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

A TS-1, flake technology, applied in the field of flake TS-1 molecular sieve, can solve the problems of cumbersome steps, high production cost, complicated process and the like of flake MFI molecular sieve, and achieves simple and feasible preparation method, low cost and synthetic cost. low effect

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1 Preparation of amorphous titanium dioxide / silicon

[0052] At 50 ° C agitation conditions, 0.20 g of hexadalkyltrimethyla bromide (structural guide) was dissolved in 60 ml of deionized water and ethanol solution, and then the pH of the ammonia water regulated solution was added to the solution. 1.0 g of orthosilicate and 0.05 g of tetrabutyl titanate were added, and stirring was continued for 2 h. The product was filtered, washed, washed, and then dried, and the structural guiding agent was removed by calcitating 6 hours at 550 ° C to give a white powder, labeled a sample I. SEM results show that the obtained product is 50-200 nm spherical material, the particle size is uniform, and the dispersibility is good. According to Table 1 Adjust the pH of the combined process and the addition of the added amount of orthosilicate and butyl butyl butyl addition, the resulting product can be changed, the resulting sample number and performance parameters are shown in Table...

Embodiment 2

[0055] Example 2: Preparation of Samples TS-1-1 ~ TS-1-6

[0056] First, the urea, inorganic alkali source and organic amine are added to deionized water, stirred, and dissolved, resulting in a mixed solution. The amorphous titanium dioxide / silicon complex prepared by the above solution or the like was extracted, and the solid was obtained for a period of time. The above solid mixture was transferred to the upper plate of the upper portion of the stainless steel high pressure reactor, and the reaction could be added to the bottom of the reaction. The stainless steel reactor was sealed, placed in an oven, and 12 to 40 h at 130 to 180 ° C. After the reaction, the solid product was separated, and the solid product was separated, and the deionized water was washed, dried at 110 ° C in the air atmosphere and 550 ° C for 6 hours, i.e., the sheet TS-1 molecular sieve. The correspondence between the sample number and the preparation conditions are shown in Table 2.

[0057] XRD characte...

Embodiment 3

[0062] Example 3: 1-hexene ring oxidation reaction evaluation

[0063] Experiments use traditional hydrothermal synthesis TS-1 samples, synthetic gel ratio of 1SIO 2 : 0.25TPAOH: 0.02TIO 2 : 35h 2 O. Specific gel formulation step: First, tetrapropyl hydroxide (TPAOH) is added to deionized water at room temperature; a certain amount of orthosilicate and butyl butyl ester is slowly added after sufficient dissolution; After stirring at room temperature for 24 h, the raw material was transferred to a stainless steel synthetic kettle and crystallized at 150 ° C for 24 h. The resulting solid product was centrifuged, then washed, then dried overnight at 110 ° C, and finally the organic template agent was removed at 550 ° C for 6 h, named CONV-TS-1.

[0064] The prepared CONV-TS-1 was evaluated by epoxidation reaction of 1-hexene by a sheet TS-1 molecular sieve prepared in Example 2. The specific steps of the reaction are as follows: Weigh 0.05 g of sample, 1.0 g 1-hexene, 0.375GH 2 O 2 A...

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Abstract

The invention discloses a lamellar TS-1 molecular sieve. The lamellar TS-1 molecular sieve has an MFI topological structure, the axis b of the lamellar TS-1 molecular sieve is shorter than the axis a and the axis c of the lamellar TS-1 molecular sieve, and the thickness of the lamellar TS-1 molecular sieve is 50-500 nm. The invention also provides a preparation method and application of the lamellar TS-1 molecular sieve. The lamellar TS-1 molecular sieve is relatively small in size in the b-axis direction, so diffusion of guest molecules is facilitated, and the lamellar TS-1 molecular sieve has excellent catalytic performance. The straight pore channel direction (b-axis) of the TS-1 molecular sieve is a main molecular diffusion path, so the diffusion efficiency of the product is improved due to the thinner b-axis thickness.

Description

Technical field [0001] The present application relates to a sheet-like TS-1 molecular sieve, which is prepared and applied to chemical chemical. Background technique [0002] In many kinds of multi-kind materials, zeolite molecules are sieved in which they have developed, orderly aperture structure, which can be adjusted, as catalysts, catalyst carriers, and adsorption separation materials in petrochemical, fine Chemicals and coal chemicals have an extremely wide range of applications (Chem.Rev., 1997, 97, 2373-2419; Chem.Eng., 2011, 118, 16-20). [0003] In 1983, the Italian Scientist Taramasso et al [US Patent, 4410501, 1983, 10, 18] were reported for the first time of Titanium Silicalite-1 (TS-1) titanium silicon molecular sieve for MFI topologies. TS-1 molecular skeleton structure has a unique catalytic oxidation function in the skeleton structure, and the TS-1 molecular sieve also has high water thermal stability and a certain hydrophobicity to perform it in a catalytic syst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B39/04B01J29/89C07D301/12C07D303/04
CPCC01B39/085C01B39/04B01J29/89C07D301/12C07D303/04C01P2004/22C01P2004/03C01P2002/72B01J2229/36B01J2229/38
Inventor 许磊张晓敏袁扬扬李沛东
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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