Method for preparing mesoporous TS-1 titanium silicalite molecular sieves through hydrothermal crystallization method

A titanium-silicon molecular sieve and hydrothermal crystallization technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of high production cost of titanium-silicon molecular sieve, low content of framework titanium, complicated preparation method, etc., so as to reduce the concentration of anatase. The effect of generation, high content of skeleton titanium and simple preparation method

Active Publication Date: 2016-11-09
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The problems to be solved by the present invention are the problems of high production cost, cumbersome preparation method, poor repeatability, less skeleton titanium content, and small pore size in the production of titanium-silicon molecular sieves in the prior art.

Method used

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  • Method for preparing mesoporous TS-1 titanium silicalite molecular sieves through hydrothermal crystallization method
  • Method for preparing mesoporous TS-1 titanium silicalite molecular sieves through hydrothermal crystallization method
  • Method for preparing mesoporous TS-1 titanium silicalite molecular sieves through hydrothermal crystallization method

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Experimental program
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Effect test

Embodiment 1

[0032] At 25°C, first mix tetrapropylammonium bromide, tetraethyl orthosilicate, and water to form A; mix the pore expander with water to form B; add emulsifier TX-10 to butyl titanate to form emulsion C; Pass inert gas into the emulsion C and use the shock generated by the bubble burst to demulsify the emulsion to release the titanium source; then mix A and B and drop them into C to form D, and use tetramethyl hydroxide during the dropwise addition Adjust the pH value with ammonium to make the pH value = 12. After the titration is completed, place D in a stainless steel crystallization reaction kettle for crystallization at 170°C for 48 hours, filter and wash the resulting crystallized product, and dry 6 pieces at 120°C. Hours, calcined at 550°C for 6 hours to obtain a large-diameter TS-1 molecular sieve. Among them, tetraethyl orthosilicate: emulsifier (TX-10): butyl titanate: tetrapropylammonium bromide: pore expander (hexamethyleneimine): the molar ratio of water is 1:0.06...

Embodiment 2

[0034] At 25°C, tetrapropylammonium bromide, tetraethyl orthosilicate, and water are first mixed to form A; the pore expander is mixed with water to form B; the emulsifier acetylacetone is added to butyl titanate to form emulsion C; The inert gas is introduced into the emulsion C, and the shock generated by the bursting of the bubbles is used to demulsify the emulsion to release the titanium source; then A and B are mixed and dropped into C to form D, and tetramethyl hydroxide is used during the dropwise addition process. Adjust the pH value with ammonium to make the pH value = 12. After the titration is completed, place D in a stainless steel crystallization reaction kettle for crystallization at 170°C for 60 hours, filter and wash the resulting crystallized product, and dry 5 pieces at 120°C. Hours, calcined at 550°C for 5 hours to obtain a large-diameter TS-1 molecular sieve. Among them, ethyl orthosilicate: emulsifier acetylacetone: butyl titanate: tetrapropylammonium brom...

Embodiment 3

[0036] At 25°C, first mix tetrapropylammonium bromide, propyl orthosilicate, and water to form A; mix the pore expander with water to form B; add emulsifier TX-10 to butyl titanate to form emulsion C; Pass inert gas into the emulsion C and use the shock generated by the bursting of the bubbles to break the emulsion to release the titanium source; then mix A and B and drop them into C to form D, and use tetramethyl hydrogen in the process of dropping Adjust the pH value with ammonium oxide to make the pH value = 12. After the titration is completed, place D in a stainless steel crystallization reactor and crystallize at 170°C for 60 hours. Filter and wash the obtained crystallized product, and dry it at 120°C for 60 hours. hour, and roasted at 550°C for 6 hours to obtain a large-diameter TS-1 molecular sieve. Among them, propyl orthosilicate: emulsifier TX-10: butyl titanate: tetrapropylammonium bromide: pore expander (trimethylbenzene): the molar ratio of water is 1:0.06:0.06:...

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Abstract

The invention relates to a method for preparing mesoporous TS-1 titanium silicalite molecular sieves through a hydrothermal crystallization method. The method includes the following main steps of firstly, mixing a template agent, water and a silicon source at a temperature of 5-50 DEG C to form a solution A; secondly, mixing a pore-enlarging agent and water to form a solution B; thirdly, adding an emulsifying agent to a titanium source to form an emulsion C; fourthly, introducing inert gas into the emulsion C to conduct demulsification on the emulsion and release the titanium source, mixing the solution A and the solution B according to the volume ratio of 1:1, dropwise adding the mixture into the emulsion C to form D, adjusting pH to be 8-13 in the dropwise adding process, and conducting hydrothermal crystallization, washing and dry-roasting on the D after titration is completed to obtain the product. The method reduces production cost, the preparation method is simple, TS-1 aperture is large, framework titanium content is high, and repeatability is good.

Description

technical field [0001] The invention relates to a method for preparing a mesoporous TS-1 titanium-silicon molecular sieve by using a hydrothermal crystallization method. Background technique [0002] Titanium-silicon molecular sieve TS-1 is a new type of heteroatom molecular sieve synthesized for the first time in 1981 by Marco Taramasso et al. in Italy. It is found that TS-1 has the MFI structure like ZSM-5, and is a catalytic material with good catalytic selective oxidation activity, suitable for a series of organic chemical reactions using hydrogen peroxide as the oxidant (such as the epoxidation reaction of olefin , Hydroxylation of aromatic hydrocarbons, oximation of ketones and selective oxidation of alkanes and alcohols, etc.) and the reaction conditions are mild, and the by-product is water, which does not pollute the environment. Titanium silicate molecular sieves have excellent catalytic activity and selectivity when used as catalysts, and are widely used in petro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B39/04
CPCC01B39/04C01B39/08C01P2002/72C01P2004/03C01P2006/12C01P2006/16C01P2006/14
Inventor 王广建李佳佳王芳邴连成
Owner QINGDAO UNIV OF SCI & TECH
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