Integrated reaction equipment for producing ferrous oxalate

Abstract

The utility model belongs to the technical field of ferrous oxalate production equipment, and particularly relates to integrated reaction equipment for producing ferrous oxalate, which comprises a reaction kettle body, and a stirring device, a permanent magnet disc, a gas dispersion disc, a liquid distributor and the like are arranged in the reaction kettle body. The continuous reaction of continuous feeding and continuous discharging is realized, the production efficiency of ferrous oxalate is improved, and the investment of equipment and land occupation is reduced.

Description

Technical Field

[0001] The utility model belongs to the technical field of ferrous oxalate production equipment, and particularly relates to an integrated reaction equipment for producing ferrous oxalate. Background Technique

[0002] At present, most of the processes for preparing ferrous oxalate are synthesized by the reaction of oxalic acid and ferrous sulfate. In China, industrial-grade ferrous sulfate products are usually obtained as by-products of titanium dioxide production, and they contain relatively high levels of heavy metals such as Zn, Mg, Mn, Ni, and S content. The prepared products do not meet the product indicators of battery-grade ferrous oxalate, and ferrous oxalate products that meet the indicators cannot be obtained even through water washing and impurity removal agents. In the process of synthesizing ferrous oxalate with iron powder, after first using iron powder and sulfuric acid to generate a ferrous sulfate solution, oxalic acid is then added to the ferrous sulfate solution to continue the reaction to form ferrous oxalate precipitate. In this process route, the consumption of iron powder raw materials is large, there are many reaction devices, the floor area is large, and there are many post-treatment processes for the acidic solution after filtering out the ferrous oxalate precipitate, resulting in high investment costs. Content of the Utility Model

[0003] The utility model provides an integrated reaction equipment for ferrous oxalate production, which solves the technical problems of many reaction devices and insufficient and discontinuous reactions in the process from iron powder to ferrous sulfate and then from ferrous sulfate to ferrous oxalate, and realizes the continuous production of ferrous oxalate from iron powder in one reaction device.

[0004] The solution of the utility model to the above technical problems is as follows: An integrated reaction equipment for producing ferrous oxalate, characterized in that it includes a reaction kettle body, a jacket is arranged outside the reaction kettle body, the jacket is provided with a jacket inlet and a jacket outlet, a iron powder inlet, an exhaust port, a temperature measuring port, an oxalic acid inlet, and a stirring device are arranged at the top of the reaction kettle body, and the stirring device includes a motor, a reducer, a linkage shaft, a stirring shaft, and a stirring paddle; a liquid distributor, a permanent magnet disk, and a gas dispersion disk are arranged inside the reaction kettle body, an air inlet is arranged at the bottom of the reaction kettle body, and the permanent magnet disk is arranged above the gas dispersion disk through a bracket; the liquid distributor is arranged above the permanent magnet disk and is communicated with a liquid inlet outside the reaction kettle body through a pipeline, and a discharge port is arranged at the lower part of the side of the reaction kettle body.

[0005] Further, the motor is a variable frequency motor.

[0006] Further, the permanent magnet disk is of a C-shaped structure, and liquid channels are arranged on the permanent magnet disk.

[0007] Further, the permanent magnet disk is wrapped with a corrosion-resistant non-metallic outer layer.

[0008] Further, the gas dispersion disk is an internal cavity structure made of polytetrafluoroethylene or polypropylene. The outlet end of the gas dispersion disk is provided with a round hole to connect the internal cavity of the gas dispersion disk with the inside of the reaction kettle, and the inlet end of the gas dispersion disk is connected to the nitrogen pipe outside the reaction kettle body through a pipeline.

[0009] Further, the liquid distributor is an umbrella-shaped disk structure.

[0010] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0011] (1) By providing a permanent magnet disk, the present utility model adsorbs iron powder to keep the iron powder in the supernatant, enabling the iron powder to react fully, thereby reducing the consumption of iron powder.

[0012] (2) The permanent magnet disk with a C-shaped structure of the present utility model is convenient for disassembly and maintenance without disassembling the stirring shaft.

[0013] (3) Since the ferrous oxalate precipitate particles are small and easy to aggregate and difficult to disperse, the present utility model sets a gas dispersion disk to continuously agitate the precipitate in a large area from the bottom by nitrogen gas, ensuring that the precipitated iron powder contacts the liquid and continues to participate in the reaction, avoiding the iron powder that loses magnetism during the reaction process being covered by the continuously produced ferrous oxalate precipitate and unable to participate in the reaction normally; it can also displace hydrogen inside the reaction kettle body, thereby improving the purity of ferrous oxalate.

