Ceramic membrane batch preparation device

Abstract

The utility model discloses a ceramic membrane batch preparation device, which comprises a material storage tank for storing membrane casting liquid and a coating groove for placing a plurality of ceramic tubes, the coating groove is communicated with the bottom of the material storage tank through a two-way pump, an overflow port is arranged on one side of the coating groove and close to the top, and the overflow port is communicated with the bottom of the material storage tank. The overflow port is communicated with the material storage tank through a pipeline; and a plurality of ultrasonic rods are erected in the coating groove. Through mutual cooperation of the material storage tank, the two-way pump and the film coating tank, large-scale preparation of tubular ceramic films of different types and pore diameters is realized by utilizing the types of injected film casting solutions, the film coating time and the film coating times.

Description

Technical Field

[0001] The utility model relates to the technical field of ceramic membrane preparation, in particular to a ceramic membrane batch preparation device. Background Art

[0002] Ceramic membranes are a type of membrane material with great development prospects, with the characteristics of high mechanical strength, high temperature resistance, chemical corrosion resistance, easy regeneration and long service life. Usually, ceramic membranes are made of Al2O3, SiO2, ZrO2, TiO2 and their composite materials by repeated coating-high temperature sintering on a macroporous ceramic support. The preparation process is cumbersome, time-consuming and energy-consuming. Therefore, optimizing the preparation process and cost of ceramic membranes is of great significance to improve the competitiveness in practical applications. Utility Model Content

[0003] In order to solve the above technical problems, the utility model provides a device for batch preparation of ceramic membranes.

[0004] In order to achieve the above purpose, the technical solution adopted by the utility model is as follows:

[0005] The utility model discloses a device for batch preparation of ceramic membranes, comprising a storage tank for storing casting liquid and a coating tank for placing a plurality of ceramic tubes, the coating tank is connected to the bottom of the storage tank by a two-way pump, an overflow port is opened on one side of the coating tank and near the top, the overflow port is connected to the storage tank by a pipeline, and a plurality of ultrasonic rods are set in the coating tank.

[0006] Preferably, the bottom of the coating tank has a plurality of limiting rods for placing ceramic tubes. When the plurality of ceramic tubes are placed on the limiting rods one by one, there is a gap between two adjacent ceramic tubes, and there is also a gap between the ceramic tubes and the wall of the coating tank.

[0007] Preferably, the ultrasonic rod is located in one of the gaps in the coating tank.

[0008] Preferably, when the ceramic tube is assembled in the coating tank, the level of the overflow port is lower than the level of the top of the ceramic tube, so as to prevent the casting liquid from entering the inner wall of the ceramic tube.

[0009] The utility model also discloses a method for batch preparation of ceramic membranes, which is prepared by the above-mentioned batch preparation device of ceramic membranes, comprising the following steps:

[0010] S1: Treatment of ceramic support

[0011] After high-temperature calcination and water boiling, the outer side of the ceramic tube is coated with a suspension to form a bottom layer;

[0012] S2: Preparation of the middle layer of hollow nanomaterials

[0013] On the treated ceramic tube, the hollow nano material suspension is applied to the bottom layer by spraying or dipping, and then dried and sintered to form an intermediate layer together with the bottom layer;

[0014] S3: coating-sintering

[0015] S3.1. Place the ceramic tubes with the intermediate layer into the coating tank in sequence, and introduce the casting solution into the storage tank;

[0016] S3.2, controlling the bidirectional pump to inject the casting liquid into the coating tank to coat the ceramic tube. Preferably, after the ceramic tube is coated for the first time, the arrangement direction of the ceramic tube is reversed and coated again;

[0017] S3.3. After coating, control the bidirectional pump to discharge the casting liquid in the coating tank, take out the ceramic tube, dry it, and place it on the hanging firing bracket for sintering in a box-type muffle furnace.

[0018] Compared with the prior art, the utility model has the following beneficial effects:

[0019] The utility model realizes the large-scale preparation of tubular ceramic membranes of different types and pore sizes by cooperating with each other through the provided storage tank, bidirectional pump and coating tank and by injecting different types of casting liquids, coating time and coating times. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the structure of a ceramic membrane batch preparation device;

[0021] Figure 2 It is the SEM image of the cross-sectional structure of the bottom layer;

[0022] Figure 3 It is a SEM image of the surface state of the bottom layer;

[0023] Figure 4 is the SEM image of the cross-sectional structure of the particle layer of 200nm Al203 NPs;

[0024] Figure 5 is the SEM image of the surface state of the particle layer of 200nm Al203 NPs;

[0025] Figure 6 is the SEM image of the cross-sectional structure of the particle layer of 50nm Al203 NPs;

[0026] Figure 7 is the SEM image of the surface state of the particle layer of 50nm Al203 NPs;

[0027] Figure 8 The data and repeatability are measured by the gas-liquid method at the bottom layer;

[0028] Fig. 9 The data and repeatability are obtained by the gas-liquid method of 200nm Al203 particle layer;

[0029] Fig.10 The data and repeatability are obtained by the gas-liquid method using a 50nm Al2O3 particle layer.

