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Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method

A zeolite molecular sieve, a technology for synthesizing zeolite, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problem of long gel ageing time, unfavorable industrial production, and long synthesis period, etc. problems, to achieve excellent adsorption and exchange performance, avoid high pressure hazards, and simplify the operation.

Inactive Publication Date: 2014-08-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the synthesis process of nano-zeolite molecular sieves, organic templates need to be added during the traditional solvothermal synthesis of nano-zeolites. For example, nano-type A and X-type zeolite molecular sieves are usually synthesized under the condition of adding alkylamines, but the cost of organic templates is high. Moreover, environmental pollution will be generated during roasting, which is not conducive to industrial production; when nano-zeolite molecular sieves are synthesized without using organic templates, longer gel aging time is often used to induce more crystal nuclei, which ultimately makes the synthesis cycle longer.

Method used

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  • Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method
  • Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method
  • Method for quickly synthesizing zeolite molecular sieve by microwave solid-phase method

Examples

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Effect test

Embodiment 1

[0033] Example 1: Rapid synthesis of FAU zeolite molecular sieves by microwave solid-phase method

[0034] 3.7g sodium silicate nonahydrate, 0.34g pseudo-boehmite, 0.28g ammonium chloride solid were mixed, and after grinding for 5 minutes with a mortar, put into a bottle stopper with a hole (for safety considerations, the system kept constant Press, use a bottle stopper with a hole), microwave in a household microwave oven for 50 minutes, filter after cooling, wash with water until nearly neutral, and dry at 60°C to obtain a nano FAU zeolite molecular sieve product.

[0035] The molar ratio of the reaction mixture is Na 2 O: SiO 2 :Al 2 o 3 :H 2 O: NH 4 + =2.55:4.2:1:37.7:1.65.

[0036] attached figure 1 , 2 are XRD and SEM figure of embodiment 1 sample respectively. The product was analyzed by X-ray powder diffraction to be FAU type zeolite molecular sieve. The crystal grain size is about 300-600nm analyzed by scanning electron microscope.

Embodiment 2

[0037] Example 2: Rapid synthesis of FAU zeolite molecular sieves by microwave solid-phase method

[0038]Mix 3.23g sodium silicate nonahydrate, 0.34g pseudo-boehmite, and 0.2g ammonium chloride solid raw materials, grind them with a mortar for 5 minutes, put them into a reaction bottle with a stopper with a hole, and put them in a household microwave oven. Medium microwave for 50 minutes, filter after cooling, wash with water until nearly neutral, and dry at 60°C to obtain nano FAU type zeolite molecular sieve products.

[0039] The molar ratio of the reaction mixture is Na 2 O: SiO 2 :Al 2 o 3 :H 2 O: NH 4 + =2.5:3.7:1:33.5:1.2.

[0040] attached image 3 , 4 are XRD and SEM figure of embodiment 2 samples respectively. The product was analyzed by X-ray powder diffraction to be FAU zeolite molecular sieve. The crystal grain size is about 300-600nm analyzed by scanning electron microscope.

Embodiment 3

[0041] Example 3: Rapid synthesis of FAU zeolite molecular sieves by microwave solid-phase method

[0042] Mix 3.25g of sodium silicate nonahydrate, 0.34g of pseudo-boehmite, 0.1g of ammonium acetate and 0.2g of potassium chloride as solid raw materials, grind them with a mortar for 10 minutes, and put them into a reaction bottle with a hole in the stopper Microwave in a household microwave oven for 50 minutes, filter after cooling, wash with water until nearly neutral, and dry at 60°C to obtain a nanometer FAU zeolite molecular sieve product.

[0043] The molar ratio of the reaction mixture is Na 2 O: SiO 2 :Al 2 o 3 :H 2 O: NH 4 + :K + =3.3:3.7:1:33.5:0.42:0.86. The product was analyzed by X-ray powder diffraction to be FAU zeolite molecular sieve.

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Abstract

The invention provides a method for quickly synthesizing a zeolite molecular sieve by the microwave solid-phase method, and belongs to the technical field of synthesis of the zeolite molecular sieves. The method comprises the following steps: mixing and grinding a solid silicon source, an aluminum source, an alkali source, a non-essential ammonium salt and / or sylvite for 2 to 15min; feeding the ground powder into a reaction flask; heating for 2 to 60 minutes through a microwave oven to quickly crystallize the reaction mixture to synthesize the zeolite molecular sieve; and processing the zeolite molecular sieve by washing, filtering and drying to obtain the finished zeolite molecular sieve, wherein the molar ratio range of the reaction mixture fed is shown as that Na2O: SiO2: Al2O3: H2O: NH<4+> / K<+> =(0.2-8.5): (1-10.5): 1: (7-95): (0-5). With the adoption of the method, the unification of green and economy is realized, the production cost is decreased, the yield of single kettle is increased, and the production cycle is greatly reduced; and the most important is that the method is applicable to quick and high-yield synthesis of A type, X type and AX type detergent builder zeolite molecular sieves.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve synthesis, and in particular relates to a method for rapidly synthesizing zeolite molecular sieves by combining a microwave method and a solid-phase method. Background technique [0002] Zeolite molecular sieves are widely used in adsorption separation, catalysis, ion exchange and other fields due to their regular pore structure, large specific surface area and pore volume. Since the 1960s, artificially synthesized zeolite molecular sieves (such as A-type, X-type, Y-type and L-type zeolite molecular sieves) have been widely used as adsorbents and catalysts. Especially A-type, X-type and AX-type zeolite molecular sieves, because these low-silica zeolite molecular sieves have a low silicon-alumina ratio (SiO 2 / Al 2 o 3 ≤1.5) and larger pore volume, more cations in the balanced skeleton charge, so it has a higher ion exchange capacity, so it is used in detergent additives, and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/14C01B39/20C01B39/46
Inventor 王润伟曾尚景付静茹
Owner JILIN UNIV
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