[0014] (4) The present utility model realizes the continuous production of ferrous oxalate using iron powder in a reaction device, reduces the investment in reaction equipment and the consumption of iron powder raw materials, and can operate continuously, safely and efficiently. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 is a schematic structural diagram of the present utility model;

[0016] Figure 2 is a schematic structural diagram of the permanent magnet disk of the present utility model;

[0017] Figure 3 is a schematic cross-sectional structural diagram of the gas dispersion disk of the present utility model;

[0018] In the figure, 1. iron powder inlet; 2. reaction kettle body; 3. permanent magnet disk; 4. support; 5. gas dispersion disk; 6. air inlet; 7. nitrogen pipe; 8. discharge port; 9. liquid distributor; 10. liquid inlet; 11. oxalic acid inlet; 201. motor; 202. reducer; 203. linkage shaft; 204. stirring shaft; 205. stirring paddle; 206. jacket. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0019] Example 1

[0020] As Figures 1 - 3As shown in the figure, the utility model provides an integrated reaction device for producing ferrous oxalate, which is characterized by comprising a reaction kettle body 2, and a jacket 206 is arranged outside the reaction kettle body 2; a jacket inlet and a jacket outlet are arranged on the jacket (206). Media such as steam or hot water can be introduced into the jacket to provide heat source for the reaction.

[0021] A ferrous powder inlet 1, an exhaust port, a temperature measuring port, an oxalic acid inlet 11 and a stirring device are arranged at the top of the reaction kettle body 2. The stirring device comprises a motor 201, a speed reducer 202, a linkage shaft 203, a stirring shaft 204 and a stirring paddle 205; the motor 201 is a variable frequency motor. Stirring drives the required flow state of the precipitate and the solution in the kettle to form a liquid. Since the particle size of the ferrous oxalate precipitate is small and viscous, it is necessary to mix the solution regularly during the reaction process to fully carry out the reaction. During the discharging process, it is necessary to fully mix the ferrous oxalate precipitate solution before discharging for the next operation to ensure the stable operation of the reaction.

[0022] Inside the reactor body 2, a liquid distributor 9, a permanent magnet disk 3, and a gas dispersion disk 5 are provided. An air inlet 6 is provided at the bottom of the reactor body 2. The permanent magnet disk 3 is arranged above the gas dispersion disk 5 through a bracket 4. The liquid distributor 9 is arranged above the permanent magnet disk 3 and is connected to a liquid inlet 10 outside the reactor body 2 through a pipeline. An outlet 8 is provided at the lower part of the side of the reactor body 2. The permanent magnet disk 3 is of a C-shaped structure and is wrapped by a corrosion-resistant non-metallic outer layer. It is set as a C-shaped structure to facilitate the removal of the permanent magnet disk for cleaning without disassembling the stirring device. Liquid channels are provided on the permanent magnet disk 3. The purpose of the liquid channels is to make the liquid in the kettle mix evenly with a consistent concentration, facilitate the rapid mixing of the solution and precipitate in the upper and lower parts of the permanent magnet disk during the stirring process, prevent the ferrous oxalate precipitate from covering the iron powder, and ensure a wide contact area between the iron powder and the liquid. The purpose of using a permanent magnet is to adsorb the iron powder entering the reactor body on the permanent magnet disk, so that it can always remain in the supernatant and continuously participate in the reaction. The gas dispersion disk 5 is of an internal cavity structure made of polytetrafluoroethylene. Round holes are provided at the outlet end of the gas dispersion disk 5 to connect the internal cavity of the gas dispersion disk 5 with the inside of the reactor. The inlet end of the gas dispersion disk 5 is connected to a nitrogen pipe 7 outside the reactor body 2 through a pipeline. The liquid distributor 9 is of an umbrella-shaped disk structure. The liquid distributor is set as an umbrella-shaped disk structure and is provided with round holes. The purpose is to disperse the pressure of the liquid input into the reactor body from the liquid inlet, prevent the liquid water column from washing off the iron powder on the permanent magnet disk, resulting in the iron powder being covered by the ferrous oxalate precipitate and unable to participate in the reaction normally, leading to a decrease in the yield. When iron powder reacts with sulfuric acid, a large amount of hydrogen gas is generated. Nitrogen is introduced into the bottom of the reactor body to displace hydrogen gas, and at the same time, the precipitate at the bottom of the reactor is agitated. The iron powder that has lost magnetism and precipitated at the bottom will be covered by the continuously generated ferrous oxalate precipitate, contact the acidic liquid to participate in the reaction to generate ferrous sulfate, and the large area of the gas dispersion disk can agitate most of the ferrous oxalate precipitate at the bottom of the reactor body.

[0023] Another embodiment is different from Embodiment 1 in that: the gas dispersion disk 5 is of an internal cavity structure made of polypropylene.

