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TS-1 molecular sieve with macroporous-microporous composite pore channel structure as well as preparation method and application of TS-1 molecular sieve

A TS-1, composite channel technology, used in molecular sieve compounds, molecular sieve catalysts, molecular sieve characteristic silicates, etc., can solve the problem that the diffusion efficiency of guest molecules in the molecular sieve channels cannot be effectively improved, the improvement of molecular sieve diffusion performance is limited, and the multi-level pores cannot be effectively improved. The problem of high production cost of molecular sieve, to achieve the effect of good heat and mass transfer ability, excellent catalytic performance, simple and feasible method

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

Most of the above-mentioned secondary templates are difficult to obtain. Before synthesizing the hierarchical pore molecular sieve, it is necessary to invest more manpower and material resources to synthesize the secondary template, which makes the production cost of the direct synthesis method to prepare the hierarchical pore molecular sieve higher.
On the other hand, the pore structure of the product obtained by the above synthesis method is mostly a combination of mesopores and micropores, which has limited improvement on the diffusion performance of molecular sieves, especially in the liquid phase reaction system, where the mesopores and micropores are combined. The structure is still unable to effectively improve the diffusion efficiency of guest molecules in the molecular sieve channels

Method used

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  • TS-1 molecular sieve with macroporous-microporous composite pore channel structure as well as preparation method and application of TS-1 molecular sieve
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  • TS-1 molecular sieve with macroporous-microporous composite pore channel structure as well as preparation method and application of TS-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Example 1 Preparation of Amorphous Mesoporous Titanium Oxide / Silicon Ball MTS-I~MTS-Ⅴ

[0055] Preparation of sample MTS-I:

[0056] Under the condition of stirring at 50°C, dissolve 0.20 g of cetyltrimethylammonium bromide (structure directing agent I) in 60 mL of deionized water and ethanol solution, then add ammonia water to the solution to adjust the pH value of the solution, and stir Then add 1.0 g of ethyl orthosilicate, 0.05 g of tetrabutyl titanate after 30 min, and continue stirring for 2 h. After the product was filtered, washed, washed with water, and dried, the structure directing agent I was removed by calcination, wherein the calcination temperature was 550° C., and the calcination time was 6 hours to obtain a white powder. That is, amorphous titania / silica spheres, labeled MTS-I.

[0057] Preparation of samples MTS-II, MTS-III, MTS-IV, MTS-Ⅴ:

[0058] According to the conditions listed in Table 1 below, samples MTS-II and MTS-III were prepared respecti...

Embodiment 2

[0064] Embodiment 2: the preparation of sample HTS-1~HTS-8

[0065] First, the structure directing agent II was added into deionized water, stirred and dissolved to obtain a mixed solution. A certain amount of the above solution was taken to impregnate the amorphous titanium dioxide / silicon spheres prepared in Example 1, and dried at room temperature for a period of time to obtain a solid mixture. The above solid mixture was transferred to the upper plate of the stainless steel autoclave, and water was added to the bottom of the autoclave. Seal the stainless steel reaction kettle, put it in an oven, and crystallize at 100-200°C for 12-100h. Cool rapidly after the reaction, separate the solid product, wash with deionized water, dry at 110°C in air atmosphere and calcined at 550°C for 6 hours to obtain nano TS-1 molecular sieve. Samples are labeled HTS-1 to HTS-8. Table 2 shows the raw material types and proportions, crystallization temperature and crystallization time of the...

Embodiment 3

[0071] Embodiment 3: 1-hexene epoxidation reaction evaluation

[0072] In the experiment, the TS-1 sample was synthesized by the traditional hydrothermal method, and the ratio of the synthetic gel was 1SiO 2 :0.25TPAOH:0.02TiO 2 :35H 2 O. Concrete gel preparation steps: first, add tetrapropylammonium hydroxide (TPAOH) to deionized water at room temperature and stir; after it is fully dissolved, slowly add a certain amount of ethyl orthosilicate and butyl titanate; After continuing to stir at room temperature for 24h, the raw material was transferred to a stainless steel synthesis kettle and crystallized at 150°C for 24h. The resulting solid product was centrifuged, washed, dried overnight at 110°C, and finally calcined at 550°C for 6 hours to remove the organic template, which was named conv-TS-1.

[0073] The prepared conv-TS-1 and the nano-TS-1 molecular sieve prepared in Example 2 were evaluated for the epoxidation reaction of 1-hexene. The specific steps of reaction e...

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Abstract

The invention discloses a TS-1 molecular sieve with a macroporous-microporous composite pore channel structure. According to the invention, macropores and micropores are embedded in the TS-1 molecular sieve, and the pore diameters of the macropores are in a range of 50-500 nm. The TS-1 molecular sieve obtained by the method has the same excellent stability as a single crystal and an interpenetrating macroporous-microporous composite pore channel structure, the titanium content of the produced TS-1 molecular sieve can be controlled and adjusted in a wide range, the TS-1 molecular sieve shows excellent catalytic performance in an olefin epoxidation reaction, and the defect of a single microporous system is relieved.

Description

technical field [0001] The application relates to a TS-1 molecular sieve with macropore-micropore composite channel structure, its preparation method and application, and belongs to the technical field of catalyst synthesis. Background technique [0002] 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. At the same time, TS-1 molecular sieve also has high hydrothermal stability and certain hydrophobicity, which makes it perform well in the catalytic system in the presence of water-soluble oxidants. It has the characteristics of high activity, high selectivity and easy separation of the catalyst. The development and application of TS-1 molecular sieve has extended the application of molecular...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00B01J29/89B01J37/08B01J35/10C07D301/12C07D303/04
CPCC01B37/005B01J29/89B01J37/088B01J37/082C07D301/12C07D303/04C01P2006/16B01J35/60
Inventor 张晓敏许磊李沛东赵晓炜
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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