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Preparation method and application of magnetic Ti-MWW molecular sieve microsphere catalyst

A technology of magnetic microspheres and molecular sieves, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as non-magnetic composite reaction processes, achieve low catalyst consumption, improve product quality, and save costs Effect

Active Publication Date: 2018-06-08
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 of preparing magnetic catalytic materials, but none of them involve the reaction process of the combination of magnetic composite Ti-MWW molecular sieve microsphere catalyst and magnetic stable bed for propylene epoxidation (HPPO)

Method used

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  • Preparation method and application of magnetic Ti-MWW molecular sieve microsphere catalyst

Examples

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Embodiment 1

[0030] This example illustrates the preparation method of composite magnetic Ti-MWW molecular sieve catalyst microspheres

[0031] (1) 500g superparamagnetic NiFe with a thickness of 0.5-2μm 2 o 4 The powder was ultrasonically dispersed into 5L of HCl solution with a concentration of 0.1mol / L for pretreatment, the magnetic particles were fully washed with deionized water, and then ultrasonically dispersed into 5kg of ethanol-water mixture (ethanol content: 77wt%). Then add 750ml of 25% ammonia solution, add 48ml of ethyl silicate (TEOS) during stirring, continue stirring at 50°C for 6h, separate the product with a magnet, and obtain amorphous SiO 2 Coated magnetic particles, denoted as NiFe 2 o 4 @SiO 2 .

[0032] (2) The magnetic NiFe in (1) 2 o 4 @SiO 2 Mix with silica sol (concentration 30wt%), Ti-MWW molecular sieve, and turnip powder to form a slurry with a solid content of 45wt%, and then prepare microspheres of 50-70 μm by spray drying and molding, and then bake...

Embodiment 2

[0034] This example illustrates the preparation method of composite magnetic Ti-MWW molecular sieve catalyst microspheres

[0035] (1) 500g of superparamagnetic 0.5-1.0μm Fe 3 o 4 Ultrasonic dispersion of powder into 3L of HNO with a concentration of 0.4mol / L 3 Pretreatment was carried out in the solution, the magnetic particles were fully washed with deionized water, and then ultrasonically dispersed into 3 kg of methanol-water mixture (methanol content: 32 wt%). Then add 600ml of 28% ammonia water, add 100ml of ethyl silicate (TEOS) during the stirring process, continue to stir at 60°C for 5h, separate the product with a magnet, and then dry it in vacuum at 60°C for 12h to obtain amorphous SiO 2 Coated magnetic particles, denoted as Fe 3 o 4 @SiO 2 .

[0036] (2) The magnetic Fe in (1) 3 o 4 @SiO 2 It is mixed with silica sol (concentration 30wt%), Ti-MWW molecular sieve and methyl cellulose to form a 35wt% slurry, and then prepared into 40-70μm microspheres by spra...

Embodiment 3

[0038] This example illustrates the preparation method of composite magnetic Ti-MWW molecular sieve catalyst microspheres

[0039] (1) 500g of superparamagnetic 0.5-2μm γ-Fe 2 o 3 Ultrasonic dispersion of the powder into 4L concentration of 0.25mol / L acetic acid solution for pretreatment, fully wash the magnetic particles with deionized water, and ultrasonically disperse it into 4kg isopropanol-water mixture (isopropanol content: 25wt% )middle. Then add 800ml of 20% ammonia water, add 139ml of methyl silicate (TMOS) during the stirring process, continue to stir at 45°C for 8h, separate the product with a magnet, and then vacuum dry at 50°C for 20h to obtain amorphous SiO 2 Coated magnetic particles, denoted as γ-Fe 2 o 3 @SiO 2 .

[0040] (2) The magnetic γ-Fe in (1) 2 o 3 @SiO 2 It is mixed with silica sol (concentration 30wt%), Ti-MWW molecular sieve and polymethacrylate to form a 40wt% slurry, and then prepared into 50-70μm microspheres by spray drying method, and ...

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Abstract

The invention discloses a preparation method and application of a magnetic Ti-MWW molecular sieve microsphere catalyst. The preparation method comprises the following steps: mixing a SiO2-coated inorganic magnetic particle material with silica sol, a Ti-MWW molecular sieve and deionized water into a slurry with the concentration of 25-50wt%, moulding through spray drying to obtain magnetic microspheres with the sizes of 30-100 microns, and then calcining at 450-650 DEG C for 2-12 hours to obtain the magnetic Ti-MWW molecular sieve microsphere catalyst, wherein the inorganic magnetic particle material is any one of Fe3O4, gamma-Fe2O3, NiFe2O4 and CuFe2O4 and accounts for 20-50wt% of the microsphere content. The magnetic catalyst particles can be suspended in a magnetically stabilized bed reactor and can catalyze an epoxidation reaction of propylene to produce propylene oxide, and a result shows that the product selectivity, the yield and the effective H2O2 utilization rate are very high.

Description

technical field [0001] The invention relates to a preparation method and application of a magnetic Ti-MWW molecular sieve microsphere catalyst, belonging to the field of synthesis of inorganic chemical materials. Background technique [0002] The magnetic Ti-MWW molecular sieve microsphere catalyst can simultaneously utilize the magnetic material suspended in the magnetically stable bed and the excellent oxidation catalytic properties of the Ti-MWW molecular sieve to 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 struct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/76B01J35/08C07D301/12C07D303/04
CPCC07D301/12C07D303/04B01J29/7676B01J2229/186B01J35/33B01J35/51Y02P20/52
Inventor 王志光李进
Owner CHINA CATALYST HLDG CO LTD
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