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A monolithic honeycomb structure forming method for molecular sieve catalyst

A molecular sieve and catalyst technology, applied in the field of monolithic honeycomb structural molding of molecular sieve catalysts, can solve the problems of inability to solve active components, high temperature sensitivity index, molecular sieve catalyst falling off, etc., and achieve stable and efficient catalytic performance and temperature sensitivity index. High and maintain the effect of catalytic performance

Active Publication Date: 2017-12-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The monolithic molecular sieve catalyst prepared by the coating method, although the active components can be evenly distributed by certain techniques, can not solve the shortcomings of less active components, different thermal expansion coefficients between the carrier and the molecular sieve, which cause the molecular sieve to fall off, and the activity is easy to lose.
The in-situ generation method is to use the formed monolithic honeycomb structure to generate new molecular sieves on its surface through hydrothermal synthesis to prepare a honeycomb monolithic molecular sieve catalyst. Synthetic molecular sieves for N 2 Catalytic direct decomposition of O, the molecular sieve mass is 5% to 30% of the mass of the monolithic catalyst. This method also faces the problem of molecular sieve catalyst falling off after a period of use. At the same time, the preparation process of this method is complicated, which is not conducive to industrial production.
[0006] And patent CN103111322A has reported a kind of N 2 The preparation method of the monolithic honeycomb molecular sieve catalyst for O decomposition, the method is to directly form the active components, binders, extrusion aids, etc. through pressurization, and prepare the monolithic honeycomb molecular sieve catalyst, but this method is limited to the experiment chamber, the size of the preparation is small, and a complete process route has not been formed in the industry, the problem of engineering scale-up needs to be solved, and the application field is narrow
[0007] Molecular sieve is a porous material with a high temperature sensitivity index and is easy to crack during the drying process. Therefore, its molding preparation is a technical bottleneck, which directly affects the industrial application of molecular sieve catalysts.

Method used

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  • A monolithic honeycomb structure forming method for molecular sieve catalyst
  • A monolithic honeycomb structure forming method for molecular sieve catalyst
  • A monolithic honeycomb structure forming method for molecular sieve catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) Impregnation modification: 65kg copper nitrate (Cu(NO 3 ) 2 ·3H 2 0) crushed and dissolved in 1000kg of deionized water to prepare a copper ion impregnating solution, and pour the prepared impregnating solution into the reaction kettle. Turn on the stirring device of the reactor, and set the rotating speed to 80rpm. Then slowly add 800kg of microporous molecular sieve ZSM-5 carrier into the impregnation solution, and the speed of adding the molecular sieve should be gradually slowed down to ensure that the stirring paddle of the reactor can rotate smoothly. After the mixing was completed, the mixture was uniformly stirred for 24 hours while maintaining the temperature of the water bath in the reactor at 80°C.

[0042] (2) Drying: after stirring for 24 hours, turn off the stirring paddle. The output is packed in a stainless steel drying tray (1m×0.5m×0.1m), and the height of the material layer does not exceed 3cm. Put the wet material contained in the drying tra...

Embodiment 2

[0054] For the preparation of the powdered molecular sieve catalyst, the process steps are basically the same as the steps (1) to (4) in Example 1, mainly because the preparation of each material and the parameters of the control conditions are different. That is, the following steps are:

[0055] (5) Dry mixing: take 50kg of Cu-ZSM-5 molecular sieve, 17kg of SB powder, and 4kg of safflower powder, put them into a mixer and mix until uniform, the time is 20 minutes, and the temperature is controlled at 30°C.

[0056] (6) Kneading: Add 38kg of water and 7kg of nitric acid to the above-mentioned mixed materials at a rate of 5 kg / min. During the addition, keep the stirring device turned on. After the addition is complete, continue to stir and knead for 20 to 30 minutes. Control the temperature at 35°C, and the stirring speed is 60 rpm.

[0057] (7) Mud refining: Put the evenly stirred muddy billet into the mud mixer for repeated mixing and extrusion. The temperature of the mud m...

Embodiment 3

[0064] In embodiment 3, the concrete steps are basically the same as in embodiment 1, the difference is the selection of the mould, i.e. the extrusion molding process, the step (8) in embodiment 3 is as follows

[0065] (8) Extrusion molding: Put the refined mud into a high-pressure vacuum extruder for molding and extrusion. During extrusion, the temperature is controlled at 30°C, the extrusion rate is 20mm / s, the extrusion pressure is 15MPa, and the vacuum degree is 8KPa. The extrusion die is a square specification of 100mm×100mm, the channel structure is a regular quadrilateral, the aperture is 1.4mm, the wall thickness is 1.0mm, and the cutting length of the green body is 110mm, that is, the formed honeycomb molecular sieve catalyst wet-based green body is obtained, such as image 3 shown.

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Abstract

The invention provides a forming method of an integral cellular molecular sieve based catalyst. The forming method comprises the following steps: (1) impregnating a molecular sieve in a metal solution, and performing stirring, drying and high-temperature calcining to prepare a powdery molecular sieve based catalyst; (2) adding an adhesive, an extrusion aid, an acid solution and water, and mixing and kneading to obtain a wet material paste; (3) performing primary smelting, vacuum refining and high-pressure vacuum extrusion on the wet material paste to extrude to form a cellular integral wet-based blank body; (4) preparing the cellular integral molecular sieve based catalyst from the blank body by drying, cutting, polishing and calcining for 6-10 h at 500-550 DEG C. The forming method can precisely control key parameters in the drying process and limit the water loss rate of the blank body, and ensures that the blank body is high in strength and neat and orderly in shape. The forming method can be applied to industrial mass production, and adopts equipment in the prior art to reasonably arrange the process route so as to obtain qualified industrial application products.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a method for forming an integral honeycomb structure of a molecular sieve catalyst. Background technique [0002] Molecular sieves are widely used in many fields, such as microporous molecular sieves, as the main catalytic materials, adsorption separation materials and ion exchange materials, play an increasingly important role in petroleum processing, petrochemical, fine chemical, daily chemical and environmental protection fields. role. The application forms of molecular sieve catalysts are usually powder and granular, and granular catalysts can be divided into spherical, strip and clover, etc. These types of monolithic catalysts are widely used because of their simple preparation and mature industrial routes. [0003] With the intensification of environmental pollution, industrial waste gas is in urgent need of deep treatment, and molecular sieves have been used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J37/02B01J35/04B01J29/46
CPCB01J29/46B01J35/04B01J37/0201B01J2229/183
Inventor 张润铎史东军沙宇陈标华
Owner BEIJING UNIV OF CHEM TECH
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