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Lamellar titanium silicalite molecular sieve TS-1 as well as preparation method and application thereof

A titanium-silicon molecular sieve, TS-1 technology, applied in crystalline aluminosilicate zeolite, organic chemistry, etc., can solve the problems of cumbersome steps, high production cost and complicated process of sheet MFI molecular sieve, and achieve high conversion rate of hydrogen peroxide, High selectivity, the effect of increasing the titanium content of the skeleton

Active Publication Date: 2021-06-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above work, the preparation of sheet-like MFI molecular sieves by the exfoliation method is cumbersome and complicated.
However, when organosilane is used as the template for sheet-like molecular sieves, it usually takes more time and effort to synthesize the special template, which is expensive and has high production costs, and there is still a certain distance from industrial application.

Method used

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  • Lamellar titanium silicalite molecular sieve TS-1 as well as preparation method and application thereof
  • Lamellar titanium silicalite molecular sieve TS-1 as well as preparation method and application thereof
  • Lamellar titanium silicalite molecular sieve TS-1 as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The preparation of embodiment 1 sample TS-1-1

[0042] First, as shown in Table 1, the molar ratio of SiO 2 :0.03TiO 2 :0.25R:0.05M:40H 2 O Calculate the amount of each raw material required. Tetrapropylammonium hydroxide was added into deionized water, stirred and dissolved to obtain a mixed solution. Add tetraethyl orthosilicate to the above mixed solution, stir at 40°C for 4h; then add isopropyl titanate, and stir at 50°C for 3h; add crystallization aid sodium persulfate into solution and add to the above mixing The solution was stirred at 50° C. for 0.5 h; then the above mixed solution was transferred to a high-pressure crystallization reactor, and statically crystallized at 180° C. for 36 h. The obtained product is centrifuged, washed, dried and calcined to finally obtain the titanium-silicon molecular sieve TS-1-1.

Embodiment 2

[0043] The preparation of embodiment 2 sample TS-1-2

[0044] First, as shown in Table 1, the molar ratio of SiO 2 :0.03TiO 2 :0.25R:0.1M:40H 2 O Calculate the amount of each raw material required. Tetrapropylammonium hydroxide was added into deionized water, stirred and dissolved to obtain a mixed solution. Add tetraethyl orthosilicate to the above mixed solution, stir at 40°C for 4h; then add isopropyl titanate, and stir at 50°C for 3h; add crystallization aid sodium persulfate into solution and add to the above mixing The solution was stirred at 50° C. for 0.5 minutes; then the above mixed solution was transferred to a high-pressure crystallization reactor, and statically crystallized at 150° C. for 72 hours. The obtained product is centrifuged, washed, dried and calcined to finally obtain the titanium-silicon molecular sieve TS-1-2.

Embodiment 3

[0045] The preparation of embodiment 3 sample TS-1-3

[0046] First, as shown in Table 1, the molar ratio of SiO 2 :0.03TiO 2 :0.25R:0.15M:40H 2 O Calculate the amount of each raw material required. Tetrapropylammonium hydroxide was added into deionized water, stirred and dissolved to obtain a mixed solution. Add tetraethyl orthosilicate to the above mixed solution, stir at 40°C for 4h; then add isopropyl titanate, and stir at 50°C for 3h; add crystallization aid sodium persulfate into solution and add to the above mixing The solution was stirred at 50° C. for 0.5 h; then the above mixed solution was transferred to a high-pressure crystallization reactor, and statically crystallized at 200° C. for 24 h. The obtained product is centrifuged, washed, dried and calcined to finally obtain the titanium-silicon molecular sieve TS-1-3.

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Abstract

The invention discloses a lamellar titanium silicalite molecular sieve TS-1, the lamellar titanium silicalite molecular sieve TS-1 has an MFI topological structure, a b axis is shorter than an a axis and a c axis, and the grain size of the lamellar titanium silicalite molecular sieve TS-1 is 1-10 [mu] m * 0.05-0.8 [mu] m * 0.1-2 [mu] m. The invention also discloses a preparation method and application of the lamellar titanium silicalite molecular sieve TS-1. The straight pore channel direction (b-axis) of the TS-1 molecular sieve prepared by the method is a main molecular diffusion path, and the diffusion efficiency of a reaction product is improved due to the thinner b-axis thickness. The lamellar titanium silicalite molecular sieve synthesized in the invention shows the characteristics of high hydrogen peroxide conversion rate and high epoxypropane selectivity in the epoxidation reaction of propylene.

Description

technical field [0001] The application relates to a flaky titanium-silicon molecular sieve TS-1 and its preparation method and application, belonging to the field of chemistry and chemical engineering. Background technique [0002] Among many kinds of porous materials with different properties, zeolite molecular sieves are used as catalysts, catalyst carriers and adsorption separation materials in petrochemical, fine It is widely used in chemical industry and coal chemical industry (Chem. Rev., 1997, 97, 2373-2419; Chem. Eng., 2011, 118, 16-20). [0003] In 1983, Italian scientist Taramasso et al [US patent, 4410501, 1983, 10, 18] first reported the preparation method of Titanium Silicalite-1 (TS-1) titanium silicon molecular sieve with MFI topology. The isolated four-coordinated titanium atom in the framework structure of TS-1 molecular sieve has a unique catalytic oxidation function, which makes it have important applications in the fields of olefin epoxidation and phenol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C07D301/12C07D303/04
CPCC01B39/08C07D301/12C07D303/04C01P2002/72C01P2004/03
Inventor 张晓敏许磊陈磊史鑫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI