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Multi-level-pore composite material supported with TS-1 zeolite film and preparation method of composite material

A composite material, TS-1 technology, applied in the direction of chemical instruments and methods, crystalline aluminosilicate zeolite, ceramic products, etc., can solve problems such as the limitation of application range, achieve easy adjustment and control, simple and easy repeatability, and reduce side effects Effects of reaction and carbon deposition

Inactive Publication Date: 2018-10-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the zeolite obtained by this method is a powder, and its application range is greatly limited compared with the monolithic molding material.

Method used

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  • Multi-level-pore composite material supported with TS-1 zeolite film and preparation method of composite material
  • Multi-level-pore composite material supported with TS-1 zeolite film and preparation method of composite material
  • Multi-level-pore composite material supported with TS-1 zeolite film and preparation method of composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] This embodiment is a micron-scale through-hole α-Al 2 o 3 Preparation of monolithic material A1.

[0047] 0.09g polyethylene oxide, 4.32g AlCl 3 ·6H 2 O was dissolved in 4 mL of water and 4.35 g of absolute ethanol in a mixed solvent, and stirred until it was uniformly dissolved to form a colorless and transparent homogeneous solution. Add 3.11 g of propylene oxide under stirring and ice-bath conditions, and after vigorously stirring for 5 minutes, transfer the resulting mixture sol into a polytetrafluoroethylene test tube or a glass tube. The tube was sealed, aged at 40°C for 24 hours, and the wet gel was dried and calcined to obtain micron-sized through-hole α-Al 2 o 3 Overall material A1.

Embodiment 2

[0052] Dissolve 0.25g of potassium hydroxide in 20g of water, add 2.52g of tetrapropylammonium bromide and stir to mix evenly. Slowly add 1.67 g of tetraethyl orthosilicate into the system under vigorous stirring, and after mixing uniformly, continue hydrolysis for 16 hours under magnetic stirring. Add 0.08 g of tetrabutyl titanate and 0.2 g of hydrogen peroxide into 8 g of water, stir for 4 hours, then slowly drop them into the silicon source hydrolysis solution system, and stir for 1 hour after the dropwise addition is complete. The temperature of the system was raised to 80°C, and the alcohol was fully removed by heating for 5 hours. Water was added to replenish the lost mass, and the system was cooled to room temperature to obtain a crystallization solution. Under ultrasonic or negative pressure, the micron-scale through-hole α-Al 2 o 3 The carrier was immersed in the crystallization solution for 30min. Then, the carrier and the crystallization solution were placed in a...

Embodiment 3

[0054] Dissolve 0.18g of sodium hydroxide in 22.34g of water, add 1.95g of TPAOH and stir to mix evenly. Slowly add 1.67 g of tetraethyl orthosilicate into the system under vigorous stirring, and after mixing uniformly, continue hydrolysis for 24 hours under magnetic stirring. Add 0.07g of tetrabutyl titanate and 0.2g of hydrogen peroxide into 5g of water, stir for 2 hours, then slowly drop into the silicon source hydrolysis solution system, and stir for no less than 30 minutes after the dropwise addition. The temperature of the system was raised to 85°C, and the alcohol was fully removed by heating for 3 hours, and the lost mass was replenished by adding water, and the system was lowered to room temperature to obtain a crystallization solution. Under ultrasonic or negative pressure, the micron-scale through-hole α-Al 2 o 3 The carrier was immersed in the crystallization solution for 30min. Then the carrier and the crystallization solution were placed in a closed stainless ...

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Abstract

The invention provides a multi-level-pore composite material supported with a TS-1 zeolite film. The composite material comprises an alpha-Al2O3 carrier and the TS-1 zeolite film, the composite material is an integral forming material having macropores of 0.20-2 [mu]m, mesopores of 2-10 nm and micropores of 0.5-2 nm, and based on a total weight of the composite material, a content of the TS-1 zeolite is 4-15 wt%. The multi-level-pore composite material provided by the invention is prepared by adopting an in-situ crystallization method, and the prepared multi-level-pore composite material supported with the TS-1 zeolite film has the relatively-uniform TS-1 zeolite film and a transparent micron-sized macroporous structure, and overcomes limitation of zeolite micropores on material mass transfer in a catalytic reaction, thereby having very important significance for a macromolecular catalytic reaction.

Description

technical field [0001] The invention relates to a multi-level hole composite material loaded with TS-1 zeolite membrane and a preparation method thereof. Background technique [0002] Zeolite molecular sieve refers to a kind of natural and synthetic hydrated silicate, which has the structure and characteristics of crystal, the surface is a solid skeleton, and the internal micropores can play the role of adsorbing molecules. Zeolite molecular sieves have regular and orderly pore sizes, large pore volume and specific surface area, and good hydrothermal stability. They are widely used in the fields of gas adsorption and separation, ion exchange, fossil raw material processing and refining, and environmental protection, and their role is increasing day by day. . [0003] In 1983, US Patent No. USP4410501 first reported the introduction of transition metal titanium into the framework of pure silicon molecular sieves to synthesize TS-1 molecular sieves. Due to this type of molec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J35/10C01B39/08C04B35/10C04B38/00C04B35/624
CPCC01B39/085C04B35/10C04B35/624C04B38/0045B01J29/89C01P2004/03C01P2002/72B01J35/64C04B38/0054
Inventor 赵天波宗保宁杜泽学曾建立孙明亮王佳
Owner CHINA PETROLEUM & CHEM CORP
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