TS-1 zeolite material with multi-level pores and preparation method of TS-1 zeolite material

A technology of TS-1 and zeolite materials, applied in chemical instruments and methods, molecular sieve compounds, inorganic chemistry, etc., can solve the problems of limited application range, shorten the diffusion distance, simplify the operation process, reduce side reactions and carbon deposition the effect produced

Active 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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  • TS-1 zeolite material with multi-level pores and preparation method of TS-1 zeolite material
  • TS-1 zeolite material with multi-level pores and preparation method of TS-1 zeolite material
  • TS-1 zeolite material with multi-level pores and preparation method of TS-1 zeolite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] This example is carrier preparation.

[0050] Under the condition of stirring, add 9.6g of acetic acid to 29g of tetrapropyl titanate under ice bath, after stirring for 30min, add the mixture of 0.86g of polyethylene oxide, 5.42g of hydrochloric acid, and 3.8g of water, and stir evenly. A clear homogeneous solution was formed. Add 10.42g ethyl orthosilicate, and continue stirring for no less than 3h. Then 4.44 g of N-methylformamide was added, and after vigorous stirring for 5 min, the resulting mixture sol was transferred to a polytetrafluoroethylene test tube or a glass tube. The tube was sealed, aged at 60°C for 24 hours, and the wet gel was dried and calcined to obtain micron-sized through-hole TiO 2 -SiO 2 Overall material A1.

Embodiment 2

[0052] This example is carrier preparation.

[0053] Dissolve 0.4g of polyethylene oxide in a mixture of 3g of hydrochloric acid and 2g of water, and add this solution to a solution containing 18g of tetrabutyl titanate and 5.6g of acetic acid under stirring conditions. After stirring evenly, the Transparent homogeneous solution. Add 6.3g ethyl orthosilicate and continue stirring for 4h. Then 2.5 g of N-methylformamide was added, and after vigorous stirring for 4 min, the resulting mixture sol was transferred to a polytetrafluoroethylene test tube or a glass tube. The tube was sealed, aged at 70°C for 24 hours, and the wet gel was dried and calcined to obtain micron-sized through-hole TiO 2 -SiO 2 Overall material A2.

Embodiment 3

[0063] Dissolve 0.08g of sodium hydroxide in 12g of water, add 6.9g of tetrapropylammonium hydroxide, stir and mix evenly to obtain a precursor solution. Under ultrasound and / or negative pressure, micron-sized through-hole TiO 2 -SiO 2 Carrier A1 was immersed in the precursor solution for 30 min. The impregnated carrier was filtered and taken out, and placed on a support in the autoclave, the precursor filtrate was poured into the bottom of the autoclave, and water was added to make the solution at the bottom of the autoclave reach 10 g. The reaction kettle was sealed, and hydrothermal reaction was carried out at 175° C. for 2 d. The carrier was taken out and washed with water, dried at 110° C. for 12 hours, and calcined in an air atmosphere of 550° C. for 6 hours to obtain the hierarchically porous TS-1 zeolite material A3.

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Abstract

The invention discloses a TS-1 zeolite material with multi-level pores. The TS-1 zeolite material comprises TS-1 zeolite and a TiO2-SiO2 carrier, and a weight ratio of the TS-1 zeolite to the TiO2-SiO2 carrier is 1:(4.8-9); the zeolite material is an integral forming material having macropores of 0.20-2 [mu]m, mesopores of 2-15 nm and micropores of 0.5-2 nm, a crystal lattice structure of the zeolite material is that a part of Ti<4+> enters a molecular sieve skeleton, a part of Ti<4+> is uniformly embedded in a SiO2 skeleton in a manner of an anatase crystal form, and SiO2 exhibits an amorphous state. The zeolitic material disclosed by the invention adopts a TiO2-SiO2 material as the carrier, a silicon source and a titanium source, under the vapor phase condition, the skeleton is partiallyconverted into the TS-1 zeolite, and a micron-sized through-hole skeleton structure of the carrier is maintained; and the prepared TS-1 zeolite has an uniform and stable structure and the multi-levelpores communicating with one another, thereby having very important significance for a macromolecular catalytic reaction.

Description

technical field [0001] The invention relates to a multi-level channel TS-1 zeolite material 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 size, large pore volume and specific surface area, and good hydrothermal stability. They are widely used in gas adsorption and separation, ion exchange, fossil raw material processing and refining, environmental protection and other fields, 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 molecular sieve for H 2 o 2 , has un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/00B01J29/03B01J35/10
CPCB01J29/03B01J35/1004B01J35/1057B01J35/1061B01J35/1071B01J35/1076B01J2229/60C01B37/005C01P2002/72C01P2004/03C01P2006/12C01P2006/16C01P2006/17
Inventor 李凤艳宗保宁杜泽学曾建立
Owner CHINA PETROLEUM & CHEM CORP
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