Dipping device for catalyst processing

Abstract

The invention discloses an impregnation device for catalyst processing, and relates to the field of catalyst preparation, the impregnation device comprises an impregnation container and a reflux pump, a reflux pipe is arranged in the impregnation container, a water inlet and a water outlet of the reflux pipe are both located in the impregnation container, and the reflux pipe forms reflux under the action of the reflux pump. The tail end of the backflow pipe at least comprises a flexible section, and a plurality of radial grooves are formed in the tail end of the flexible section. Compared with the prior art, the device has the beneficial effects that the device is simple in structure and convenient to use, a metal precursor solution can be fully mixed and contacted with a fixed powder carrier through backflow of the backflow pipe, and the position is continuously changed in the liquid flowing process based on a flexible material at the tail end of the backflow pipe, so that the metal precursor solution can be fully mixed and contacted with the fixed powder carrier. Therefore, the solid powder carrier can be fully and thoroughly impregnated, and a necessary guarantee is provided for preparing a high-performance catalyst.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of catalyst preparation, and particularly relates to an impregnation device for catalyst processing. BACKGROUND

[0002] In the field of catalyst preparation, the initial wet impregnation method is a common processing method, which needs to immerse the solid powder carrier in a metal precursor solution. For example, in the preparation process of a Ru-Co dual active site catalyst, the impregnation effect of the carbon black substrate and the Ru-Co monatomic precursor solution directly determines the active site distribution, dispersion uniformity and final catalytic performance of the catalyst, so the impregnation device is a key equipment to ensure the quality of catalyst preparation. At present, the commonly used impregnation device for catalyst processing in the industry mostly adopts a static soaking or fixed pipeline spraying mode to realize the contact between the metal precursor solution and the solid powder carrier. However, such devices have significant technical defects. On the one hand, the solid powder carrier is prone to agglomeration during static soaking, which makes it difficult for the metal precursor solution to penetrate into the agglomerates, resulting in local insufficient impregnation. On the other hand, the design of the fixed pipeline spraying or flow guide structure makes the solution flow path fixed, and the contact with the solid powder carrier is limited to a specific area, which cannot realize omnidirectional and dead angle-free mixing contact, thereby causing uneven loading of the metal precursor on the surface of the solid powder carrier, and the active site distribution is disorderly, which directly affects the modification effect and performance of the subsequent catalyst.

[0003] In addition, although some existing impregnation devices attempt to improve the mixing effect by adding a stirring mechanism, the stirring intensity is small and the impregnation effect is poor. If the stirring intensity is too large, the shear force generated during stirring can easily damage the structural integrity of the carbon black substrate. The design of the conventional reflux structure can only realize the recycling of the solution, and cannot strengthen the impregnation effect by changing the flow direction or contact position of the solution, resulting in insufficient impregnation completeness of the solid powder carrier and restricting the stable preparation of high-performance catalysts. SUMMARY

[0004] The present application aims to provide an impregnation device for catalyst processing to solve the problems raised in the background.

[0005] To achieve the above-mentioned purpose, the present application provides the following technical solutions. An impregnation device for catalyst processing, comprising an impregnation container and a reflux pump, a reflux pipe is arranged inside the impregnation container, the water inlet and the water outlet of the reflux pipe are both located inside the impregnation container, the reflux pipe forms a reflux under the action of the reflux pump, the end of the reflux pipe comprises at least one flexible section, and a plurality of radial grooves are formed at the end of the flexible section.

[0006] As a further scheme of the present application, a separation net is clamped inside the impregnation container, and the catalyst raw material is located above the separation net.

[0007] As a further scheme of the present application: the inside of the impregnation container is fixedly connected with a partition plate below, the reflux pump is located below the partition plate, a stirring shaft is arranged in the middle of the partition plate, the top of the stirring shaft is fixedly connected with stirring blades, and the lower end of the stirring shaft is in transmission connection with a driving motor.

[0008] As a further scheme of the present application: a reciprocating driving unit is arranged outside the stirring shaft, and the reflux pipe is connected with the reciprocating driving unit.

[0009] As a further scheme of the present application: the reciprocating driving unit comprises a cam fixedly connected outside the stirring shaft, a sliding rod is connected above the partition plate through a spring, the sliding rod abuts against the surface of the cam under the action of the spring, and the reflux pipe is connected with the sliding rod.

