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Method for synthesizing pure silicon Beta molecular sieves in hydrothermal and fluoride-free manner

A molecular sieve and pure silicon technology, applied in the field of zeolite molecular sieve preparation, can solve the problem of expensive

Active Publication Date: 2019-09-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The object of the present invention is to provide a kind of with tetraethyl ammonium hydroxide as template agent, crystal seed assists, the method for hydrothermal fluorine-free synthesis of pure silicon Beta molecular sieve, overcomes existing synthetic need to use expensive template agent, uses fluoride ion or Disadvantages of Steam Assisted Crystallization

Method used

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  • Method for synthesizing pure silicon Beta molecular sieves in hydrothermal and fluoride-free manner
  • Method for synthesizing pure silicon Beta molecular sieves in hydrothermal and fluoride-free manner
  • Method for synthesizing pure silicon Beta molecular sieves in hydrothermal and fluoride-free manner

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preparation example Construction

[0037] Preparation of seed crystals:

[0038] (1) 3.535 grams of tetraethylammonium hydroxide and 5 milliliters of distilled water are added to the reaction vessel, and stirred at room temperature until the two are evenly mixed;

[0039] (2) Add 4.5 grams of ethyl orthosilicate to the above solution under stirring, and continue stirring until the hydrolysis of ethyl orthosilicate is complete;

[0040] (3) Continue to stir until the moisture evaporates and becomes a dry gel, and the sample is ground into powder;

[0041] (4) Weigh 0.324 grams of ammonium fluoride, add it to the powder of step (3), and continue grinding until the two are evenly mixed; the silicon source is converted into SiO 2 For calculation, the active ingredient and molar ratio are SiO 2 :TEAOH:NH 4 F:H 2 O=100:40:40:100;

[0042] (5) crystallize the mixture obtained in step (4) at 150°C for 7 days;

[0043](6) After being cooled to room temperature, the obtained solid is washed with distilled water and...

Embodiment 1

[0048] (1) 0.421 gram of tetraethylammonium hydroxide solution and 5.4 milliliters of distilled water are added in the reaction vessel, stirred at room temperature until the two are evenly mixed;

[0049] (2) Add 1.929 grams of ethyl orthosilicate (wherein SiO 2 Quality is 0.54 gram), continue to stir until hydrolysis of ethyl orthosilicate is complete;

[0050] (3) Add 0.02 gram of sodium hydroxide to the above solution, and stir under airtight and room temperature conditions to form a uniform mixed solution;

[0051] (4) Add 0.027 gram of Beta molecular sieve seed crystals to the homogeneous mixed solution formed in step (3). Stir the gel at room temperature to the desired water-to-silicon ratio, converting the silicon source to SiO 2 For calculation, the active ingredients and molar ratio of the gel are SiO 2 :TEAOH:NaOH:H 2 O=90:10:5:1000, the input amount of seed crystal is to convert the silicon source used in step (2) into SiO 2 5% of the mass.

[0052] (5) hydrot...

Embodiment 2

[0056] (1) 0.631 gram of tetraethylammonium hydroxide solution and 5.4 milliliters of distilled water are added in the reaction vessel, and stirred at room temperature until the two are evenly mixed;

[0057] (2) Add 2.143 grams of ethyl orthosilicate (wherein SiO 2 Quality is 0.6 gram), continue to stir until hydrolysis of ethyl orthosilicate is complete;

[0058] (3) Add 0.008 gram of sodium hydroxide to above-mentioned solution, stir under airtight, room temperature condition to form uniform mixed solution;

[0059] (4) Add 0.03 gram of Beta molecular sieve seed crystals to the homogeneous mixed solution formed in step (3). Stir the gel at room temperature to the desired water-to-silicon ratio, converting the silicon source to SiO 2 For calculation, the active ingredients and molar ratio of the gel are SiO 2 :TEAOH:NaOH:H 2 O=100:15:2:1500, the input amount of seed crystal is to convert the silicon source used in step (2) into SiO 2 5% of the mass.

[0060] (5) hydrot...

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Abstract

A method for synthesizing pure silicon Beta molecular sieves in a hydrothermal and fluoride-free manner belongs to the technical field of preparation of zeolite molecular sieves. The method is implemented by adding Beta molecular sieve seed crystals into an initial gel to synthesize the pure silicon Beta molecular sieves under hydrothermal and fluoride-free conditions. Specifically, the method comprises taking low-price silicon sources, templates and alkali sources as well as the homemade pure silicon Beta molecular sieve seed crystals as the raw materials, dissolving the silicon sources, the templates, the alkali sources and the seed crystals into distilled water, performing mixing to obtain a uniform gel, and then performing hydrothermal crystallization; washing and drying the hydrothermally crystalized products to obtain the pure silicon Beta molecular sieves. Compared with the prior art, the method for synthesizing the pure silicon Beta molecular sieves in a hydrothermal and fluoride-free manner has the advantages of being low in price of the synthetic raw materials, simple in synthesis and free from application of fluoride ions during synthesizing processes, thereby having a good industrialized application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of zeolite molecular sieves, and specifically relates to a method of adding ball-milled pure silicon Beta seeds to an initial gel system, using tetraethylammonium hydroxide as a template, and not introducing fluoride ions into the reaction system. A method for synthesizing pure silicon Beta molecular sieves by hydrothermal method. Background technique [0002] Volatile organic compounds (VOCs) generally refer to organic compounds with a boiling point between 50-260°C, which mainly come from industrial production processes and exhaust emissions from motor vehicles. As a common air pollutant, VOCs not only have strong biological toxicity and seriously affect human health; but also, as an important precursor of ozone, photochemical smog and PM2.5, are a major international issue in environmental protection. Therefore, how to deal with it has always attracted much attention. [0003] At present,...

Claims

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Application Information

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IPC IPC(8): C01B37/02B82Y40/00
CPCC01B37/02B82Y40/00
Inventor 闫文付米珍睿白璞于吉红徐如人
Owner JILIN UNIV
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