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Preparation technology of titanium silicon molecular sieve catalyst

A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of preparation of titanium-silicon molecular sieve catalysts, can solve the problems of decreased catalyst activity, unsatisfactory catalyst strength, etc.

Inactive Publication Date: 2006-09-27
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Patent 4,701,428 reported that n-ethyl silicate was used as a binding agent, and the particle size of the catalyst was increased by spray drying and granulation, but the activity of the obtained catalyst decreased, and the strength of the catalyst could not satisfy users in practical applications.

Method used

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  • Preparation technology of titanium silicon molecular sieve catalyst
  • Preparation technology of titanium silicon molecular sieve catalyst
  • Preparation technology of titanium silicon molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Add 400g of 12.5% ​​tetrabutylammonium hydroxide aqueous solution into a 1000mL glass reactor, add 180g of tetraethyl silicate, stir vigorously for 15min, and raise the temperature to 50-60°C. Add 10 g of n-butyl titanate into 55 g of isopropanol, stir to dissolve, add the obtained n-butyl titanate isopropanol solution into the reactor dropwise, and stir at the same time. After the dropwise addition, continue to stir for 2 hours, and raise the temperature to At 85°C, remove the alcohol in the reaction system, add 200g of deionized water, stir for 1 hour, and let stand for one day to obtain raw gum.

[0031] Put the original rubber into a 1L stainless steel autoclave, seal the reactor, start stirring, and control the heating rate of the reactor through a temperature program temperature controller. The heating curve of the reactor is as follows: figure 1 shown. After 120 hours, the temperature controller was turned off, the stirring was stopped, the temperature was natur...

Embodiment 2

[0037] The system of catechol and hydroquinone produced by hydroxylation of phenol was investigated. The reaction was carried out in a 1-liter four-neck flask, with 30% hydrogen peroxide as the oxidant and acetone as the solvent, the reaction temperature was 60°C, the hydrogen peroxide was added within 1 hour, and the reaction was continued for 10 hours after the dropwise addition. The ratio of reaction materials is: phenol: H 2 o 2 =3:1 (mol / mol), phenol:acetone=1:2 (v / v), phenol:catalyst=10:1 (mass ratio). Catalyst activity as H 2 o 2 The selectivity of forming quinone as an indicator:

[0038] λ = ( y CA + y HQ ) · w t / 110 w ...

Embodiment 3

[0042] The system of cyclohexane oxidation to cyclohexanone was investigated. Acetone was used as solvent and 30% hydrogen peroxide was used as oxidant, and the reaction was carried out in a stirred 100ml pressure reactor lined with polytetrafluoroethylene. 0.42g catalyst, 20ml acetone, 10.5ml 30% H 2 o 2 , 4ml cyclohexane was placed in a 100ml pressure vessel. The temperature was raised under stirring, the timing was started after the temperature reached 100° C., and the temperature was lowered after 8 hours of reaction. The catalyst in the product was filtered.

[0043] The composition of the sample is analyzed by gas chromatography. The chromatographic column is an OV-101 capillary column with a diameter of 0.2mm and a length of 60m. Hydrogen flame detection is carried out. The chromatographic analysis conditions are as follows:

[0044] Carrier gas (N 2 ) Reflux ratio: 35ml / min, FID temperature: 285°C, columnarity: 55°C.

[0045] The selectivity to H2O2 is λ=0.85.

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Abstract

The preparation process of Ti-Si molecular sieve catalyst includes the following steps: reacting titanium source in alcohol solution and silicon source template agent solution for 3-15 hr and adding water in 3-8 times the silicon source into the reaction product to obtain colloid solution; reacting the colloid solution through heating in non-steady state program control condition to crystallize; filtering, washing, drying and roasting to obtain white solid catalyst powder. The non-steady state program control condition increases the size of the molecular sieve, and this reduces the filtering resistance greatly, eliminates the loss of catalyst, lowers the production cost and reduces the crushing of catalyst during use.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve catalyst. Background technique [0002] Titanium-silicon molecular sieve catalysts play a very important role in the selective oxidation of organic compounds, such as the epoxidation of propylene with hydrogen peroxide under the action of titanium-silicon molecular sieve catalysts to prepare propylene oxide, such as cyclohexanone under the action of titanium-silicon molecular sieve catalysts Use hydrogen peroxide to carry out ammoxidation to prepare cyclohexanone oxime, such as phenol under the action of titanium silicon molecular sieve, prepare catechol and hydroquinone with hydrogen peroxide oxidation, the most typical titanium silicon molecular sieve catalyst is document 1( Taramasso M, et al.Preparation of porous crystalline synthetic material comprised of silicon and titanium oxides [P]. US: 4410501, 1983) and literature 2 (Reddy J.S., et al. Titanium Silicalite-2:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/06B01J29/89
Inventor 曹贵平张明华徐军
Owner EAST CHINA UNIV OF SCI & TECH
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