Preparation method of hierarchical pore nano TS-1 molecular sieve

A TS-1, multi-level pore technology, applied in the direction of nanotechnology, crystalline aluminosilicate zeolite, etc., can solve the problems of high production cost of TS-1 molecular sieve, green micropore channel limitation, etc., to reduce synthesis cost, The effect of high crystallinity and high hydrothermal stability

Pending Publication Date: 2022-05-10
FUZHOU UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of high production cost of TS-1 molecular sieve, greening and limitation of micropore channel, the present invention provides a preparation method of multi-level porous nano TS-1 molecular sieve

Method used

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  • Preparation method of hierarchical pore nano TS-1 molecular sieve
  • Preparation method of hierarchical pore nano TS-1 molecular sieve
  • Preparation method of hierarchical pore nano TS-1 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0043] (1) Activation of diatomite: 20.00 g of natural diatomite raw soil was weighed and calcined at 800° C. for 4 hours to obtain activated diatomite.

[0044] (2) Impurity removal of diatomite: add activated diatomite to 1mol / L sulfuric acid solution at a mass ratio of 1:5 and mix, stir at 80°C (stirring speed is 600rpm) for 6h and then filter, and the obtained filter cake is washed to neutral , Modified diatomite can be obtained after drying at 100°C.

[0045] (3) Preparation of molecular sieve: Mix 0.84g of modified diatomite with 40.0g of deionized water, then add 0.52g of NaOH and 6.5g of TPAOH and stir for 30min to obtain A solution, slowly add 0.49g of TBOT into 2.64g of IPA and stir evenly Solution B was obtained; then solution B was slowly added dropwise to solution A to obtain an initial gel, stirred in a water bath at 70°C for 2 hours, then transferred to a reaction kettle lined with polytetrafluoroethylene, and crystallized at 170°C for 72 hours. After the cryst...

Embodiment 2

[0048] (1) Activation of diatomite: 20.00 g of natural diatomite raw soil was weighed and calcined at 600° C. for 6 hours to obtain activated diatomite.

[0049] (2) Impurity removal of diatomite: add activated diatomite to 0.1mol / L sulfuric acid solution at a mass ratio of 1:2 and mix, stir at 40°C (stirring speed is 300rpm) for 8 hours and then filter, and the obtained filter cake is washed to neutral The modified diatomite can be obtained after drying at 100°C.

[0050] (3) Preparation of molecular sieve: Mix 0.84g of modified diatomite with 40.0g of deionized water, then add 0.52g of NaOH and 6.5g of TPAOH and stir for 30min to obtain A solution, slowly add 0.49g of TBOT into 2.64g of IPA and stir evenly Obtain solution B; then slowly add solution B dropwise to solution A to obtain an initial gel, stir in a water bath at 70°C for 2 hours, then transfer to a reaction kettle lined with polytetrafluoroethylene, and crystallize at 140°C for 96 hours. After the crystallization...

Embodiment 3

[0053] (1) Activation of diatomite: 20.00 g of natural diatomite raw soil was weighed and calcined at 1000° C. for 2 hours to obtain activated diatomite.

[0054] (2) Impurity removal of diatomite: add activated diatomite to 2mol / L sulfuric acid solution at a mass ratio of 1:10, mix, stir at 95°C (stirring speed is 900rpm) for 1h, and then filter, and the obtained filter cake is washed to neutral , Modified diatomite can be obtained after drying at 100°C.

[0055] (3) Preparation of molecular sieve: Mix 0.84g of modified diatomite with 40.0g of deionized water, then add 0.52g of NaOH and 6.5g of TPAOH and stir for 30min to obtain A solution, slowly add 0.49g of TBOT into 2.64g of IPA and stir evenly Solution B was obtained; then solution B was slowly added dropwise to solution A to obtain an initial gel, stirred in a water bath at 70°C for 2 hours, then transferred to a reactor lined with polytetrafluoroethylene, and crystallized at 200°C for 48 hours. After the crystallizati...

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Abstract

The invention belongs to the field of synthesis of molecular sieves, and relates to a preparation method of a hierarchical pore nano TS-1 molecular sieve. The method comprises the following steps: carrying out roasting and acid treatment on natural diatomite to obtain modified diatomite, uniformly mixing the modified diatomite with alkali liquor, a microporous template agent and a titanium source, and crystallizing the obtained mixture to obtain the hierarchical pore nano TS-1 molecular sieve. The diatomite subjected to roasting and acid treatment is used as a silicon source, green synthesis of the hierarchical-pore nano TS-1 molecular sieve is realized by controlling the composition of initial gel in a synthesis system, and the TS-1 molecular sieve synthesized by the method has the advantages of high crystallinity, large external specific surface area, a micro-mesoporous composite pore structure and the like, and can be used for preparing the hierarchical-pore nano TS-1 molecular sieve. And a mesoporous pore-forming agent does not need to be added in synthesis, and the synthesis process is simple, convenient, efficient, green, environment-friendly and low in cost.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, and in particular relates to a preparation method of a multi-level porous nanometer TS-1 molecular sieve. Background technique [0002] TS-1 molecular sieve is a titanium-containing heteroatom molecular sieve synthesized by Taramasso hydrothermally in 1983. It belongs to the orthorhombic microporous molecular sieve and has an MFI topology. TS-1 molecular sieve is composed of primary structural units such as silicon-oxygen tetrahedron and titanyl-oxygen tetrahedron connected by oxygen bridges to form a secondary structural unit of a five-membered ring. The four-coordinated framework titanium is the active center for selective oxidation, and the Si-O-Ti bonds formed by uniformly distributed titanium in the framework have shape-selective catalytic properties. Because the skeleton does not contain Al ions, it has hydrophobicity, which makes it difficult for water molecules to approach the ac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B82Y40/00
CPCC01B39/08B82Y40/00C01P2006/16C01P2004/64C01P2004/62C01P2002/72C01P2004/03C01P2006/14C01P2006/12
Inventor 岳源源邓青桃董鹏鲍晓军王婵王廷海王鹏照朱海波
Owner FUZHOU UNIV
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