Method for preparing TS-1 titanium-silicon molecular sieve with nanoclusters

A technology of titanium-silicon molecular sieves and nanocrystals, which is applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of high production costs of titanium-silicon molecular sieves, high production cost skeleton titanium content, non Low content of skeleton titanium, etc., to achieve the effect of reducing anatase, uniform solution concentration distribution, and reducing non-skeleton titanium

Active Publication Date: 2016-11-16
QINGDAO UNIV OF SCI & TECH
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  • Abstract
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  • Claims
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Problems solved by technology

[0005] In order to solve the problems of high production cost, cumbersome preparation method, poor repeatability, and low content of non-skeleton titanium in the prior art to produce titanium-silicon molecular sieve, the present invention proposes a method for preparing TS-1 titanium-silicon molecular sieve by using nanocrystal clusters. The production cost is reduced, the preparation method is simple, the skeleton titanium content is high, and the repeatability is good

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  • Method for preparing TS-1 titanium-silicon molecular sieve with nanoclusters
  • Method for preparing TS-1 titanium-silicon molecular sieve with nanoclusters

Examples

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Embodiment 1

[0038] Step 1: Mix tetrapropylammonium hydroxide and ethyl orthosilicate at 20°C under anhydrous conditions as A, organic alkali source tetramethylammonium hydroxide as B, and titanium source as butyl titanate Denote it as C; in an ultrasonic environment, mix A, B, and C in a certain proportion and drop them into a beaker and keep the pH value = 9-12, then place it in an ultrasonic environment for crystallization for 30 minutes, and filter to obtain nano clusters and dry them. Step 2: Take a certain proportion of dried nanocrystal clusters and put them into the bottom of the beaker, then mix tetrapropylammonium hydroxide and tetramethylammonium hydroxide to form D, and mix ethyl orthosilicate and butyl titanate to form E ; Under anhydrous and ultrasonic conditions, add D to the beaker, then add E dropwise to the beaker, and obtain the mixed solution F after the titration is completed, move F to the polytetrafluoroethylene reactor, and finally add 200mL of Water, crystallized ...

Embodiment 3

[0040] Step 1: Mix tetrapropylammonium hydroxide and ethyl orthosilicate at 25°C under anhydrous conditions as A, organic alkali source tetraethylammonium hydroxide as B, and titanium source as titanium trichloride as C ; In an ultrasonic environment, mix A, B, and C in a certain proportion and drop them into a beaker and keep the pH value = 11-13, then place it in an ultrasonic environment for crystallization for 90 minutes, filter to obtain nanocrystal clusters and Let it dry. Step 2: Take a certain proportion of dried nano-crystal clusters and put them into the bottom of the beaker, then mix tetrapropylammonium hydroxide and tetraethylammonium hydroxide evenly into D, and mix ethyl orthosilicate and titanium trichloride evenly It is E; under the condition of no water and ultrasound, add D into the beaker, then add E dropwise into the beaker, after the titration is completed, the mixed solution F is obtained, move F to the polytetrafluoroethylene reactor, and finally add 10...

Embodiment 4

[0042] Step 1: Mix tetrapropylammonium hydroxide and ethyl orthosilicate at 20°C under anhydrous conditions as A, organic alkali source tetramethylammonium hydroxide as B, titanium source titanyl sulfate as C; In an ultrasonic environment, mix A, B, and C in a certain proportion and drop them into a beaker and keep the pH value = 11-13, then place it in an ultrasonic environment for crystallization for 70 minutes, and filter to obtain nanocrystal clusters after the ultrasonic is over. its dry. The second step: take a certain proportion of dried nano-crystal clusters and put them into the bottom of the beaker, then mix tetrapropylammonium hydroxide and tetramethylammonium hydroxide evenly to D, and mix ethyl orthosilicate and titanyl sulfate evenly to D E: Under the condition of no water and ultrasonic, add D into the beaker, then add E dropwise into the beaker, after the titration is completed, the mixed solution F is obtained, move F to the polytetrafluoroethylene reactor, an...

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Abstract

The invention relates to a method for preparing a TS-1 titanium-silicon molecular sieve with nanoclusters. The method includes the following steps that a template agent and a silicon source are mixed into A under 5-90 DEG C, an alkali source is recorded as B, and a titanium source is recorded as C; A, B and C are mixed in the ultrasonic environment and dropwise added into a beaker, and the pH value is kept to be 8-13; crystallization is carried out for 5-55 min in the normal-temperature and normal-pressure ultrasonic environment after titration is finished, and TS-1 nanoclusters are obtained through filtration; a template agent and an alkali source are mixed into D, and a silicon source and a titanium source are mixed into E; D is mixed with the dried nanoclusters under the anhydrous ultrasonic condition, E is added, mixed liquor F is obtained after titration is finished, F is transferred into a reaction kettle, 50-200 mL of water is added, the temperature is controlled to be 150-200 DEG C, washing, drying and roasting are carried out after crystallization is carried out for 12-120 h, and TS-1 is obtained. The method for preparing TS-1 is simple and good in repeatability and solves the problem of high production cost.

Description

technical field [0001] The invention relates to a method for preparing TS-1 titanium-silicon molecular sieve by using nano crystal clusters. Background technique [0002] Titanium-silicon molecular sieve TS-1 is a new type of heteroatom molecular sieve synthesized for the first time in 1981 by Marco Taramasso et al. in Italy. It is found that TS-1 has the MFI structure like ZSM-5, and is a catalytic material with good catalytic selective oxidation activity, suitable for a series of organic chemical reactions using hydrogen peroxide as the oxidant (such as the epoxidation reaction of olefin , Hydroxylation of aromatic hydrocarbons, oximation of ketones and selective oxidation of alkanes and alcohols, etc.) and the reaction conditions are mild, and the by-product is water, which does not pollute the environment. Titanium silicate molecular sieves have excellent catalytic activity and selectivity when used as catalysts, and are widely used in petrochemical, fine chemical and m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
CPCC01B39/085C01P2002/72C01P2002/82
Inventor 王广建李佳佳邴连成王芳
Owner QINGDAO UNIV OF SCI & TECH
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