Large blocked TS-1 molecular sieve with high catalytic activity and synthetic method thereof

Abstract

The invention relates to a large blocked TS-1 molecular sieve with high catalytic activity and a synthetic method thereof, belonging to the technical fields of catalytic chemistry and chemical engineering. The large blocked TS-1 molecular sieve is a titanium-silicalite molecular sieve which has an MFI structure and formed by mutually piling nano-level TS-1 crystal grains with the blocked size of 20-100 micrometers and the mesoporous volume of 0.55cm<3>/g. The large blocked TS-1 molecular sieve is formed by evenly mixing tetraethoxysilane as a silicon source, tetrabutyl titanate as a titanium source, tetrapropylammonium hydroxide as a template agent, water and isopropanol as a solvent and H2O2 as an inorganic additive and carrying out hydrothermal crystallization on the mixture at a temperature between 160 DEG C and 180 DEG C for 6-96 hours. The large blocked TS-1 molecular sieve maintains a single crystal grain nano-size structure, has favorable catalytic reaction activity and can realize the separation on the entire device by filtering operation; and the adopted inorganic addictive H2O2 is friendly to the environment and has low price, thus the invention has important significance in the practical chemical engineering production.

Description

technical field [0001] The invention belongs to the technical fields of inorganic chemistry, physical chemistry, material chemistry, catalytic chemistry and chemical engineering, and in particular relates to a multi-stage hole large block TS-1 molecular sieve with high catalytic activity and its preparation and characterization. Background technique [0002] As an important part of inorganic microporous crystal materials, molecular sieves have a hollow structure and large surface area, so they are widely used in many fields, such as ion exchange, adsorption and separation, host-guest chemistry, etc. In the catalytic industry, molecular sieves are also very important. An important class of catalysts and catalyst supports. In 1983, Italian Enichem Company developed an environmentally friendly microporous TS-1 molecular sieve with MFI structure, see Taramasso, M.; Perego, G.; Notari, B.US Patent No.4410501, 1983, this molecular sieve In a series of oxidation reactions, it exhi...

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Problems solved by technology

[0003] The grain size of the traditional TS-1 molecular sieve is about 200 to 300nm. The smaller particle size makes the separation of TS-1 in the liquid phase very difficult, and high-speed centrifugation is often required to separate it.

Difficulties in separation will reduce the yield of TS-1 molecular sieve and cause unnecessary loss of catalyst during use. In order to solve this problem, people try to synthesize micron-sized TS-1, among which A.J.H.P.Van der Pol, A.J.Verduyn, J.H.C. van Hooff, Appl.Catal.A: General 92 (1992) 113, discloses that the size of the prepared TS-1 molecular sieve is 5-10 μm, although the larger size TS-1 molecular sieve can realize suction filtration separation, but in some catalytic The reactivity in the reaction will be greatly reduced, such as phenol hydroxylation reaction, almost no catalytic activity

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