[0010] As a further scheme of the present application: a sealing cover is fixedly connected above the partition plate, and the sliding rod and the spring are located in the sealing cover.

[0011] As a further scheme of the present application: a snap ring is fixedly connected at the end of the sliding rod, and the reflux pipe is clamped in the snap ring.

[0012] As a further scheme of the present application: the reflux pump is a peristaltic pump, an electric heating pipe is fixedly connected at the bottom of the impregnation container, the reflux pipe is wound outside the electric heating pipe, and an electric heating plate is fixedly connected below the partition plate.

[0013] As a further scheme of the present application: a counterweight is connected with the water inlet of the reflux pipe.

[0014] Compared with the prior art, the present application has the beneficial effects that: the present application has simple structure and is convenient to use, the reflux of the reflux pipe enables the metal precursor solution to fully mix with the fixed powder carrier, the flexible material at the end of the reflux pipe continuously changes position during the flow of the liquid, thereby enabling the impregnation of the solid powder carrier to be sufficient and thorough, and providing necessary guarantee for the preparation of high-performance catalysts. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a structural schematic view of an impregnation device for catalyst processing.

[0016] Figure 2 It is a structural schematic view of another view of an impregnation device for catalyst processing.

[0017] Figure 3 It is a partial structural schematic view of the upper part of a partition plate in an impregnation device for catalyst processing.

[0018] Figure 4 It is a partial structural schematic view of the lower part of a partition plate in an impregnation device for catalyst processing.

[0019] Figure 5 For Figure 4 Another perspective structural diagram.

[0020] Figure 6 For a partial structure diagram of the internal part of a peristaltic pump in a catalyst processing impregnation device.

[0021] Figure 7 For a partial enlarged view of the end of the reflux pipe in a catalyst processing impregnation device.

[0022] Figure 8 For an elevation view of the position of the sealing cover in a catalyst processing impregnation device.

[0023] Figure 9 For a front view of the snap ring in a catalyst processing impregnation device.

[0024] In the figure: 1, impregnation container; 2, reflux pump; 3, reflux pipe; 4, radial groove; 5, screen; 6, partition; 7, stirring shaft; 8, stirring blade; 9, driving motor; 10, reciprocating driving unit; 11, cam; 12, spring; 13, sliding rod; 14, sealing cover; 15, snap ring; 16, electric heating pipe; 17, electric heating plate; 18, counterweight. DETAILED DESCRIPTION

[0025] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict.

[0026] In the description of the present application, it should be understood that the terms "center", "longitudinal", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the purpose of facilitating the description of the present application and simplifying the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application. In addition, the terms "first", "second" and the like are only for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined with "first", "second" and the like can explicitly or implicitly include one or more of the features. In the description of the present application, unless otherwise stated, the meaning of "a plurality of" is two or more.

[0027] In the description of the present application, it should be noted that unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting" should be understood in a broad sense, for example, it can be fixed connection, or detachable connection, or integrally connected; it can be mechanical connection, or electrical connection; it can be directly connected, or indirectly connected through intermediate medium, or the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances.

[0028] The present application will be described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.

[0029] Embodiment one: please refer to Figure 1 , Figure 2 and Figure 3 , an impregnation device for catalyst processing mainly includes an impregnation container 1 and a reflux pump 2, wherein the reflux pump 2 is a peristaltic pump type, the specific structure and connection relationship of each part are as follows: The impregnation container 1 is the core bearing part of the device, and the impregnation container 1 is internally provided with a screen 5, a partition plate 6 and an electric heating tube 16 from top to bottom. The screen 5 is connected to the inner side of the impregnation container 1 by clamping or other detachable connection method, which facilitates removal and cleaning, and also facilitates cleaning of the inside of the impregnation container 1. The catalyst raw material is directly placed above the screen 5, which can separate the carbon black base from the internal moving mechanism and avoid damage to the carbon black base.

