Preparation method of TS-1 molecular sieve microspherical catalyst with magnetism and application

A TS-1, magnetic microsphere technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as no reaction process involved, save the cost of product purification, convenient operation, secondary less reactive effect

Active Publication Date: 2018-06-22
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The above-mentioned documents mainly disclose the method for preparing magnetic catalytic materials, but none of them involve the rea

Method used

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  • Preparation method of TS-1 molecular sieve microspherical catalyst with magnetism and application

Examples

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Effect test

Embodiment 1

[0028] This example illustrates the preparation method of composite magnetic TS-1 molecular sieve catalyst microspheres

[0029] (1) 500g of superparamagnetic 0.5-1.0μm Fe 3 o4 Ultrasonic dispersion of powder into 5L of HNO with a concentration of 0.2mol / L 3 Pretreatment was carried out in the solution, the magnetic particles were fully washed with deionized water, and then ultrasonically dispersed into 5 kg of ethanol-water mixture (ethanol content: 32 wt%). Then add 750ml of 25% ammonia solution, add 50ml of ethyl silicate (TEOS) during stirring, continue to stir at 50°C for 6h, separate the product with a magnet, and then dry it in vacuum at 55°C for 16h to obtain amorphous SiO 2 Coated magnetic particles, denoted as Fe 3 o 4 @SiO 2 .

[0030] (2) The magnetic particle Fe in (1) 3 o 4 @SiO 2 It is mixed with silica sol (concentration 30wt%), TS-1 molecular sieve, and methylcellulose to form a 30wt% slurry, and then prepared into 30-60μm microspheres by spray-drying ...

Embodiment 2

[0032] This example illustrates the preparation method of composite magnetic TS-1 molecular sieve catalyst microspheres

[0033] (1) 500g of superparamagnetic 0.5-2μm γ-Fe 2 o 3 The powder is ultrasonically dispersed into 3L of 0.4mol / L acetic acid solution for pretreatment, fully washes the magnetic particles with deionized water, and then ultrasonically disperses it into a 3kg isopropanol-water mixture (isopropanol content: 25wt%) )middle. Then add 600ml of 28% ammonia water, add 57ml of methyl silicate (TMOS) during the stirring process, continue to stir at 60°C for 5h, separate the product with a magnet, and then vacuum dry at 60°C for 12h to obtain amorphous SiO 2 Coated magnetic particles, denoted as γ-Fe 2 o 3 @SiO 2 .

[0034] (2) The magnetic particle γ-Fe in (1) 2 o 3 @SiO 2 It is mixed with silica sol (concentration 30wt%), TS-1 molecular sieve, and polymethacrylate to form a 35wt% slurry, and then prepared into 30-60μm microspheres by spray-drying molding ...

Embodiment 3

[0036] This example illustrates the preparation method of composite magnetic TS-1 molecular sieve catalyst microspheres

[0037] (1) 500g superparamagnetic 0.5-2μm CuFe 2 o 4 The powder was ultrasonically dispersed into 4L of citric acid solution with a concentration of 0.25mol / L for pretreatment, the magnetic particles were fully washed with deionized water, and then ultrasonically dispersed into 4kg of ethanol-water mixture (ethanol content: 81wt%). Then add 800ml of 20% ammonia water, add 118ml of propyl silicate (TPOS) during the stirring process, keep stirring at 45°C for 8h, separate the product with a magnet, and then dry it in vacuum at 50°C for 20h to obtain amorphous SiO 2 Coated magnetic particles, denoted as CuFe 2 o 4 @SiO 2 .

[0038] (2) The magnetic particles CuFe in (1) 2 o 4 @SiO 2 It is mixed with silica sol (concentration: 30wt%), TS-1 molecular sieve, and turnip powder to form a 40wt% slurry, and then prepared into 40-70μm microspheres by spray-dry...

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Abstract

The invention discloses a preparation method of a magnetic composite TS-1 molecular sieve catalyst and application. The method comprises the following steps: mixing a SiO2 coated inorganic magnetic particle material with silica sol, a TS-1 molecular sieve and deionized water into 25 to 50wt percent slurry, and performing spray drying molding, so as to obtain a 30 to 100 micrometer magnetic microsphere, and then calcining for 2 to 12h at 450 to 650 DEG C, so as to obtain the magnetic TS-1 molecular sieve catalyst. The inorganic magnetic particle material adopts any of Fe3O4, gama-Fe2O3, NiFe2O4and CuFe2O4; the content of the inorganic magnetic particle material is 20 to 50wt percent of that of the microsphere; the content of the amorphous SiO2 is 5 to 30wt percent of that of the microsphere. The magnetic catalyst microsphere can suspend in a magnetically stabilized bed reactor, and catalyze propylene epoxidation reaction to produce propylene epoxide, and results show that the magneticcatalyst microsphere has good product selectivity, yield and effective utilization of H2O2.

Description

technical field [0001] The invention relates to a preparation method and application of a magnetic TS-1 molecular sieve microsphere catalyst, belonging to the field of synthesis of inorganic chemical materials. Background technique [0002] The magnetic TS-1 molecular sieve microsphere catalyst can simultaneously utilize its magnetic suspension in a magnetically stable bed and the excellent oxidation catalytic performance of TS-1 molecular sieve, and become a valuable new composite catalytic material. Because it combines the magnetic responsiveness of inorganic magnetic materials and the characteristics of large surface area and easy functionalization of molecular sieve materials, combined with the magnetically stabilized bed process, it will have a wide application prospect in the field of chemical catalytic reactions. [0003] Patent CN101299366B discloses a method for preparing magnetic inorganic nanoparticles / zeolite microspheres with a core-shell structure. It is a kind...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D301/12C07D303/04
CPCB01J29/89B01J35/0033C07D301/12C07D303/04Y02P20/52
Inventor 王志光李进
Owner CHINA CATALYST HLDG CO LTD
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