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Synthetic method of TS-1 titanium silicate molecular sieve

A technology of titanium-silicon molecular sieve and synthesis method, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., and can solve the problem of high synthesis cost of TS-1 molecular sieve, large grain size of TS-1 molecular sieve, and the price of template agent Expensive and other issues, to achieve the effect of facilitating industrial application, reducing the content of non-skeleton titanium, and reducing the time of hydrothermal crystallization

Active Publication Date: 2017-05-31
山西华阳集团新能股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional synthesis method, tetrapropylammonium hydroxide is used as a template, and its molar ratio to silicon content is 1:0.4-1.0, which is used in a large amount. However, the template is expensive, resulting in high synthesis cost of TS-1 molecular sieve.
Afterwards, many literatures reported cost-reducing synthesis methods, including finding alternatives to TPAOH, reducing the amount of TPAOH, etc. However, the synthesized TS-1 molecular sieve has large grains or low titanium skeleton content, which makes it difficult to achieve high catalytic activity.

Method used

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  • Synthetic method of TS-1 titanium silicate molecular sieve
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  • Synthetic method of TS-1 titanium silicate molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Preparation of precursor solution

[0033] Add the template agent to the silicon source, stir and hydrolyze at 25°C for 0.5h to obtain the mixed solution A; add the titanium source to the polyol at a molar ratio of 1:3, stir at 25°C for 0.5h to obtain the mixed solution B; , add the mixed solution B to the mixed solution A drop by drop. After the mixing is completed, gradually raise the temperature to 42°C and stir for 1 hour; raise the temperature again to 75°C, wash off the alcohol for 3 hours, and continue to replenish water to keep the liquid level unchanged; The mixed solution was transferred to a hydrothermal synthesis kettle for pre-crystallization at 110° C. for 24 hours, taken out and cooled to obtain a precursor solution. Among them, each material ratio (mole) silicon source SiO 2 : Titanium source TiO 2 : Templating agent: water is 1:0.100:0.30:20.

[0034] The silicon source is tetraethyl silicate, the titanium source is tetrabutyl titanate, and the p...

Embodiment 2

[0041] (1) Preparation of precursor solution

[0042] Add the template agent to the silicon source, stir and hydrolyze at 25°C for 1 hour to obtain the mixed solution A; add the titanium source to the polyol at a molar ratio of 1:5, and stir at 25°C for 0.5 hours to obtain the mixed solution B; Add the mixed solution B to the mixed solution A drop by drop. After mixing, gradually raise the temperature to 42°C, stir for 1 hour; raise the temperature again to 80°C, wash off the alcohol for 2 hours, and continue to replenish water to keep the liquid level unchanged; The solution was transferred to a hydrothermal synthesis kettle for pre-crystallization at 115°C for 22 hours, and cooled after taking it out to obtain a precursor solution. Among them, each material ratio (mole) silicon source SiO 2 : Titanium source TiO 2 : Templating agent: water is 1:0.125:0.40:20.

[0043]The silicon source is tetraethyl silicate, the titanium source is tetrabutyl titanate, and the polyhydric ...

Embodiment 3

[0050] (1) Preparation of precursor solution

[0051] Add the template agent to the silicon source, stir and hydrolyze at 25°C for 1 hour to obtain the mixed solution A; add the titanium source to the polyol at a molar ratio of 1:7, and stir at 25°C for 1 hour to obtain the mixed solution B; Add mixed solution B to mixed solution A drop by drop. After mixing, gradually raise the temperature to 45°C and stir for 0.5h; raise the temperature again to 80°C, wash off the alcohol for 2 hours, and continue to replenish water to keep the liquid level unchanged; The liquid was transferred to a hydrothermal synthesis kettle for pre-crystallization at 120° C. for 15 h, taken out and cooled to obtain a precursor liquid. Among them, each material ratio (mole) silicon source SiO 2 : Titanium source TiO 2 : Templating agent: water is 1:0.150:0.30:20.

[0052] The silicon source is tetraethyl silicate, the titanium source is tetrabutyl titanate, and the polyhydric alcohol is isopropanol. ...

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Abstract

The invention relates to a titanium silicate molecular sieve and a synthetic method thereof. The synthetic method comprises the following steps: mixing a silicon source, a titanium source, a template and water, stirring and hydrolyzing, putting the product into a hydro-thermal synthesis kettle and carrying out a pre-crystallization reaction; mixing the pre-crystallization product and a silicon source, uniformly stirring, carrying out hydro-thermal synthesis, washing and roasting to obtain the TS-1 molecular sieve. The synthesis process of the titanium silicate molecular sieve is easy to control and has good repeatability. Meanwhile, the catalyst has a higher catalytic activity, and use amount of the template is greatly reduced and synthesizing cost of the titanium silicate molecular sieve is decreased. The synthetic method of the invention is convenient for industrial production.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, and in particular relates to a molecular sieve and a synthesis method thereof, that is, a synthesis method of TS-1 titanium-silicon molecular sieve. Background technique [0002] Titanium silicate molecular sieve (TS-1) is a heteroatom molecular sieve developed in the early 1980s. It introduces titanium atoms into the silicon framework with MFI topology to form a special Ti-O-Si bond, which makes it have both catalytic oxidation activity and type-selective catalytic performance. TS-1 is mostly used to catalyze a variety of organic oxidation reactions, especially the oxidation system of hydrogen peroxide, such as phenol hydroxylation, cyclic ketone ammoxidation, etc. Its catalytic process is simple, with few other by-products, and it has good atom economy and environmental friendliness properties, showing good application prospects. [0003] The catalytic activity of TS-1 molecular sieve...

Claims

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Application Information

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IPC IPC(8): C01B37/00B01J29/89C07C37/60C07C39/08
CPCY02P20/52C01B37/005B01J29/89C01P2002/72C01P2004/03C01P2004/62C07C37/60C07C39/08
Inventor 赵君冯志武李伟斌潘丽刘甜甜史竹青
Owner 山西华阳集团新能股份有限公司
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