[0030] Please refer to Figure 4 , Figure 5 and Figure 6 , the partition plate 6 is fixedly connected to the inner side below the impregnation container 1, which can divide the inside of the impregnation container 1 into two areas. The upper area is the impregnation area, and the lower area is the functional area, which mainly includes stirring and heating the impregnation liquid. The stirring shaft 7 is provided in the middle of the partition plate 6, and the stirring shaft 7 rotates under the driving action of the driving motor 9, thereby driving the stirring blade 8 fixedly connected to the top to rotate. The electric heating tube 16 is fixedly connected to the inner bottom of the impregnation container 1, and the reflux pipe 3 is wound outside the electric heating tube 16. By winding, the reflux liquid in the reflux pipe 3 can be heated during flow. A plurality of electric heating plates 17 are also fixedly connected below the partition plate 6, which assist the electric heating tube 16 to heat the impregnation liquid and improve the heating efficiency.

[0031] Please refer to Figure 7, the water inlet and the water outlet of the reflux pipe 3 are both located inside the immersion container 1, and the water inlet is further connected with a counterweight 18, which can be of different types, when the counterweight 18 has a large buoyancy, it will float in the immersion liquid, and the position of the suction liquid will change with the flow of the liquid. When the density and mass of the counterweight 18 are large, it can sink to the bottom of the immersion liquid, at this time, the position of the water inlet of the reflux pipe 3 is relatively fixed, so as to meet different immersion requirements. The reflux pipe 3 is connected by a plurality of pipes of different materials, and at least one flexible section is arranged at the end of the reflux pipe 3, a plurality of radial grooves 4 are arranged at the end of the flexible section, and the structure of the flexible section is arranged to change the position under the reaction force during the liquid discharge, so that the immersion effect is more sufficient, and the radial grooves 4 can make the reflux liquid be sprayed and resist the resistance, so as to reduce the impact force of the reflux liquid. The radial grooves 4 are at least two, so that the end of the reflux pipe 3 is divided into two parts, when a plurality of radial grooves 4 are arranged, the end of the reflux pipe 3 is divided into a plurality of parts, and the impact force of the reflux liquid will be more dispersed. Under the action of the reflux pump 2, the reflux pipe 3 can form a closed loop reflux, and the end of the reflux pipe 3 realizes directional movement through the reciprocating driving unit 10.

[0032] In the second embodiment, the following improvements are made on the basis of the previous embodiment: please refer to Figure 8 , the reciprocating driving unit 10 is arranged above the partition plate 6, and a sealing cover 14 is fixedly connected above the partition plate 6, and the core components of the reciprocating driving unit 10 are located inside the sealing cover 14, so that the immersion liquid can not enter the reciprocating driving unit 10, and the reciprocating driving unit 10 can work normally. Specifically, the reciprocating driving unit 10 includes a cam 11 fixedly connected to the outside of the stirring shaft 7, a sliding rod 13 connected with the partition plate 6 through a spring 12, the sliding rod 13 is L-shaped, and the sliding rod 13 always abuts against the surface of the cam 11 under the elastic force of the spring 12, and a snap ring 15 is further fixedly connected to the end of the sliding rod 13, and the reflux pipe 3 is installed in the snap ring 15 through clamping, so as to realize linkage with the sliding rod 13. The reciprocating driving unit 10 composed of the cam 11, the spring 12 and the sliding rod 13 can drive the snap ring 15 to reciprocate, so as to drive the flexible section of the reflux pipe 3 to reciprocate and adjust the position of the reflux liquid. Other reciprocating driving structures can also be used, for example, a crank slider mechanism, at this time, the driving of the crank slider mechanism is fixedly connected with the stirring shaft 7, and the end of the reflux pipe 3 is connected with the slider of the crank slider mechanism, so as to realize reciprocating adjustment of the position of the end of the reflux pipe 3.

[0033] Please refer to Figure 9 , a plurality of elastic clamping protrusions are arranged on the inner surface of the snap ring 15, and the clamping protrusions abut against the reflux pipe 3 under the extrusion force, so that the position of the reflux pipe 3 can be manually adjusted. The connection position of the reflux pipe 3 and the snap ring 15 is different, the movement track of the end is different when the reflux pipe 3 refluxes, and the stirring and mixing state of the immersion liquid will also change.

[0034] The top of the stirring shaft 7 is fixedly connected with stirring blades 8, and the lower end of the stirring shaft 7 extends below the partition plate 6 and is in transmission connection with a driving motor 9, so that the driving motor 9 can directly drive the stirring shaft 7 to rotate or indirectly drive the stirring shaft 7 to rotate through a gear transmission mechanism.

