate, and the low-polymerized silicate is combined with aluminate to generate an effective silicoaluminate precursor and a faujasite micro-crystal nucleus; and synthesizing the low-silicon NaX zeolite through controlling the crystallization conditions and crystallization temperature of the molecular sieve preparation process.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, and in particular relates to a method for preparing low-silicon NaX zeolite by using an activated silicon source. Background technique [0002] Both NaX and NaY zeolites have a natural faujasite structure, but they differ in their silica-to-alumina ratios. The silicon-aluminum ratio of NaX zeolite (SiO 2 / Al 2 o 3 ) theoretically ranges from 2 to 3. However, the silicon-aluminum ratio of NaX zeolite synthesized by conventional methods is greater than 2.3 (Milton R.M. US Pat. 2,882,244). The low-silicon NaX zeolite mentioned in the present invention refers to a NaX zeolite with a silicon-aluminum ratio lower than 2.3, especially close to 2.0. This NaX zeolite has a high aluminum content and has special properties. It has important application value in functional materials, catalytic reaction, adsorption separation and ion exchange. At present, it has been used in i...

Claims

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Application Information

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IPC IPC(8): C01B39/22
Inventor 王润伟李守贵曾尚景
Owner JILIN UNIV
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