[0024] Working principle of the utility model: The utility model adsorbs iron powder by adding a permanent magnet disk to keep the iron powder in the upper clear liquid, ensuring a wide contact area with the liquid, enabling the iron powder to react fully, and thus reducing the amount of iron powder used; oxalic acid is used to promote the forward reaction; and the C-shaped permanent magnet disk is convenient for disassembly and maintenance without disassembling the stirring shaft; since the particles of ferrous oxalate precipitate are small and easy to aggregate and difficult to disperse, the utility model is provided with a gas dispersion disk to continuously churn and stir the precipitate in a large area from the bottom by nitrogen, ensuring that the precipitated iron powder contacts the liquid and continues to participate in the reaction, avoiding the iron powder that loses magnetism during the reaction being covered by the continuously produced ferrous oxalate precipitate and unable to participate in the reaction normally; it can also displace hydrogen inside the reactor body, thereby also improving the purity of ferrous oxalate. This device can realize the continuous production of ferrous oxalate using iron powder in a reaction equipment, reduce the investment in reaction equipment and the consumption of iron powder raw materials, and can operate continuously, safely and efficiently.

[0025] The operation process of the utility model is as follows:

[0026] As Figures 1 - 3 shown, when feeding materials for the first time in this embodiment, a liquid inlet 7 is arranged on the side of the reactor body 2, and the liquid inlet 7 is connected to a liquid distribution disk 8. The liquid distribution disk 8 evenly disperses sulfuric acid liquid with a certain concentration into the reactor body 2 to reach the controlled liquid level of the reactor; a certain amount of iron powder is added into the reactor body 2 from the iron powder inlet 1 at the top of the reactor body 2 according to a certain proportion; a certain amount of oxalic acid is added into the reactor body 2 from the oxalic acid inlet 11 at the top of the reactor body 2 according to a certain proportion; the iron powder enters the reactor body 2 and is adsorbed by the permanent magnet disk 3. After starting the stirring device and reacting the iron powder with sulfuric acid for a certain time, solid oxalic acid is added, and then the operation of the stirring device is stopped. During the reaction of oxalic acid with ferrous sulfate, ferrous oxalate precipitate and sulfuric acid are continuously generated. Since the iron powder is adsorbed on the permanent magnet disk 3, it can ensure that the iron powder is always in the upper acidic clear liquid for continuous reaction to generate ferrous sulfate, and the ferrous sulfate continues to react with oxalic acid, and ferrous oxalate precipitate is continuously generated to ensure the continuous and stable operation of the reaction; nitrogen is introduced into the gas dispersion disk 5 connected to the air inlet 6, and the precipitate at the bottom of the reactor body 2 is churned, so that the precipitated iron powder at the bottom contacts the liquid and participates in the reaction; the stirring device is started to mix the ferrous oxalate solution evenly, and it is discharged through the discharge port 8 and enters the subsequent process section.

[0027] The above is only an embodiment of the utility model and does not impose any formal limitation on the utility model.

Claims

1. An integrated reaction device for producing ferrous oxalate, characterized in that, It includes a reactor body (2), a jacket (206) is arranged outside the reactor body (2), the jacket (206) is provided with a jacket inlet and a jacket outlet, a iron powder inlet (1), an exhaust port, a temperature measuring port, an oxalic acid inlet (11) and a stirring device are arranged at the top of the reactor body (2), and the stirring device includes a motor (201), a reducer (202), a linkage shaft (203), a stirring shaft (204) and a stirring paddle (205); a liquid distributor (9), a permanent magnet disk (3) and a gas dispersion disk (5) are arranged inside the reactor body (2), an air inlet (6) is arranged at the bottom of the reactor body (2), and the permanent magnet disk (3) is arranged above the gas dispersion disk (5) through a bracket (4); the liquid distributor (9) is arranged above the permanent magnet disk (3) and is communicated with a liquid inlet (10) outside the reactor body (2) through a pipeline, and a discharge port (8) is arranged at the lower part of the side surface of the reactor body (2).

2. The integrated reaction equipment for producing ferrous oxalate according to claim 1, characterized in that, The motor (201) is a variable frequency motor.

3. The integrated reaction equipment for producing ferrous oxalate according to claim 1, characterized in that, The permanent magnet disk (3) is of a C-shaped structure, and a liquid channel is arranged on the permanent magnet disk (3).

4. The integrated reaction equipment for producing ferrous oxalate according to claim 1, characterized in that, The permanent magnet disk (3) is wrapped by a corrosion-resistant non-metallic outer layer.

5. The integrated reaction equipment for producing ferrous oxalate according to claim 1, wherein, The gas dispersion disk (5) is of an internal cavity structure made of polytetrafluoroethylene or polypropylene, a round hole is arranged at the outlet end of the gas dispersion disk (5) to communicate the internal cavity of the gas dispersion disk (5) with the inside of the reactor, and the inlet end of the gas dispersion disk (5) is communicated with a nitrogen pipe (7) outside the reactor body (2) through a pipeline.

6. The integrated reaction equipment for producing ferrous oxalate according to claim 1, wherein The liquid distributor (9) is of an umbrella-shaped disk structure.

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