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A kind of preparation method of the MWW type molecular sieve of a kind of cavity structure

A technology of molecular sieve and cavity, which is applied in the field of preparation of MWW type molecular sieves, can solve the problems of hollow spheres being easily broken, the amount of hard template used, and the particle size of hollow spheres, etc., and achieve the effect of uniform particles, less dosage and less emissions

Active Publication Date: 2017-07-28
SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with polystyrene microsphere templates, the carbon black templates used are widely sourced and cost-effective. However, due to the inhomogeneity and particle size of carbon black particles generally above 20 microns, the resulting hollow spheres have a larger particle size and correspondingly thinner pore walls. Therefore, the hollow spheres easily broken
The amount of hard formwork is relatively large, and it is difficult to burn out. At the same time, the burning of the formwork will bring a lot of environmental pollutants
[0005] CN201110353565.4 discloses a hollow spherical IM-5 molecular sieve and its preparation method. The method uses cetyltrimethylammonium bromide (CTAB) as a micelle template to prepare the IM-5 hollow sphere structure. The CTAB used is Cationic surfactants are expensive and used in large amounts

Method used

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  • A kind of preparation method of the MWW type molecular sieve of a kind of cavity structure
  • A kind of preparation method of the MWW type molecular sieve of a kind of cavity structure
  • A kind of preparation method of the MWW type molecular sieve of a kind of cavity structure

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Experimental program
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Effect test

Embodiment 1

[0037] Under mechanical stirring and ultrasonic conditions, dissolve sodium hydroxide into water, and then add sodium aluminate, cycloheximide, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =30,OH - / SiO 2 =0.10, cycloheximide / SiO 2 =0.8,H 2 O / SiO 2 =40. First, the above mixture is ultrasonically (1KW / L) at room temperature of 25°C and the material is stirred for 40 minutes to make the material evenly mixed, and then aged for 3 hours under the same stirring and ultrasonic conditions, and the aged mixture is put into the reaction kettle at Crystallization at 160°C for 82 hours. Then the temperature was lowered to 130°C at a rate of 0.1°C / min, and after 1.5 hours of constant temperature, the water vapor was slowly released through the pressure reducing valve, and the final H 2 O / SiO 2 The molar ratio was 15. Afterwards, the constant temperature was continued for 2 hours. The final product obtained was washed with distilled water unti...

Embodiment 2

[0039] Under mechanical stirring and ultrasonic conditions, dissolve sodium hydroxide into water, and then add sodium aluminate, cycloheximide, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =25,OH - / SiO 2 =0.12, cycloheximide / SiO 2 =0.60,H 2 O / SiO 2=40. First, the above mixture is ultrasonically (1KW / L) at room temperature of 25°C and the material is stirred for 40 minutes to make the material evenly mixed, and then aged for 3 hours under the same stirring and ultrasonic conditions, and the aged mixture is put into the reaction kettle at Crystallize at 170°C for 48 hours, then lower the temperature to 120°C at a rate of 0.1°C / min, keep the temperature for 2 hours, release water vapor slowly through the pressure reducing valve, and the final H 2 O / SiO 2 The molar ratio is 10. The temperature was then continued for 3 hours. The final product obtained was washed with distilled water until neutral, dried at 120°C for 12 hours, and then...

Embodiment 3

[0041] Under mechanical stirring and ultrasonic conditions, dissolve sodium hydroxide into water, and then add sodium aluminate, cycloheximide, and silica sol in sequence. The final material ratio satisfies: Al 2 o 3 / SiO 2 =25,OH - / SiO 2 =0.12, cycloheximide / SiO 2 =0.35,H 2 O / SiO 2 =25. First, the above mixture is ultrasonically (1KW / L) at room temperature of 25°C and the material is stirred for 40 minutes to make the material evenly mixed, and then aged for 3 hours under the same stirring and ultrasonic conditions, and the aged mixture is put into the reaction kettle at Crystallize at 140°C for 36 hours, then lower the temperature to 105°C at a rate of 0.1°C / min, and after constant temperature for 3 hours, slowly release water vapor through the pressure reducing valve, and the final H 2 O / SiO 2 The molar ratio was 8, and then the temperature was continued for 2 hours. The final product obtained was washed with distilled water until neutral, dried at 120°C for 12 h...

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Abstract

The invention discloses a method for preparing a cavity-structured MWW molecular sieve. The method slowly releases the water vapor in the reaction system to highly concentrate the excess template agent in the molecular sieve synthesis to form a micellar structure, and the MWW molecular sieves are adsorbed and arranged along the micellar structure, finally forming a cavity-shaped MWW molecular sieve aggregate. The molecular sieve of the invention is simple to prepare, and the obtained structure is favorable for material mass transfer, does not use special organic matter, produces less discharge, and has little environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of molecular sieve synthesis, and in particular relates to a method for preparing a cavity-structured MWW type molecular sieve. Background technique [0002] The MWW type molecular sieves are widely used in industry as MCM-22 and MCM-49. MWW molecular sieve has two sets of independent pore systems of ten-membered ring and twelve-membered ring, high thermal stability, hydrothermal stability and suitable acidity, and has been well applied in the alkylation reaction of benzene and propylene. Molecular sieve materials have shapes such as rods, strips, blocks, or spheres. At present, the preparation of molecular sieves with hollow structures or their aggregates has aroused great interest. Because this special hollow structure often leads to some special properties of materials, especially in the fields of catalysis, adsorption, and controlled release of drugs. [0003] At present, molecular sieves in hollow for...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 杨卫亚凌凤香王少军沈智奇季洪海王丽华郭长友
Owner SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEMICALS CO LTD