Reaction apparatus for preparing iron oxide black

Abstract

This utility model discloses a reaction apparatus for preparing iron oxide black, belonging to the field of iron oxide preparation technology. The apparatus includes a vessel body and a cylindrical body. The vessel body is equipped with a first inlet pipe and a first outlet pipe, and a first drain pipe is connected to the side wall of the vessel body. The cylindrical body is lower than the vessel body and is equipped with a first inlet pipe and a first outlet pipe. A heat exchange tube is installed inside the cylindrical body, and both the first inlet pipe and the first outlet pipe are connected to the heat exchange tube. The first drain pipe is connected to the first inlet pipe. The cylindrical body also has a second inlet pipe and a second outlet pipe. The second outlet pipe is connected to a transfer pump, which is connected to the first inlet pipe. This utility model allows the supernatant in the vessel body to be directly discharged into the cylindrical body, eliminating the need for a separate pump to extract the supernatant from the vessel body, thus improving the efficiency of iron oxide black preparation. It also adapts to the different stratification heights of the supernatant and the precipitate during the cyclic preparation of iron oxide black. Furthermore, the supernatant from the previous reaction can be preheated in the heat exchange tube within the cylindrical body to preheat the ferrous sulfate solution for the next reaction, saving energy and reducing consumption.

Description

Technical Field

[0001] This utility model belongs to the field of iron oxide preparation technology, specifically relating to a reaction apparatus for preparing iron oxide black. Background Technology

[0002] Iron oxide black, with the molecular formula Fe3O4, is a black powder. It is an adduct of Fe2O3 and FeO, insoluble in water, magnetic, and possesses high tinting strength and hiding power. It is non-toxic and pollution-free. As an industrial raw material, iron oxide black is widely used in coatings, cosmetics, biomedicine, and other fields, and has broad development prospects. Precipitation oxidation is a common process for producing iron oxide black. In this process, a purified ferrous sulfate solution is neutralized with liquid alkali to generate Fe(OH)2. The solution is then heated to 85℃~95℃ while air is introduced for oxidation (also serving as a stirring action) to produce an iron oxide black slurry. After filtration, washing, drying, fine grinding, and blending, the final iron oxide black product is obtained. This direct oxidation method is an innovation over the addition method, and the resulting product has superior coloring properties. Our company has improved upon the existing precipitation oxidation method and applied for a patent for the improved method. The invention patent application is titled "A Method for Producing Iron Oxide Black by Liquid-Phase Addition," and the application publication number is CN113772741A. This method uses the iron oxide black produced in the previous batch as the nucleus for the formation of the next batch of iron oxide black, repeating this process multiple times. This improves the chemical stability and color quality of the iron oxide black, effectively enhancing the quality of the iron oxide black product. However, existing reactors are inconvenient to use when manufacturing iron oxide black using this method. During the removal of the supernatant, an external pipeline needs to be inserted into the reactor from the top inlet each time, and then a pump is used to extract the supernatant. This process is inconvenient and affects operational efficiency. Utility Model Content

[0003] The technical problem solved by this invention is to provide a reaction apparatus for preparing iron oxide black to improve the preparation efficiency of iron oxide black.

[0004] Technical solution: To solve the above-mentioned technical problems, the technical solution adopted by this utility model is as follows:

[0005] A reaction apparatus for preparing iron oxide black includes a vessel body and a cylinder body. The vessel body is provided with a first feed pipe and a first discharge pipe. A first drain pipe is connected to the side wall of the vessel body. The cylinder body is lower in height than the vessel body. The cylinder body is provided with a first inlet pipe and a first outlet pipe. A heat exchange pipe is provided inside the cylinder body. The first inlet pipe and the first outlet pipe are both connected to the heat exchange pipe. The first drain pipe is connected to the first inlet pipe. The cylinder body is also provided with a second inlet pipe and a second outlet pipe. The second outlet pipe is connected to a delivery pump. The delivery pump is connected to the first feed pipe through a delivery pipe.

[0006] Furthermore, a second drain pipe and a third drain pipe are connected to the side wall of the vessel body and are connected to the first inlet pipe. The second drain pipe is higher than the first drain pipe, and the third drain pipe is higher than the second drain pipe.

[0007] Furthermore, the internal space height of the vessel body is H, the height of the third drain pipe is h3, h3≥0.5H, the height of the second drain pipe is h2, h2≥0.25H, and the height of the first drain pipe is h1, h1≥0.125H.

[0008] Furthermore, the vessel body is connected to a main gas passage pipe, the vessel body is provided with an air inlet pipe connected to the main gas passage pipe, the first drain pipe is provided with a first branch pipe connected to the main gas passage pipe, the second drain pipe is provided with a second branch pipe connected to the main gas passage pipe, and the third drain pipe is provided with a third branch pipe connected to the main gas passage pipe.

