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Preparation method of TS-2 molecular sieve/nanometer silicon carbide whisker composite catalyst

A nano-silicon carbide, titanium-silicon molecular sieve technology, applied in molecular sieve catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of long reaction time, difficult to avoid, complicated operation process, etc.

Inactive Publication Date: 2015-01-28
华文蔚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This synthesis method has the following disadvantages: the operation process is complicated, the reaction time is long, and it takes 6 to 30 minutes, and it is difficult to avoid the hydrolysis of tetraethyl titanate and polymerization into non-bulk anatase TiO2
At present, no one has directly mixed TS-1 powder and CNF to prepare composite catalysts to solve the liquid phase dispersion and separation problems of TS-1 industrial applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add a mixture of 50.0 grams of tetraethyl orthosilicate, 22 grams of tetrabutylammonium hydroxide and 1.6 milliliters of 17% (weight) concentration of titanium trichloride solution to a container with a stirring device, stir and mix, and then add nano 50 grams of silicon carbide whiskers; slowly heated to 70° C., kept stirring for 24 hours, and at the same time, oxygen or air was passed into the reaction mixture.

[0021] The obtained reaction mixture was transferred into a stainless steel high-pressure crystallization kettle lined with polytetrafluoroethylene, and the crystallization kettle was sealed, and the temperature was raised to 120° C. within 2 hours, and the temperature was kept constant for 120 hours. Then cool, filter and recover the solid product, wash with water, dry at 120°C, and then calcinate to a temperature of 250°C to obtain TS-2 titanium-silicon molecular sieve / nano-silicon carbide whisker composite catalyst. The molar ratio of each component in the...

Embodiment 2

[0023] According to each step of embodiment 1, just tetrabutyl ammonium hydroxide add-on is 40 grams, and the add-on of 17% (weight) concentration titanium trichloride solution is 0.8 milliliters, and nano-silicon carbide add-on is 100 grams. The heating temperature when passing oxygen or air is 90°C, the stirring and heating time is 36 hours, the crystallization temperature is 200°C, and the crystallization time is 36 hours, so that the molar ratio of each component in the reaction mixture is: SiO2 / TiO2=200 , OH- / SiO2=0.6, H2O / SiO2=60.

Embodiment 3

[0025] According to each step of embodiment 1, just tetrabutyl ammonium hydroxide add-on is 22 grams, and the add-on of 17% (weight) concentration titanium trichloride solution is 4.0 milliliters, nano silicon carbide whisker 150 grams. When feeding oxygen or air, the heating temperature is 80°C, the stirring and heating time is 72 hours, the crystallization temperature is 175°C, and the crystallization time is 96 hours, so that the molar ratio of each component in the reaction mixture is: SiO2 / TiO2= 40, OH / SiO2=0.35, H2O / SiO2=80.

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PUM

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Abstract

The invention provides a preparation method of a TS-2 molecular sieve / nanometer silicon carbide whisker composite catalyst. The method comprises the following steps: a titanous compound is taken as a titanium source, tetraethyl orthosilicate or a silica solution is taken as a silicon source, and quaternary ammonium base or quaternary ammonium salt and organic amine are taken as raw material, wherein in the reaction mixture, the molar ratio value of Si to Ti is 20-200, the molar ratio value of OH- to SiO2 is 0.03-0.06, the molar ratio value of H2O to SiO2 is 60-100, and the molar ratio value of organic amine to SiO2 is 0.1-0.5, stirring and mixing are performed, nanometer silicon carbide whiskers are added at the temperature of 70-90 DEG C, and stirring is performed for 24-72 h, wherein the addition amount of the nanometer silicon carbide whiskers is as follows: the weight ratio of the nanometer silicon carbide whiskers to the titanium source is 1:(1-20); oxygen or air is introduced into the reaction mixture at the same time; then the reaction material is subjected to crystallization for 24-120 h at the crystallization temperature of 115-250 DEG C, the mixture obtained through crystallization is separated, washed and dried, and then is roasted to be prepared into the TS-2 molecular sieve / nanometer silicon carbide whiskers; the diameter of each nanometer silicon carbide whisker is 2-30 nm; the TS-2 molecular sieve / nanometer silicon carbide whisker composite catalyst is coacervate particles with the diameter of 1-10 microns; the quaternary ammonium base adopts tetrabutyl ammonium hydroxide, the organic amine includes hexamethylenediamine, triethylamine, tripropylamine and diethylamine; the quaternary ammonium salt adopts tetrabutyl ammonium halide, and the titanous compound includes titanium trichloride and titanium tribromide; the roasting temperature is 200-350 DEG C.

Description

technical field [0001] The invention relates to a preparation method of a TS-2 titanium silicon molecular sieve / nano silicon carbide whisker composite catalyst. Background technique [0002] Titanium silicate molecular sieve is a new heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized so far. This type of molecular sieve has excellent catalytic activity and directional oxidation performance for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oxidation of cyclohexanone, and oxidation of alcohols. They are used as redox molecular sieves The catalyst has a good application prospect. [0003] Titanium silicalite (TS-1 for short) with MFI structure has excellent catalytic oxidation activity and selectivity. One of the main factors affecting the activity of TS-1 is particle size. TS-1 with a small particle s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89
Inventor 华文蔚
Owner 华文蔚
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