A kind of preparation method of nanoscale titanium silicon molecular sieve

A titanium-silicon molecular sieve, nano-scale technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of reduced specific surface area, reduced catalytic performance of molecular sieves, etc., to achieve good catalytic performance and save energy Production procedure and cost control, effect of large specific surface area

Active Publication Date: 2016-12-07
CHINA TIANCHEN ENG +1
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  • Summary
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under the existing preparation methods, the particle size of titanium-silicon molecular sieves is generally around 200nm to 300nm, and there are also a few micron-sized molecular sieve preparation methods, but the micron-sized molecular sieves are too large in size, resulting in a decrease in specific surface area, which reduces the catalytic performance of molecular sieves.

Method used

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  • A kind of preparation method of nanoscale titanium silicon molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) After mixing the silicon source and the titanium source, add them to the aqueous solution of tetrapropylammonium hydroxide and stir them fully, and hydrolyze them for 0.5h at 0°C to obtain the hydrolyzed solution of the silicon source and the titanium source, the molar composition of which is Si:Ti: Tetrapropylammonium hydroxide: water=1: 0.01: 0.03: 1;

[0022] (2) Remove alcohol from the obtained hydrolysis solution at 50° C. for 3 hours, continuously add water to it during the alcohol removal process to prevent gelation, and the quality of the solution after adding water does not exceed the quality before alcohol removal;

[0023] (3) After removing the alcohol, the mother liquor is put into a closed reactor for pre-crystallization at 100°C for 0.5h, and then a certain amount of tetramethylguanidine is added, wherein the molar ratio Si:tetramethylguanidine=1:0.05;

[0024] (4) Continue to put the above mixed solution into a closed reactor for hydrothermal crystal...

Embodiment 2

[0026] (1) After mixing the silicon source and the titanium source, add them to the aqueous solution of tetraethylammonium hydroxide and stir fully, hydrolyze for 5 hours at 50° C. to obtain the hydrolysis solution of the silicon source and the titanium source, and its molar composition is Si: Ti: tetra Ethyl ammonium hydroxide: water = 1: 0.05: 0.6: 100;

[0027] (2) Dealcoholize the obtained hydrolyzed solution at 60° C. for 2 h, continuously add water to it during the process of dealcoholization to prevent gelation, and the quality of the solution after adding water does not exceed the quality before dealcoholization;

[0028] (3) After removing the alcohol, the mother liquor is put into a closed reactor for pre-crystallization at 150° C. for 10 h, and then a certain amount of tetramethylurea is added, wherein the molar ratio Si: tetramethylurea = 1: 0.6;

[0029] (4) Continue to put the above mixed solution into a closed reaction kettle for hydrothermal crystallization at ...

Embodiment 3

[0031] (1) After mixing the silicon source and the titanium source, add them to the aqueous solution of tetramethylammonium hydroxide and stir fully, and hydrolyze for 1 hour at 50° C. to obtain the hydrolyzed solution of the silicon source and the titanium source, and its molar composition is Si: Ti: tetramethylammonium hydroxide Methyl ammonium hydroxide water = 1: 0.03: 0.2: 20;

[0032] (2) dealcoholize the obtained hydrolyzed solution at 85° C. for 0.5 h, continuously add water to it during the process of dealcoholization to prevent gelation, and the quality of the solution after adding water does not exceed the quality before dealcoholization;

[0033] (3) After alcohol removal, the mother liquor was put into a closed reactor for pre-crystallization at 120° C. for 4 hours, and then a certain amount of tetramethylguanidine was added, wherein the molar ratio Si:tetramethylguanidine=1:0.2.

[0034] (4) Continue to put the above mixed solution into a closed reactor for hydro...

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Abstract

The invention provides a preparation method of a nanoscale titanium silicalite molecular sieve. The preparation method comprises adding a proper amount of organic alkali to the molecular sieve after pre-crystallization and then continuously performing a hydrothermal crystallization process to obtain the molecular sieve product. The preparation method is capable of obtaining the molecular sieve product smaller in particle size, larger in specific surface area and more excellent in catalytic performance.

Description

technical field [0001] The invention belongs to the technical field of petrochemical catalysis, and in particular relates to a preparation method of a TS-1 titanium-silicon molecular sieve with an MFI structure. Background technique [0002] Titanium-silicon molecular sieve TS-1 is a Pentasil-type heteroatom molecular sieve containing skeleton titanium atoms. In addition to maintaining the topological structure of the original MFI molecular sieve, TS-1 has a special skeleton Si-O-Ti bond due to the uniform distribution of titanium atoms in the skeleton, which makes it have both catalytic oxidation activity and shape-selective catalytic performance. [0003] In 1981, Macro Taramasso and others disclosed the synthesis method of TS-1 for the first time, which is called the classic hydrothermal synthesis method. After 40 years of continuous development and research, the hydrothermal synthesis of TS-1 has formed two systems. One is to use tetrapropylammonium hydroxide (TPAOH) a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B82Y30/00
Inventor 袁海朋耿玉侠刘文
Owner CHINA TIANCHEN ENG
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