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

A high catalytic activity, TS-1 technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. Catalytic activity, loss reduction, low cost effect

Inactive Publication Date: 2010-04-21
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: the synthesis of bulk TS-1 molecular sieve

[0021] The ratio of the reaction raw materials is as follows, SiO 2 :0.015~0.025TBOT:0.28TPAOH:40H 2 O: 0.33 Isopropanol: 1.3H 2 o 2 . First, mix TBOT with isopropanol evenly, then add TPAOH, H 2 O, mix evenly, then add TEOS while stirring vigorously, after adding TEOS, continue to stir until the solution is clear, replenish the water evaporated from the solution in time, and finally add H 2 o 2 , Stir evenly, add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallize at 180°C for 48-72 hours, and then take out the product and separate it by suction filtration.

[0022] figure 1 It is the XRD characterization result of the product. From the XRD point of view, the product has a typical MFI zeolite molecular sieve structure, and the sample has a high degree of crystallinity.

[0023] figure 2 , image 3 UV and IR spectra of the samples, respectively. From...

Embodiment 2

[0027] Example 2: Reduction of H 2 o 2 Addition amount, synthesis of block TS-1 molecular sieve

[0028] The ratio of the reaction raw materials is as follows, SiO 2 :0.015~0.025TBOT:0.28TPAOH:40H 2 O: 0.33 Isopropanol: 0.85H 2 o 2 . First, mix TBOT with isopropanol evenly, then add TPAOH, H 2 O, mix evenly, then add TEOS while stirring vigorously, after adding TEOS, continue to stir until the solution is clear, replenish the water evaporated from the solution in time, and finally add H 2 o 2 , Stir evenly, add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallize at 180°C for 48-72 hours, and then take out the product and separate it by suction filtration.

[0029] The product has no big difference compared with Example 1, except that the size of the bulk product is slightly smaller.

Embodiment 3

[0030] Example 3: Increase H 2 o 2 Addition amount, synthesis of block TS-1 molecular sieve

[0031] The ratio of the reaction raw materials is as follows, SiO 2:0.015-0.025TBOT:0.28TPAOH:40H 2 O: 0.33 Isopropanol: 2.0H 2 o 2 . First, mix TBOT with isopropanol evenly, then add TPAOH, H 2 O, mix evenly, then add TEOS while stirring vigorously, after adding TEOS, continue to stir until the solution is clear, replenish the water evaporated from the solution in time, and finally add H 2 o 2 , Stir evenly, add the reaction raw materials into a polytetrafluoroethylene stainless steel reaction kettle, crystallize at 180°C for 48-72 hours, and then take out the product and separate it by suction filtration.

[0032] The product has no big difference compared with Example 1, except that the size of the bulk product is slightly larger.

[0033] In Examples 1-3, if the crystallization time is shortened to 6 hours or increased to 96 hours, bulk TS-1 molecular sieves can also be o...

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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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89
Inventor 肖丰收单志超孟祥举王亮刘思宇马淑杰
Owner JILIN UNIV
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