[0035] Taking the preparation of the Ru-Co b-active site catalyst as an example, the impregnation step of the carbon black substrate and the Ru-Co single atom precursor solution is as follows: S1, Co(NO3)2·6H2O (0.0198 g) and RuCl3·3H2O (0.0017 g) are weighed according to the proportion, dissolved in 20 mL of deionized water, 0.005 g of citric acid (chelating agent) is added, and stirred until dissolved; S2, the processed carbon black substrate is added to the chelated precursor solution of step S1, first stirred at room temperature for 1 h, and then stirred at 60℃ for 1 h.

[0036] The stirring until dissolved in step S1 can be directly carried out in the device of the present application, after complete dissolution, the carbon black substrate is placed in the mesh 5, so that Ru³+ and Co²+ are preferentially adsorbed on the "Co-O-C" defect sites of the carbon black, forming a "precursor-carrier" directional combination, laying a spatial position foundation for the Ru single atom to replace the Co lattice during subsequent calcination.

[0037] It is apparent for those skilled in the art that the present application is not limited to the details of the above exemplary embodiments, but can be implemented in other concrete forms without departing from the spirit or essential characteristics of the present application. Therefore, the embodiments should be considered as exemplary and non-limiting, and the scope of the present application is defined by the appended claims rather than the above description, and all changes falling within the meaning and range of the equivalent elements of the claims are intended to be included in the present application. Any reference signs in the claims should not be considered as limiting the claims involved.

[0038] In addition, it should be understood that although the present specification is described in terms of embodiments, not every embodiment contains only one independent technical solution, and the description of the specification is only for the sake of clarity, and those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can be appropriately combined to form other embodiments that those skilled in the art can understand.

Claims

1. A kind of impregnation device for catalyst processing, including impregnation container (1) and reflux pump (2), the inside of impregnation container (1) is provided with reflux pipe (3), the water inlet and water outlet of reflux pipe (3) are located in the inside of impregnation container (1), reflux pipe (3) forms reflux under the action of reflux pump (2), it is characterized in that, The end of the reflux pipe (3) comprises at least one flexible section, and a plurality of radial slots (4) are formed at the end of the flexible section.

2. The impregnation device for catalyst processing according to claim 1, characterized by The impregnation container (1) is internally clamped with a separation net (5), and the catalyst raw material is located above the separation net (5).

3. The impregnation device for catalyst processing according to claim 2, characterized by The impregnation container (1) is fixedly connected with a separation plate (6) below the inner side, the reflux pump (2) is located below the separation plate (6), the separation plate (6) is provided with a stirring shaft (7) in the middle part, the stirring shaft (7) is fixedly connected with stirring blades (8) at the top, and the lower end of the stirring shaft (7) is in transmission connection with a driving motor (9).

4. The impregnation device for catalyst processing according to claim 3, characterized by The stirring shaft (7) is provided with a reciprocating driving unit (10) outside, and the end of the reflux pipe (3) is connected with the reciprocating driving unit (10).

5. The impregnation device for catalyst processing according to claim 4, characterized by The reciprocating driving unit (10) comprises a cam (11) fixedly connected outside the stirring shaft (7), a sliding rod (13) connected above the separation plate (6) through a spring (12), the sliding rod (13) abuts against the surface of the cam (11) under the action force of the spring (12), and the reflux pipe (3) is connected with the sliding rod (13).

6. The impregnation device for catalyst processing according to claim 5, characterized by The separation plate (6) is fixedly connected with a sealing cover (14) above, and the sliding rod (13) and the spring (12) are located in the sealing cover (14).

7. The catalyst processing impregnation apparatus of claim 4, wherein The end of the sliding rod (13) is fixedly connected with a clamping ring (15), and the reflux pipe (3) is clamped in the clamping ring (15).

8. The catalyst processing impregnation apparatus of claim 3, wherein The reflux pump (2) is a peristaltic pump, the impregnation container (1) is fixedly connected with an electric heating pipe (16) at the bottom, the reflux pipe (3) is wound outside the electric heating pipe (16), and the separation plate (6) is fixedly connected with an electric heating plate (17) below.

9. The catalyst processing impregnation apparatus of claim 1, wherein The reflux pipe (3) is connected with a counterweight (18) at the water inlet.

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