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Synthesis method of titanium-silicon molecular sieve TS-1

A titanium silicon molecular sieve, TS-1 technology, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effect of good catalytic activity

Active Publication Date: 2014-12-03
JIANGSU YIDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

After cooling, perform solid-liquid separation operation on the crystallization reactant

Method used

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  • Synthesis method of titanium-silicon molecular sieve TS-1
  • Synthesis method of titanium-silicon molecular sieve TS-1
  • Synthesis method of titanium-silicon molecular sieve TS-1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In this example, the feeding is carried out according to the following ratio: n (tetraethyl orthosilicate): n (tetrabutyl titanate): n (tetrapropylammonium bromide): n (H 2 O):n(IPA)=1:0.025:0.4:40:0.6. First, tetraethyl orthosilicate and distilled water were mixed under the condition of mechanical stirring, and dilute acid was added to adjust the pH value of the solution to 3.0, and the temperature was kept at 40° C. for 1 hour. Add the isopropanol solution of tetrabutyl titanate and dilute ammonia solution to the silicon source hydrolyzate at the same time, then add the template agent to the above hydrolyzate, and adjust the pH value of the solution to 13 with triethylamine solution, and then 40 °C Constant temperature 1h. The temperature of the reaction solution was raised to 85°C, and the alcohol was purged with nitrogen. Cool down and replenish water after alcohol catching. The obtained titanium-silicon precursor gel was divided into three sealed stainless steel...

Embodiment 2

[0039] In this example, the feeding is carried out according to the following ratio: n (tetrabutyl orthosilicate): n (tetraethyl titanate): n (tetrapropylammonium bromide): n (H 2 O):n(IPA)=1:0.03:0.3:60:0.8. Firstly, tetrabutyl orthosilicate and distilled water were mixed under the condition of mechanical stirring, and dilute acid was added to adjust the pH value of the solution to 3.0, and the temperature was kept at 40° C. for 1 hour. Add the isopropanol solution of tetraethyl titanate and dilute ammonia solution to the silicon source hydrolyzate at the same time, then add the template agent to the above hydrolyzate, and adjust the pH value of the solution to 13 with triethylamine solution, and then 40 °C Constant temperature 1h. The temperature of the reaction solution was raised to 85°C, and the alcohol was purged with nitrogen. Cool down and replenish water after alcohol catching. The obtained titanium-silicon precursor gel was divided into three sealed stainless stee...

Embodiment 3

[0041] In this example, the feeding is carried out according to the following ratio: n (tetraethyl orthosilicate): n (tetrabutyl titanate): n (tetrapropyl ammonium hydroxide): n (H 2 O):n(IPA)=1:0.035:0.5:50:1. First, tetraethyl orthosilicate and distilled water were mixed under the condition of mechanical stirring, and dilute acid was added to adjust the pH value of the solution to 3.0, and the temperature was kept at 40° C. for 1 hour. Add the isopropanol solution of tetrabutyl titanate and dilute ammonia solution to the silicon source hydrolyzate at the same time, then add the template agent to the above hydrolyzate, and adjust the pH value of the solution to 13 with triethylamine solution, and then 40 °C Constant temperature 1h. The temperature of the reaction solution was raised to 85°C, and the alcohol was purged with nitrogen. Cool down and replenish water after alcohol catching. The obtained transparent titanium-silicon precursor gel was divided into three sealed st...

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Abstract

The invention relates to a synthesis method of a titanium-silicon molecular sieve TS-1. The method comprises the steps of: preparing titanium-silicon gel from a titanium source, a silicon source, a template agent and water by a certain mole ratio, and hydrothermally crystallizing the gel in a closed reaction kettle by utilizing the pressure generated by the gel self; and then filtering, washing, drying and roasting, thus obtaining the molecular sieve TS-1. According to the method, the titanium source can be effectively hydrolyzed in the preparation of a precursor, the sedimentation of TiO2 is reduced and avoided even, and Ti is enabled to enter a framework, so that the molecular sieve TS-1 with high activity is prepared. When the molecular sieve TS-1 is used as a catalyst for propylene epoxidation in a pilot experiment, the conversion rate of hydrogen peroxide and the selectivity of epoxy propane are enhanced greatly.

Description

technical field [0001] The invention relates to a synthesis method of titanium silicon molecular sieve TS-1. It belongs to the field of molecular sieve preparation. Background technique [0002] Titanium silicalite molecular sieve refers to a type of heteroatom molecular sieve containing titanium atoms in the zeolite molecular sieve framework. In 1983, Taramasso et al reported the preparation of titanium-silicon molecular sieve TS-1 by hydrothermal method. Titanium silicalite molecular sieve is a derivative of Silicalite-1 zeolite, and TS-1 is a titanium-containing heteroatom molecular sieve with the same MFI structure as silica-alumina molecular sieve ZSM-5. The excellent catalytic oxidation activity of titanium silicate molecular sieves is based on the neutral Ti 4+ Active neutral, its remarkable function is to H 2 o 2 Participated in the selective oxidation of organic matter has a good effect, and will not be deeply oxidized. TS-1 can catalyze epoxidation of olefins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 刘准曹惠庆吴建磊张虎祝义鹏戴露
Owner JIANGSU YIDA CHEM
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