[0030] Fig.11 is a SEM image of the cross-sectional structure of the boehmite separation membrane;

[0031] Fig.12 is a SEM image of the surface state of the boehmite separation membrane;

[0032] Fig.13 It is the nanoperm data and repeatability of the boehmite layer;

[0033] Fig.14 Nanoperm data and repeatability of silicon-zirconium layers.

[0034] Figure symbols: 1. Storage tank, 2. Coating tank, 21. Overflow port, 22. Limit rod, 3. Ceramic tube, 4. Bidirectional pump, 5. Pipeline, 6. Ultrasonic rod. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solutions and advantages of the utility model more clearly understood, the utility model is further described in detail below in conjunction with embodiments and drawings. The schematic implementation manner of the utility model and its description are only used to explain the utility model and are not intended to limit the utility model.

[0036] Example 1

[0037] like Figure 1 A ceramic membrane batch preparation device shown includes a storage tank 1 for storing casting liquid and a coating tank 2 for placing multiple ceramic tubes 3. The coating tank 2 is connected to the bottom of the storage tank 1 through a two-way pump 4. An overflow port 21 is provided on one side of the coating tank 2 and near the top. The overflow port 21 is connected to the storage tank 1 through a pipe 5. Multiple ultrasonic rods 6 are set up in the coating tank 2.

[0038] During implementation, multiple ceramic tubes 3 are placed in the coating tank 2 at the same time, and the casting liquid is controlled to flow in and out of the coating tank 2 by a two-way pump 4, so that the casting liquid can be applied to the ceramic tube 3. By controlling the type of casting liquid, coating time, and coating times, tubular ceramic membranes of different types and pore sizes can be prepared on a large scale. Specifically, after the casting liquid enters the coating tank 2, the ultrasonic rod 6 is set to eliminate bubbles in the liquid. In the process of the casting liquid being applied to the ceramic tube 3 to form a ceramic membrane, the generation of bubbles on the surface of the ceramic membrane can be reduced.

[0039] Preferably, after the ceramic tube 3 is arranged in the coating tank 2, in order to improve the stability of the arrangement of the coating tank 2, the bottom of the coating tank 2 has a plurality of limiting rods 22 for placing the ceramic tube 3. Specifically, when a plurality of ceramic tubes 3 are placed on the limiting rods 22 one by one, there is a gap between two adjacent ceramic tubes 3, and there is also a gap between the ceramic tube 3 and the wall of the coating tank 2, to ensure that the casting liquid can be applied to the surface of the entire ceramic tube 3.

[0040] Preferably, the ultrasonic rod 6 is located in one of the gaps in the coating tank 2 .

[0041] Preferably, when the ceramic tube 3 is assembled in the coating tank 2 , the level of the overflow port 21 is lower than the level of the top of the ceramic tube 3 , so as to prevent the casting liquid from entering the inner wall of the ceramic tube 3 .

[0042] Embodiment 2:

[0043] A method for batch preparation of ceramic membranes, prepared by the above-mentioned batch preparation device for ceramic membranes, wherein the prepared ceramic membranes have stable performance, comprises the following steps:

[0044] S1: Treatment of ceramic support

[0045] After high-temperature calcination and boiling treatment, the outer side of the ceramic tube 3 is coated with a suspension to form a bottom layer, wherein the suspension is an alumina particle suspension, which is a traditional material for preparing an intermediate layer and is also used here to prepare the intermediate layer.

[0046] S2: Preparation of the middle layer of hollow nanomaterials

[0047] On the treated ceramic tube 3, the hollow nano material suspension is coated on the base layer by spraying or dipping, and after drying and sintering, it forms an intermediate layer together with the base layer. The hollow nano material used here is an innovation relative to traditional alumina materials. The hollow nano material as the material of the intermediate layer can reduce the mass transfer resistance and improve the permeability of the ceramic membrane prepared subsequently.

[0048] S3: coating-sintering

[0049] S3.1, placing the ceramic tube 3 with the intermediate layer into the coating tank 2 in sequence, and introducing the casting liquid into the storage tank 1;

[0050] S3.2, control the bidirectional pump 4 to inject the casting liquid into the coating tank 2 to coat the ceramic tube 3. Preferably, after the ceramic tube 3 is coated for the first time, the arrangement direction of the ceramic tube 3 is reversed and coated again;

[0051] S3.3. After the coating is completed, the two-way pump 4 is controlled to discharge the casting liquid in the coating tank 2, and the ceramic tube 3 is taken out, dried, and then placed on a hanging firing bracket for sintering in a box-type muffle furnace.

