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Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve

A technology of skeleton titanium and molecular sieves, which is applied in the preparation of organic compounds, molecular sieve catalysts, molecular sieves and base exchange compounds, etc., can solve the problems of increasing synthesis costs and prolonging the preparation process of molecular sieves, and achieve short crystallization time and high catalytic oxidation activity and selectivity, the effect of reducing the synthesis cost

Active Publication Date: 2016-07-27
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method can eliminate the non-framework titanium in the synthesis of TS-1, it prolongs the molecular sieve preparation process and increases the synthesis cost

Method used

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  • Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve
  • Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve
  • Alcohol-removal-free preparation method for rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Add 50g TEOS into a three-necked flask, add 36g TPAOH aqueous solution (25wt.%) and 49g deionized water at 25°C under magnetic stirring, and hydrolyze for 1h to obtain a silicon source hydrolysis solution; disperse 2g TBOT into 15gIPA, then add 13.6g TPAOH aqueous solution ( 25wt.%) and 24gH 2 O, hydrolysis at room temperature for 0.5h to obtain a titanium hydrolysis solution; mix the titanium hydrolysis solution with the silicon hydrolysis solution, then add 25ml of glucose aqueous solution (5wt%), after stirring for 0.5h, transfer the synthetic glue to the In a fluorine-lined stainless steel synthesis kettle, crystallize at 170°C for 6 hours under autogenous pressure, take the kettle to cool, wash, dry, and roast the TS-1 sample of the crystallized product, and code it as A2. Sample X-ray diffraction (XRD) and ultraviolet-visible absorption (UV-Vis) spectra are shown in figure 1 and figure 2 .

Embodiment 2

[0045] Add 50g of TEOS into a three-necked flask, add 18.6g of ammonia solution (25wt.%) and 49g of deionized water at 25°C under magnetic stirring, and hydrolyze for 1 hour to obtain a silicon source hydrolysis solution; disperse 2g of TBOT into 15g of IPA, and then add 13.6g of TPAOH Aqueous solution (25wt.%) and 24gH 2 O, hydrolysis at room temperature for 0.5h to obtain a titanium source hydrolysis solution; mix the titanium source hydrolysis solution with the silicon source hydrolysis solution, then add 25mL glucose aqueous solution (10wt%), after stirring for 30min, transfer the synthetic glue to a polytetrafluoroethylene In a lined stainless steel synthesis kettle, crystallize at 170°C for 24 hours under autogenous pressure, take the kettle to cool, wash, dry, and roast the TS-1 sample of the crystallized product, and code it as A3. Sample X-ray diffraction (XRD) and ultraviolet-visible absorption (UV-Vis) spectra are shown in figure 1 and figure 2 .

Embodiment 3

[0047] Add 50g of TEOS into a three-necked flask, add 6.5g of diethylamine and 49g of deionized water at 25°C under magnetic stirring, and hydrolyze for 1.5h to obtain a silicon source hydrolysis solution; disperse 2g of TBOT into 15g of IPA, and then add 28g of TPAOH aqueous solution (25wt. %) and 10gH 2 O, hydrolyze at room temperature for 0.5h to obtain a titanium source hydrolysis solution; mix the titanium source hydrolysis solution with the silicon source hydrolysis solution, then add 25mL urea aqueous solution (2.5wt%), stir for 30min, and transfer the synthetic glue to the In a fluorine-lined stainless steel synthesis kettle, crystallize at 170°C for 6 hours under autogenous pressure, take the kettle to cool, and wash, dry, and roast the TS-1 sample of the crystallized product, which is coded as A4. Sample X-ray diffraction (XRD) and ultraviolet-visible absorption (UV-Vis) spectra are shown in figure 1 and figure 2 .

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Abstract

The invention discloses a preparation method and application of a rapidly-synthesized high-framework-titanium-content titanium silicalite molecular sieve. An organic compound of a non-surfactant is added to a synthetic glue solution, so that generation of extra framework titanium is restrained, and growth of a molecular sieve structure is promoted. A certain quantity of an organic compound of one or more non-surfactants is added to the TS-1 synthetic glue solution, polymerization of silicon-titanium species in the synthetic glue solution is affected through the hydrogen-bond interaction, agglomeration of titanium species is restrained accordingly, the speed at which titanium enters a molecular sieve framework is increased, and formation of the molecular sieve framework structure is promoted. Compared with a conventional method for hydro-thermal synthesis of the TS-1 molecular sieve, no alcohol removal is needed in the process of preparing the TS-1 synthetic glue solution through the method, the synthesis process is simplified, and industrial production is convenient. The content of framework titanium in the TS-1 prepared through the method is high, catalytic activity and selectivity are obviously improved, and the method is mainly shown in reactions such as olefin epoxidation, aromatic hydroxylation, hydroxylation of phenol, ammonia ketone oximation and alkane oxidation.

Description

technical field [0001] The invention relates to an alcohol-free preparation method for rapidly synthesizing titanium-silicon molecular sieves with high skeleton titanium content, and belongs to the field of inorganic synthesis and catalytic chemistry. Background technique [0002] Titanium silicate molecular sieve (TS-1) in H 2 o 2 In the mild reaction system of oxidant, it can catalyze olefin epoxidation, aromatic hydrocarbon hydroxylation, ketone ammonia oximation and alkane oxidation with excellent selectivity and high catalytic activity, and its by-product is only water, which is in line with green chemistry and atom economy requirements, and thus arouse widespread concern. [0003] In 1983, the Italian scientist Taramasso and his collaborators disclosed the hydrothermal synthesis of TS-1 for the first time in the patent US4410501, which is called "classical synthesis". Specifically, two methods are included: one method is to use orthoethyl silicate (TEOS) as the sili...

Claims

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Application Information

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IPC IPC(8): C01B39/08B01J29/89C07D301/12C07D303/04C07C37/60C07C39/08
CPCB01J29/89C01B39/085C01P2002/72C01P2002/84C07C37/60C07D301/12C07D303/04C07C39/08
Inventor 王祥生宋万仓龙化云
Owner DALIAN UNIV OF TECH
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