[0009] Furthermore, the vessel body is provided with a stirring assembly, which includes a geared motor assembly mounted on the vessel body, a stirring shaft connected to the geared motor assembly, and a stirring paddle connected to the stirring shaft.

[0010] Furthermore, the delivery pipe is connected to the second heater.

[0011] Furthermore, the first drain pipe is equipped with a first drain valve, the second drain pipe is equipped with a second drain valve, and the third drain pipe is equipped with a third drain valve.

[0012] Furthermore, a second feed pipe is provided on the top wall of the vessel, and the first discharge pipe is located at the bottom of the vessel.

[0013] Beneficial effects: Compared with the prior art, the present invention has the following advantages:

[0014] 1. A first drain pipe is installed on the side wall of the reactor body, which can directly drain the supernatant in the reactor body into the cylinder body without the need to install a separate pump to extract the supernatant in the reactor body, thus improving the preparation efficiency of iron oxide black;

[0015] 2. The side wall of the vessel is equipped with a second drain pipe and a third drain pipe at different heights than the first drain pipe, which can accommodate the different stratification heights of the supernatant and the precipitate during the iron oxide black recycling process, and facilitate the discharge of the supernatant;

[0016] 3. The supernatant from the previous reaction inside the cylinder can be used to preheat the ferrous sulfate solution for the next reaction in the heat exchange tube, saving energy and reducing consumption.

[0017] 4. Multiple drain pipes are connected to branch pipes, allowing external air to enter the reactor body through the drain pipes and participate in the reaction, thus improving the uniformity of the reaction. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of the device according to an embodiment of the present invention;

[0019] Figure 2 This is a schematic diagram of the vessel structure in the embodiment;

[0020] Figure 3 This is a schematic diagram of the cylindrical structure of an embodiment;

[0021] Figure 4 This is a schematic diagram of the second heater structure in the embodiment. Detailed Implementation

[0022] The present invention will be further illustrated below with reference to specific embodiments. The embodiments are implemented based on the technical solution of the present invention. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0023] like Figure 1 and Figure 2 As shown, a reaction apparatus for preparing iron oxide black includes a vessel body 1 and a cylindrical body 2. The vessel body 1 is cylindrical in shape, with its top and bottom protruding outwards. The bottom of the vessel body 1 is supported by a first bracket 7. The vessel body 1 is provided with a first feed pipe 11 and a first discharge pipe 12. The first feed pipe 11 is located at the top of the vessel body 1 for feeding, and the first discharge pipe 12 is located at the bottom of the vessel body 1 for discharging. A second feed pipe 16 is also provided at the top of the vessel body 1 for feeding. The vessel body 1 is provided with a stirring assembly 5, which includes a geared motor assembly 51, a stirring shaft 52, and a stirring paddle 53. The geared motor assembly 51 is connected to the outer top wall of the vessel body 1 and includes a conventional motor and a reducer. The upper end of the stirring shaft 52 is connected to the reducer of the geared motor assembly 51. The stirring paddle 53 is connected to the stirring shaft 52. The stirring paddle 53 is a conventional paddle-type or anchor-type stirring paddle, and more than one set of stirring paddles 53 can be provided on the stirring shaft 52. When the motor is working, it drives the reducer to work, which in turn drives the stirring paddle 53 to rotate through the stirring shaft 52, thus stirring the material in the vessel 1.

[0024] like Figure 1 and Figure 2As shown, a first drain pipe 13, a second drain pipe 14, and a third drain pipe 15 are connected to the side wall of the vessel body 1. All three drain pipes communicate with the internal space of the vessel body 1. The height of the internal space of the vessel body 1 is H. The height of the first drain pipe 13 is h1, where h1 ≥ 0.125H. In this embodiment, h1 = 0.125H. The height of the second drain pipe 14 is higher than that of the first drain pipe 13, and its height is h2, where h2 ≥ 0.25H. In this embodiment, h2 = 0.25H. The height of the third drain pipe 15 is higher than that of the second drain pipe 14, and its height is h3, where h3 ≥ 0.5H. In this embodiment, h2 = 0.5H. The first drain pipe 13 and the third drain pipe 15 are located on the same side of the vessel body 1. The second drain pipe 14 is located on the other side of the vessel body 1. The first drain pipe 13 is equipped with a first drain valve 131. When the first drain valve 131 is opened, the liquid in the vessel body 1 is discharged from the first drain pipe 13. The second drain pipe 14 is equipped with a second drain valve 141. When the second drain valve 141 is opened, the liquid in the vessel body 1 is discharged from the second drain pipe 14. The third drain pipe 15 is equipped with a third drain valve 151. When the third drain valve 151 is opened, the liquid in the vessel body 1 is discharged from the third drain pipe 15. Since the first drain pipe 13, the second drain pipe 14 and the third drain pipe 15 are at different heights, the discharge of liquid at different heights in the vessel body 1 can be controlled by selecting appropriate drain valves. The first drain valve 131, the second drain valve 141 and the third drain valve 151 are all existing butterfly valves.

