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A kind of honeycomb hexagonal titanium silicon molecular sieve and its preparation method and application

A titanium-silicon molecular sieve, hexagonal technology, applied in the direction of molecular sieve catalyst, molecular sieve compound, molecular sieve characteristic silicate, etc., to achieve the effect of reducing production cost and improving stability and activity

Active Publication Date: 2019-12-20
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Usually, the morphology of titanium-silicon molecular sieves synthesized by traditional methods is ellipsoidal, and the preparation of titanium-silicon molecular sieves with new shapes requires appropriate addition of surfactants.

Method used

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  • A kind of honeycomb hexagonal titanium silicon molecular sieve and its preparation method and application
  • A kind of honeycomb hexagonal titanium silicon molecular sieve and its preparation method and application
  • A kind of honeycomb hexagonal titanium silicon molecular sieve and its preparation method and application

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preparation example Construction

[0041] On the other hand, the preparation method of the titanium-silicon molecular sieve TS-1 provided by the present application comprises the following steps:

[0042] (1) Mixing the microporous template agent, water and silicon source to obtain a mixed solution 1;

[0043](2) mixing the mixed solution 1 with the mixed solution 2 containing the titanium source and isopropanol to obtain the mixed solution 3;

[0044] (3) aging the mixed solution 3 and removing alcohol to obtain the gel solution 5;

[0045] (4) Calcining the gel solution 5 after crystallization, centrifugal washing, and drying to obtain hexagonal-like titanium-silicon molecular sieve TS-1.

[0046] The preparation method of the titanium-silicon molecular sieve TS-1 of the present application uses a micro-template agent and isopropanol as a solvent, and reacts without reflux, especially using tetrapropylammonium hydroxide TPAOH as a template agent, and the synthesized product is Cylindrical titanium silicate ...

Embodiment 1

[0078] Preparation of Nanometer Ti-Si Molecular Sieve TS-1

[0079] Get 3g tetrapropylammonium hydroxide (molecular weight 203,0.015mol) and place in the beaker, add 12.48g tetraethyl orthosilicate (molecular weight 208,0.06mol) and 16.2g H 2 O (molecular weight 18, 0.9 mol) was stirred for 30 minutes to obtain solution A. Take 2.24mL isopropanol (molecular weight 60, 0.0294mol) and 0.5g n-butyl titanate (molecular weight 340, 0.0015mol) and mix evenly, add to A at a rate of 0.01ml / min and stir for 3 hours to obtain solution B. Aging at 60°C for 6 hours, and raising the temperature to 90°C at a rate of 5-6°C / min, removing alcohol at 90°C for 12 hours to a transparent gel liquid. Put the transparent gel liquid into an autoclave, crystallize at 170°C for 18 hours, take it out, wash and dry it, and bake it in an air atmosphere at 550°C for 6 hours. The obtained silicon-titanium molecular sieve TS-1, after testing, its shape is a hexagonal prism or a hexagonal prism, the longest...

Embodiment 2

[0081] Preparation of Nanometer Ti-Si Molecular Sieve TS-1

[0082] Get 6.09g tetrapropyl ammonium hydroxide (molecular weight 203,0.03mol) and place in the beaker, add 12.48g tetraethyl orthosilicate (molecular weight 208,0.06mol) and 48.6g H 2O (molecular weight 18, 2.7mol) was stirred for 30 minutes to obtain solution A. Take 2.24mL isopropanol (molecular weight 60, 0.0294mol) and 0.5g n-butyl titanate (molecular weight 340, 0.0015mol) and mix evenly, add to A at a rate of 0.01ml / min and stir for 3 hours to obtain solution B. Aging at 60°C for 6 hours, and raising the temperature to 90°C at a rate of 5-6°C / min, removing alcohol at 90°C for 12 hours to a transparent gel liquid. Put the transparent gel liquid into an autoclave, crystallize at 170°C for 18 hours, take it out, wash and dry it, and bake it in an air atmosphere at 550°C for 6 hours. The silicon-titanium molecular sieve TS-1 has been tested. Its shape is hexagonal prism or similar hexagonal prism. The longest di...

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Abstract

The invention discloses a honeycomb hexagonal titanium-silicon molecular sieve and its preparation method and application. A titanium-silicon molecular sieve TS-1 has a hexagonal prism-like or hexagonal prism-like morphology, and the ratio of the height of the hexagonal prism or hexagonal prism to the longest diagonal line of the hexagonal bottom is 0.8-1.2. The preparation method of the molecular sieve TS‑1 does not require reflux operation in the process. By mixing isopropanol and titanium source and controlling the appropriate feeding sequence and heating rate, a hexagonal or hexagonal-like titanium-silicon molecular sieve can be prepared. TS‑1. The section of the molecular sieve is hexagonal, and the catalytic activity and stability of the propylene epoxidation reaction are high.

Description

technical field [0001] The present invention relates to a catalyst, in particular to a titanium-silicon molecular sieve TS-1 and its preparation method, more specifically, to a titanium-silicon molecular sieve with a hexagonal section, its preparation method and application. Background technique [0002] Propylene oxide (PO), as the third largest organic chemical product in the production of propylene derivatives after polypropylene and acrylonitrile, is widely used in the preparation of derivatives such as polyurethane and polyester resins. At present, the main methods of producing PO in industry are chlorohydrin method and co-oxidation method. However, the chlorohydrin method does not meet the requirements of today's green environmental protection because of its great corrosion to equipment and the production of a large amount of waste water and chlorine-containing by-products. However, the economics of the co-oxidation method is restricted by a large number of by-product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00B01J29/89
CPCB01J29/89B01J2229/18C01B37/005C01P2002/72C01P2002/84C01P2004/03C01P2004/04C01P2004/40C01P2004/62
Inventor 冯翔盛楠宋钊宁林栋杨朝合刘熠斌陈小博李奕川
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)