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A kind of template-free two-step hydrothermal synthesis method of ultrafine type A zeolite

A technology of hydrothermal synthesis and no template agent, applied in the direction of A-type crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, etc., can solve the problems of high price and complicated steps, and achieve the effect of reducing costs

Inactive Publication Date: 2015-11-18
KUNMING UNIV OF SCI & TECH
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  • Summary
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  • Claims
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Problems solved by technology

[0004] In order to overcome the problems of high cost and cumbersome steps in the preparation of ultrafine A-type molecular sieves, the present invention proposes a two-step method for hydrothermally synthesizing ultrafine A-type zeolites without templates, which is a cheap and simple method for synthesizing ultrafine A-type zeolites. Molecular sieve method

Method used

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  • A kind of template-free two-step hydrothermal synthesis method of ultrafine type A zeolite
  • A kind of template-free two-step hydrothermal synthesis method of ultrafine type A zeolite

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Embodiment approach 1

[0021] Embodiment 1: The method for the template-free two-step hydrothermal synthesis of ultrafine type A zeolite in this embodiment is:

[0022] (1) According to the molar ratio of 2Na 2 O: 1.5Al 2 O 3 :1SiO 2 :150H 2 O Preparation of aluminum hydroxide, sodium metaaluminate, sodium silicate and distilled water;

[0023] (2) Dissolve the prepared sodium hydroxide into a sodium hydroxide solution with a concentration of 0.5 mol / L, divide it into two equally, put sodium metaaluminate and sodium silicate into two sodium hydroxide solutions, and then record them separately Is solution I and solution II;

[0024] (3) Pour solution I quickly into solution II to get the initial gel, and then put the initial gel at 35 o Under the condition of C, stir and age at a rate of 350r / min for 20h to obtain a mixed solution;

[0025] (4) The mixed solution obtained after the treatment in step (3) was crystallized for 8 hours under the hydrothermal reaction conditions of 80°C in a hydrothermal reactor,...

Embodiment approach 2

[0026] Embodiment 2: The method for the template-free two-step hydrothermal synthesis of ultrafine type A zeolite in this embodiment is:

[0027] (1) According to the molar ratio of 4Na 2 O: 0.5Al 2 O 3 :2.5SiO 2 :100H 2 O Preparation of aluminum hydroxide, sodium metaaluminate, sodium silicate and distilled water;

[0028] (2) Dissolve the prepared sodium hydroxide into a sodium hydroxide solution with a concentration of 2mol / L, divide it into two equally, and divide the sodium metaaluminate and sodium silicate into two sodium hydroxide solutions, and then record them as Solution I and Solution II;

[0029] (3) Pour solution I quickly into solution II to get the initial gel, and then put the initial gel at 45 o Under the condition of C, stir and age for 140h at a rate of 180r / min to obtain a mixed solution;

[0030] (4) The mixed solution obtained after the treatment in step (3) was crystallized for 3 hours under the hydrothermal reaction conditions of 120°C in a hydrothermal reactor...

Embodiment approach 3

[0031] Embodiment 3: The method for the template-free two-step hydrothermal synthesis of ultrafine type A zeolite in this embodiment is:

[0032] (1) According to the molar ratio of 4Na 2 O: 1Al 2 O 3 :2SiO 2 :120H 2 O Preparation of aluminum hydroxide, sodium metaaluminate, sodium silicate and distilled water;

[0033] (2) Dissolve the prepared sodium hydroxide into a sodium hydroxide solution with a concentration of 1mol / L, divide it into two equally, and divide the sodium metaaluminate and sodium silicate into two sodium hydroxide solutions, and then record them as Solution I and Solution II;

[0034] (3) Pour solution I quickly into solution II to get the initial gel, and then put the initial gel at 40 o Under the condition of C, stir and age at a rate of 300r / min for 110h to obtain a mixed solution;

[0035] (4) The mixed solution obtained after the treatment in step (3) is crystallized for 6 hours under hydrothermal reaction conditions at 100°C in a hydrothermal reactor, ultraso...

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Abstract

The invention discloses a template agent-free two-step method hydro-thermal synthesis method for ultramicro A type zeolite and belongs to the technical field of preparation of ultramicro zeolite molecular sieves. Sodium metaaluminate and sodium silicate are adopted for preparing initial gel in ratio of (2-4) parts of Na2O to (0.5-1.5) parts of Al2O3 to (1-2.5) parts of SiO2:(100-150) parts of H2O, no template agent is added, aging is carried out for 20-140 hours under the conditions that temperature is 35-45 DEG C and speed is 180-300r / min, then the aged gel is placed into a reaction kettle, crystallization is carried out for 4 hours at the temperature of 100 DEG C, and ultrasound, suction filtration, washing and drying are carried out, so that the ultramicro A type zeolite is obtained. Compared with the prior art, the template agent-free two-step method hydro-thermal synthesis method for the ultramicro A type zeolite has the advantages of low preparation cost and simple operation steps.

Description

Technical field [0001] The invention relates to a method for hydrothermally synthesizing ultrafine A-type zeolite by a two-step method without a template, and belongs to the technical field of ultrafine zeolite molecular sieve preparation. Background technique [0002] Zeolite molecular sieve is a kind of porous crystalline material, the pore size is generally 0.3-3nm, and its special microporous structure makes it have many important properties, such as ion exchange, catalytic activity, adsorption, etc. Studies have shown that the zeolite grain size has a great influence on its ion exchange, catalysis and adsorption performance. It is generally believed that a zeolite with a smaller crystallite size has a larger external specific surface area, a shorter diffusion distance, and more exposed active centers. A-type zeolite molecular sieve is often used as a typical example to study the crystallization process of zeolite due to its simple initial gel composition, regular topologica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/14
Inventor 刘艳娜肖松
Owner KUNMING UNIV OF SCI & TECH
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