Apple-shaped hollow molecular sieve microspheres and preparation method and application thereof

A molecular sieve and hollow technology, applied in the field of molecular sieves, can solve the problems such as difficulty in exerting the advantages of spatial confinement effect and channel folding, catalyst particles unable to form a hollow structure, and limited application.

Active Publication Date: 2018-08-17
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalyst particles prepared by this method cannot form an obvious hollow structure, and it is difficult to tak...

Method used

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  • Apple-shaped hollow molecular sieve microspheres and preparation method and application thereof
  • Apple-shaped hollow molecular sieve microspheres and preparation method and application thereof

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[0030] The invention provides a method for preparing apple-shaped hollow molecular sieve microspheres, comprising the following steps:

[0031] (1) Homogenizing molecular sieves, binders, pore-forming agents and water to obtain colloidal slurry;

[0032] (2) mixing and emulsifying the colloid slurry obtained in the step (1) with a surfactant to obtain a microsphere emulsion;

[0033] (3) The microsphere emulsion obtained in the step (2) is subjected to balling treatment by spray drying method to obtain primary microspheres;

[0034] (4) Calcining the primary microspheres obtained in the step (3) to obtain apple-shaped hollow molecular sieve microspheres.

[0035] The invention homogenizes molecular sieve, binder, pore-forming agent and water to obtain colloid slurry. In the present invention, the solid content of the colloidal slurry is preferably 20-45%, more preferably 30-45%, more preferably 42-43%; the solid content of the colloidal slurry refers to the dried colloidal s...

Embodiment 1

[0063] (1) Take 5.5kg of HZSM-5 molecular sieve with a grain size of 300-350nm, 3kg of kaolin, 1kg of cement and 0.5kg of ammonium carbonate into 20kg of deionized water, and use a homogeneous emulsifier to perform shear emulsification at 2000rpm for 2 hours to form Uniform colloidal slurry, the solid content of the colloidal slurry is 31.7%.

[0064] (2) Add 300 g of P123 surfactant to the colloid slurry, and continue stirring for 1 hour to obtain a microsphere slurry.

[0065] (3) Transport the above-mentioned microsphere slurry to the spray dryer, the atomization pressure of the spray dryer is 2.8Mpa, the inlet temperature of the atomization dryer is 280°C, and the outlet temperature is 120°C. The outlet flows out to obtain primary microsphere particles.

[0066] (4) The spray-dried microspheres were heated to 600° C. in a muffle furnace at a rate of 2° C. / min, and then calcined for 4 hours to obtain apple-shaped hollow molecular sieve microspheres.

[0067] Scanning elec...

Embodiment 2

[0070] (1) Take 4.5kg of SAPO-34 molecular sieve with a grain size of 400-500nm, 4kg of attapulgite powder, 1kg of kaolin, 0.3kg of urea and 0.2kg of ammonium nitrate into 15kg of deionized water, and use a homogeneous emulsifier to shear at 2000rpm Cut and emulsify for 2 hours to form a uniform colloidal slurry with a solid content of 38.0%.

[0071] (2) Add 600 g of cetyltrimethylammonium bromide surfactant to the colloid slurry and continue stirring for 1 hour to obtain a microsphere slurry.

[0072] (3) Transport the above-mentioned microsphere slurry to a spray dryer, the atomization pressure of the spray dryer is 2.5Mpa, the inlet temperature of the atomization dryer is 300°C, and the outlet temperature is 130°C, and the spray dryer is sprayed for 2 to 5 seconds. The outlet flows out to obtain primary microsphere particles.

[0073] (4) The spray-dried microspheres were heated to 580° C. in a muffle furnace at a rate of 2° C. / min, and then calcined for 5 hours to obtain...

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Abstract

The invention provides apple-shaped hollow molecular sieve microspheres and a preparation method and application thereof. The preparation method includes: homogenizing a molecular sieve, a binder, a pore forming agent and water, and mixing colloidal grout with a surfactant for emulsifying to form a spherical emulsion under action of surface tension of the surfactant, wherein at the moment of sprayforming, the pore forming agent pyrolyzes at a point inside the spherical emulsion in a centralized manner to form a cavity from the surface to the inside of the microsphere emulsion, and in the process of spray forming, the cavity contracts to a certain degree to form macropores on the surface to be communicated with a hollow structure inside; combining with the subsequent calcining process to obtain large-grained hollow molecular sieve microspheres. Results of embodiments show that by the preparation method, hollow microspheres with macropores in the surface can be prepared, particle size distribution is 50-300um; hollow structure diameter reaches 10-150um, a macropore of 5-30um is formed in the surface of each molecular sieve microsphere, thickness of a shell layer reaches 10-80um, andthe shell layer is provided with mesopores of 70-200nm.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to an apple-shaped hollow molecular sieve microsphere and its preparation method and application. Background technique [0002] The hollow core-shell structure has a shell and a large inner core space. Because of the confinement effect of the inner space, it has been widely used in capsule catalysts, confined space catalysts, bioreactors and other functional materials. Hollow molecular sieve microsphere is a special inorganic hollow material, which has good thermal and chemical stability, and has better mass and heat transfer characteristics, combined with its unique space confinement effect and channel foldability It has broad application prospects in chemical reactions. [0003] At present, the synthesis methods of hollow molecular sieve microspheres mainly include in-situ synthesis method and post-forming method. Among them, the in-situ forming method is a ...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J29/85B01J35/08B01J35/10B01J29/89C07C1/20C07C11/04C07C11/06C07C11/08C07C11/02C07C37/60C07C39/04C07C39/08C07C249/04C07C251/44C07C15/00B01J13/02
CPCB01J13/02B01J29/005B01J29/18B01J29/40B01J29/85B01J29/89B01J35/023B01J35/08B01J35/1066B01J35/1076B01J2229/12C07C1/20C07C37/60C07C249/04C07C11/04C07C11/06C07C11/08C07C11/02C07C39/04C07C39/08C07C251/44C07C15/00Y02P20/52Y02P30/20Y02P30/40
Inventor 樊卫斌吴志伟董梅焦卫勇李俊汾王建国
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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