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Method for synthesizing Silicalite-1 molecular sieve with TPABr being template agent

A technology of molecular sieves and templates, applied in the direction of silica, silicon oxide, etc., can solve the problems of expensive templates, large-scale use of templates, etc.

Active Publication Date: 2018-05-08
LUOYANG JALON MICRO NANO NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a kind of tetrapropylammonium bromide as template agent on the basis of prior art, and the method for preparing Silicalite-1 molecular sieve with auxiliary crystal seed, overcomes that existing synthesis needs to use expensive template agent and a large amount of templates Disadvantages of the agent

Method used

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  • Method for synthesizing Silicalite-1 molecular sieve with TPABr being template agent
  • Method for synthesizing Silicalite-1 molecular sieve with TPABr being template agent
  • Method for synthesizing Silicalite-1 molecular sieve with TPABr being template agent

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preparation example Construction

[0035] Preparation of seed crystals:

[0036] (1) 0.416 grams of tetrapropylammonium hydroxide and 5 milliliters of distilled water are added to the reaction vessel, and stirred at room temperature until the two are mixed evenly;

[0037] (2) 3 grams of silica sol (where SiO 2 Quality is 1.2 grams), continue to stir until the two are evenly mixed;

[0038] (3) hydrothermally crystallizing the mixture obtained in step (2) at 150°C for 2 days;

[0039] (4) After cooling to room temperature, the crystallized product is subjected to solid-liquid separation, and the obtained solid is washed with distilled water and dried;

[0040] (5) The dried product is calcined in a muffle furnace at 550° C. for 6 hours, and the product is ball milled for 6 hours after calcination;

[0041] (6) The solid after the ball milling was stirred in an aqueous sodium hydroxide solution of 0.15mol / L for 1 hour, centrifuged, washed with distilled water, and dried at 60° C. for 10 hours to obtain the MFI ...

Embodiment 1

[0044] (1) 0.106 gram of tetrapropylammonium bromide and 3.4 milliliters of distilled water are added in the reaction vessel, stirred at room temperature until the two are evenly mixed;

[0045] (2) 3 grams of silica sol (where SiO 2 Quality is 1.2 grams), continue to stir until the solution is mixed evenly;

[0046] (3) Add 0.12 grams of Silicalite-1 molecular sieve seed crystals to the above solution, and stir under airtight and room temperature conditions to form a uniform mixed solution;

[0047] (4) drop into the solution that 0.024 gram of sodium hydroxide and 2 milliliters of distilled waters form in the homogeneous mixed liquor that step (3) forms, and speed is controlled at 1 drop per second. Stir under airtight conditions at room temperature to form a uniform gel, and convert the silicon source into SiO 2 For calculation, the active ingredient composition and molar ratio of the gel are SiO 2 :TPABr:NaOH:H 2 O=100:2:3:1500, the input amount of seed crystal is to c...

Embodiment 2

[0052] (1) 0.106 gram of tetrapropylammonium bromide and 4 milliliters of distilled water are added in the reaction vessel, stirred at room temperature until the two are evenly mixed;

[0053] (2) 3 grams of silica sol (where SiO 2 Quality is 1.2 grams), continue to stir until the solution is mixed evenly;

[0054] (3) Add 0.12 grams of Silicalite-1 molecular sieve seed crystals to the above solution, and stir under airtight and room temperature conditions to form a uniform mixed solution;

[0055] (4) drop into the solution that 0.016 gram of sodium hydroxide and 2.5 milliliters of distilled waters form in the homogeneous mixed liquor that step (3) forms, and speed is controlled at 1 drop per second. Stir under airtight conditions at room temperature to form a uniform gel, and convert the silicon source into SiO 2 For calculation, the active ingredient composition and molar ratio of the gel are SiO 2 :TPABr:NaOH:H 2 O=100:2:2:1800, the input amount of the seed crystal is ...

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Abstract

The invention provides a method for synthesizing a Silicalite-1 molecular sieve with TPABr being template agent, and belongs to the technical field of zeolite molecular sieve preparation. According tothe method, a Silicalite-1 molecular seed crystal is added in initial gel, and the Silicalite-1 molecular sieve is synthesized in a short crystalizing time (1-2 days). By means of the method, with acheap silicon source, template agent, alkali source and the self-made Silicalite-1 molecular seed crystal being raw materials, firstly, the silicon source, the alkali source, a small amount of template agent and the seed crystal are dissolved in distilled water and are stirred to form the uniform gel, and then the gel is subjected to hydrothermal crystallization; the product after being subjectedto hydrothermal crystallization is subjected to solid-liquid separation, washing and drying, so that the Silicalite-1 molecular sieve is obtained. Compared with the prior art, the method has the advantages that the synthesizing raw materials are cheap, the organic template agent is small in dose and the degree of crystallinity is high, and has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of zeolite molecular sieve preparation, and specifically relates to adding MFI zeolite molecular sieve seed crystals obtained through special treatment in the initial gel system, using cheap template agent TPABr, and hydrothermally synthesizing Silicalite- 1 Molecular sieve method. Background technique [0002] Molecular sieves are a class of inorganic microporous materials with regular and uniform pore structures, and are widely used in the fields of adsorption, catalysis, and ion exchange. The secondary structural units of MFI zeolite molecular sieves are formed by connecting the shared edges of eight five-membered rings; these structural units are connected into chains through coplanarity, and such chains are connected to form the final three-dimensional MFI by sharing oxygen atoms with each other. structure. MFI type zeolite molecular sieve has two sets of pore structures, one set is a straight 10-memb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2002/72C01P2004/03
Inventor 闫文付米珍睿鲁婷婷白璞于吉红徐如人
Owner LUOYANG JALON MICRO NANO NEW MATERIALS CO LTD
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