[0025] like Figure 1 , Figure 2 and Figure 3As shown, the cylindrical body 2 is located beside the vessel body 1, and is lower than the vessel body 1. The cylindrical body 2 is a horizontally arranged cylinder, including a shell 26 and multiple heat exchange tubes 23 arranged inside the shell 26. The cylindrical body 2 is provided with a first liquid inlet pipe 21 and a first liquid outlet pipe 22. The first liquid inlet pipe 21 is located at the right end of the shell 26, and the first liquid outlet pipe 22 is located at the left end of the shell 26. Two tube sheets 27 are also provided inside the shell 26. The heat exchange tubes 23 are arranged horizontally inside the shell 26, and both ends of the heat exchange tubes 23 are connected to the two tube sheets 27 respectively. The first liquid inlet pipe 21 and the first liquid outlet pipe 22 are both connected to the heat exchange tubes 23. The liquid entering through the first liquid inlet pipe 21 enters the heat exchange tubes 23 and flows out through the first liquid outlet pipe 22. The shell 26 is also equipped with a second inlet pipe 24 and a second outlet pipe 25. Both the second inlet pipe 24 and the second outlet pipe 25 are connected to the space inside the shell 26. The second inlet pipe 24 is located at the top of the shell 26, and the second outlet pipe 25 is located at the bottom of the shell 26. The liquid entering through the second inlet pipe 24 exchanges heat with the liquid inside the heat exchange tube 23 on the outer wall of the heat exchange tube 23 and then exits through the second outlet pipe 25. In this embodiment, the shell 2 adopts an existing shell-and-tube heat exchanger. The liquid entering through the first inlet pipe 21 flows through the tube side, and the liquid entering through the second inlet pipe 24 flows through the shell side. The two liquids complete heat exchange on the tube wall of the heat exchange tube 23. Multiple baffles are set inside the shell 26 to extend the liquid path length inside the shell 26 and improve the heat exchange effect. The first drain pipe 13, the second drain pipe 14, and the third drain pipe 15 are all connected to the first inlet pipe 21. Since the height of the shell 2 is lower than that of the vessel body 1, the liquid discharged from the three drain pipes directly enters the heat exchange tube 23 through the first inlet pipe 21.

[0026] like Figure 1 , Figure 2 and Figure 3 As shown, a main gas pipe 4 is connected to the bottom of the vessel body 1 and is connected to an external air source. An air inlet pipe 40, connected to the main gas pipe 4, is located inside the vessel body 1 near the bottom wall. The air inlet pipe 40 has multiple small holes arranged in an array. Under the influence of the external air source, external air enters the vessel body 1 and is ejected upwards from the air inlet pipe 40. These small bubbles increase the gas-liquid contact area, and the oxidation effect of the air promotes the reaction. A first branch pipe 41 is connected to the first drain pipe 13, a second branch pipe is connected to the second drain pipe 14, and a third branch pipe 43 is connected to the third drain pipe 15. All three branches are connected to the main gas pipe 4, allowing air to selectively enter the vessel body 1 from either the first, second, or third branch pipe. These multiple air entry points ensure the uniformity of the air-liquid reaction within the vessel body 1. Solenoid valves are installed on the intake pipe 40, the first branch pipe 41, the second branch pipe and the third branch pipe 43 to control the opening and closing of the corresponding air passages.

[0027] like Figure 1 , Figure 3and Figure 4 As shown, the second outlet pipe 25 is connected to the input end of the transfer pump 3, and the output end of the transfer pump 3 is connected to the first feed pipe 11 through the transfer pipe 32. The liquid in the shell 26 of the cylinder 2 is transported to the vessel 1 through the transfer pump 3. The transfer pipe 32 is connected to the second heater 6. The second heater 6 adopts an existing electric heater and has multiple heating tubes 61 inside. Thermometers are installed on both the front and rear pipes of the second heater 6. The liquid entering through the second inlet pipe 24 is preheated by the cylinder 2 and its temperature rises. When the temperature of the liquid entering the vessel 1 still does not meet the requirements, the second heater 6 is turned on to heat.