[0052] Application examples:

[0053] 1. Preparation of α-Al2O3 microfiltration membrane;

[0054] 1.1. Prepare silicon zirconium sol by sol-gel method, then mix with Al2O3 powder to prepare casting solution;

[0055] 1.2. Pour the prepared casting solution into the storage tank 1 and insert the ceramic tube 3 into the coating tank 2;

[0056] 1.3. Control the bidirectional pump 4 to inject the casting liquid into the coating tank 2 and keep it for a certain period of time. At this time, the casting liquid adheres to the surface of the ceramic tube 3. Then control the bidirectional pump 4 to drain the casting liquid in the coating tank 2 and turn the arrangement direction of the ceramic tube 3. Inject the casting liquid into the coating tank 2 again, so that the casting liquid adheres to the ceramic tube 3 to form an α-Al2O3 separation layer;

[0057] 1.4. The ceramic tube 3 with the surface layer is dried and then placed in a muffle furnace and calcined at 500-1200° C.;

[0058] 1.5. Repeat steps 1.3-1.4 1-3 times to obtain a microfiltration membrane with α-Al2O3 as the separation layer.

[0059] 2. Preparation of γ-Al2O3 ultrafiltration membrane

[0060] 2.1. Coat a layer of PVA 0.5-10wt% on the ceramic tube 3 and let it dry naturally;

[0061] 2.2. Pour the boehmite sol into the storage tank 1, and operate according to step 1.3 of preparing the α-Al2O3 microfiltration membrane to form a γ-Al2O3 separation layer on the surface of the ceramic tube 3;

[0062] 2.3. Take out the ceramic tube 3 with the γ-Al2O3 separation layer, dry it and put it into a muffle furnace for sintering at 500-900°C;

[0063] 2.4. Repeat steps 2.2-2.3 1-3 times to obtain an ultrafiltration membrane with γ-Al2O3 as the separation layer.

[0064] 3. Preparation of SiO2-ZrO2 nanofiltration membrane

[0065] 3.1. Coat a layer of PVA 0.5-10 wt% on the above-mentioned α-Al2O3 ceramic tube 3 and dry it naturally;

[0066] 3.2. Pour the homemade silica-zirconium sol into the storage tank 1, and operate according to step 1.3 of preparing the α-Al2O3 microfiltration membrane to form a SiO2-ZrO2 separation layer on the surface of the ceramic tube 3, wherein the silica-zirconium sol is prepared by the hydrolysis process of a zirconium precursor and a silicon precursor;

[0067] 3.3. Take out the ceramic tube 3 with the SiO2-ZrO2 separation layer, dry it and place it in a muffle furnace for sintering at 400-600°C;

[0068] 3.4. Repeat steps 3.2-3.3 1-3 times to obtain a nanofiltration membrane with SiO2-ZrO2 as the separation layer.

[0069] 4. Preparation of TiO2 nanofiltration membrane

[0070] 4.1. Coat a layer of PVA 0.5-10wt% on the ceramic tube 3 and let it dry naturally;

[0071] 4.2. Pour the TiO2 sol into the storage tank 1, and operate according to step 1.3 of preparing the α-Al2O3 microfiltration membrane to form a TiO2 separation layer on the surface of the ceramic tube 3;

[0072] 4.3. Take out the ceramic tube 3 with the TiO2 separation layer, dry it, and then sinter it in a muffle furnace at 500-900°C;

[0073] 4.4. Repeat steps 4.2-4.3 1-3 times to obtain a nanofiltration membrane with TiO2 as the separation layer.

[0074] like Figure 1-14 As shown, a slurry composed of silicon zirconium sol and Al2O3 particles is used to coat the membrane through the above-mentioned ceramic membrane batch preparation device. The pore size of the tubular ceramic membrane obtained by sintering is in the range of 1-2nm. This method can prepare multiple ceramic membranes at the same time, and the prepared ceramic membranes have stable performance.

[0075] Of course, the present invention may have many other implementation modes. Without departing from the spirit and essence of the present invention, technicians familiar with the field may make various corresponding changes and deformations based on the present invention, but these corresponding changes and deformations should all fall within the scope of protection of the claims attached to the present invention.

Claims

1. A ceramic membrane batch preparation device, characterized in that: The invention comprises a storage tank (1) for storing a casting liquid and a coating tank (2) for placing a plurality of ceramic tubes (3); the coating tank (2) is connected to the bottom of the storage tank (1) via a two-way pump (4); an overflow port (21) is provided on one side of the coating tank (2) near the top; the overflow port (21) is connected to the storage tank (1) via a pipeline (5); and a plurality of ultrasonic rods (6) are arranged in the coating tank (2).

2. The ceramic membrane batch preparation device according to claim 1, characterized in that: The bottom of the coating tank (2) is provided with a plurality of limiting rods (22) for placing the ceramic tubes (3); when the plurality of ceramic tubes (3) are placed one by one on the limiting rods (22), a gap exists between two adjacent ceramic tubes (3), and a gap also exists between the ceramic tubes (3) and the wall of the coating tank (2).

3. The ceramic membrane batch preparation device according to claim 2, characterized in that: The ultrasonic rod (6) is located in one of the gaps in the coating tank (2).

4. The device for batch preparation of ceramic membranes according to any one of claims 1 to 3, characterized in that: When the ceramic tube (3) is installed in the coating tank (2), the horizontal height of the overflow port (21) is smaller than the horizontal height of the top end of the ceramic tube (3).

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