[0028] During operation, the ferrous sulfate solution is connected to the second inlet pipe 24 and, under the action of the transfer pump 3, is transported into the reactor body 1 through the first feed pipe 11. Passing through the second heater 6, the ferrous sulfate solution is preheated to 70°C. After entering the reactor body 1, it is kept at a temperature of 70-95°C. Air is introduced into the reactor body 1 through the air inlet pipe 40, and then 30M of air is introduced. 3 Under the condition of [unclear - likely a specific pressure] / min, sodium hydroxide (NaOH) solution is added through the second feed pipe 16. Ferrous sulfate and sodium hydroxide undergo an addition reaction to generate ferric oxide (Fe3O4). After the reaction is complete, stirring is stopped, and the ferric oxide settles and accumulates at the bottom of the vessel 1. After settling, depending on the height of the supernatant, the drain valve on the corresponding first drain pipe 13, second drain pipe 14, or third drain pipe 15 is opened. The supernatant is discharged from the corresponding drain pipe into the first inlet pipe 21 and then into the heat exchange tube 23. The generated ferric oxide is retained at the bottom of the vessel 1. Ferrous sulfate solution is then connected to the second inlet pipe 24. At this time, the ferrous sulfate solution is preheated in the vessel 2 by the supernatant in the heat exchange tube 23. After preheating, the ferrous sulfate solution reaches a temperature of 70°C and is then transported into the vessel 1 through the first feed pipe 11 by the transfer pump 3 (if the temperature is insufficient, it is assisted by heating when passing through the second heater 6). NaOH solution is added, and air is introduced at a rate of 30 m / s. 3 At a constant temperature of 70-95℃, ferric oxide continues to be generated. In reactor 1, ferrous sulfate solution is added to react and generate ferric oxide – the ferric oxide settles – the supernatant is removed, and this cycle is repeated. The supernatant removed in each cycle can be used to preheat the next batch of ferrous sulfate solution in reactor 2. This cycle is repeated 6 times. The precipitate is collected and washed, then subjected to conventional pressure filtration, drying, and grinding to obtain iron oxide black.

[0029] The above description is only a preferred embodiment of the present utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present utility model, and these improvements and modifications should also be considered within the protection scope of the present utility model.

Claims

1. A reaction apparatus for preparing iron oxide black, characterized in that, The vessel includes a vessel body (1) and a cylindrical body (2). The vessel body (1) is provided with a first feed pipe (11) and a first discharge pipe (12). A first drain pipe (13) is connected to the side wall of the vessel body (1). The cylindrical body (2) is lower than the vessel body (1). The cylindrical body (2) is provided with a first inlet pipe (21) and a first outlet pipe (22). A heat exchange pipe (23) is provided inside the cylindrical body (2). The first inlet pipe (21) and the first outlet pipe (22) are both connected to the heat exchange pipe (23). The first drain pipe (13) is connected to the first inlet pipe (21). The cylindrical body (2) is also provided with a second inlet pipe (24) and a second outlet pipe (25). The second outlet pipe (25) is connected to a delivery pump (3). The delivery pump (3) is connected to the first feed pipe (11) through a delivery pipe (32).

2. The reaction apparatus for preparing iron oxide black according to claim 1, characterized in that, The side wall of the vessel body (1) is also connected to a second drain pipe (14) and a third drain pipe (15) connected to the first inlet pipe (21). The second drain pipe (14) is higher than the first drain pipe (13), and the third drain pipe (15) is higher than the second drain pipe (14).

3. The reaction apparatus for preparing iron oxide black according to claim 2, characterized in that, The internal space height of the vessel body (1) is H, the height of the third drain pipe (15) is h3, h3≥0.5H, the height of the second drain pipe (14) is h2, h2≥0.25H, and the height of the first drain pipe (13) is h1, h1≥0.125H.

4. The reaction apparatus for preparing iron oxide black according to claim 2, characterized in that, The vessel body (1) is connected to a main gas passage (4), and the vessel body (1) is provided with an air inlet pipe (40) connected to the main gas passage (4). The first drain pipe (13) is provided with a first branch pipe (41) connected to the main gas passage (4), the second drain pipe (14) is provided with a second branch pipe connected to the main gas passage (4), and the third drain pipe (15) is provided with a third branch pipe (43) connected to the main gas passage (4).

5. The reaction apparatus for preparing iron oxide black according to claim 1, characterized in that, The vessel body (1) is provided with a stirring assembly (5), which includes a geared motor assembly (51) disposed on the vessel body (1), a stirring shaft (52) connected to the geared motor assembly (51), and a stirring paddle (53) connected to the stirring shaft (52).

6. The reaction apparatus for preparing iron oxide black according to claim 1, characterized in that, The delivery pipe (32) is connected to the second heater (6).

7. The reaction apparatus for preparing iron oxide black according to claim 2, characterized in that, The first drain pipe (13) is provided with a first drain valve (131), the second drain pipe (14) is provided with a second drain valve (141), and the third drain pipe (15) is provided with a third drain valve (151).

8. The reaction apparatus for preparing iron oxide black according to claim 1, characterized in that, The top wall of the vessel body (1) is also provided with a second feed pipe (16), and the first discharge pipe (12) is located at the bottom of the vessel body (1).

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