Water immersion liquid neutralization production equipment for rare earth production

Abstract

The utility model discloses water immersion liquid neutralization production equipment for rare earth production, particularly relates to the technical field of water immersion liquid neutralization, and comprises a microchannel reactor, and a secondary diaphragm reactor is fixedly connected with a surface filter through a pipeline. The rare earth neutralization liquid reactor is composed of the micro-channel reactor, the first-stage diaphragm reactor, the second-stage diaphragm reactor and the surface filter, rare earth feed liquid and magnesium oxide slurry are both provided with buffer tanks and then pumped into the micro-channel reactor through the electric diaphragm pump, the flow of the rare earth feed liquid is not changed, the flow of the magnesium oxide slurry is adjusted to adjust the pH value, and the surface filter is arranged on the surface of the micro-channel reactor. In order to ensure the scientificity of the experiment, a sampling valve and a pressure gauge are arranged at the rear end of each stage of equipment, the experiment equipment is optimized and improved while the experiment is analyzed in time through experiment feedback data, and after a series of continuous experiments, the pH of the rear end of each stage of equipment is stable and controllable. The occupied area is small, a large number of stirring devices are not needed, the reaction is continuously and automatically controlled, the intelligent degree is high, and the labor cost is low.

Description

Technical Field

[0001] The utility model relates to the technical field of water leaching liquid neutralization, in particular to a production device for neutralizing water leaching liquid in rare earth production. Background Art

[0002] At present, domestic rare earth enterprises mostly use magnesium oxide slurry and rare earth sulfate for neutralization reaction and then filter by plate and frame filter press to remove some heavy metal ions. In this process, the pH value after the reaction needs to be controlled to ensure the precipitation of metal ions, so as to facilitate the subsequent filtration. A large number of stirring tanks are required in the production process, which has the disadvantages of large floor space, high energy consumption, and slow reflection efficiency.

[0003] Therefore, we have made improvements on this and proposed a rare earth production water leaching neutralization production equipment. Utility Model Content

[0004] In order to solve the above technical problems, the utility model provides the following technical solutions:

[0005] The utility model discloses a rare earth production water leaching neutralization production equipment, comprising a microchannel reactor, the microchannel reactor is connected with a primary diaphragm reactor through a pipeline, the primary diaphragm reactor is provided with two groups, the two groups of primary diaphragm reactors are fixedly connected with a secondary diaphragm reactor through a pipeline, and the secondary diaphragm reactor is fixedly connected with a surface filter through a pipeline.

[0006] As a preferred technical solution of the utility model, two groups of first-level diaphragm reactors include a first-level diaphragm reactor and a second-level diaphragm reactor, and the first-level diaphragm reactor and the second-level diaphragm reactor are fixedly connected with a distribution pipe, and the discharge ends of the distribution pipes are connected to the second-level diaphragm reactor.

[0007] As a preferred technical solution of the utility model, a connecting valve is fixedly connected to the microchannel reactor, and the connecting valve is fixedly connected to the feed end of the distribution pipe.

[0008] As a preferred technical solution of the utility model, a rare earth liquid feed inlet is fixedly connected to one side of the top of the microchannel reactor, and a magnesium oxide slurry feed inlet is fixedly connected to the other side of the rare earth liquid feed inlet.

[0009] As an optimal technical solution of the utility model, a buffer tank is arranged above the rare earth liquid feed port and the magnesium oxide slurry feed port, and an electric diaphragm pump is fixedly connected to the inside of the buffer tank, and the electric diaphragm pump is arranged above the rare earth liquid feed port and the magnesium oxide slurry feed port.

[0010] As a preferred technical solution of the utility model, the ends of the microchannel reactor, the first level diaphragm reactor, the second level diaphragm reactor, the second level diaphragm reactor and the surface filter are fixedly connected with sampling valves and pressure gauges.

[0011] The beneficial effect of the utility model is as follows: In the utility model, a series of experiments were carried out using the rare earth liquid and magnesium oxide slurry currently provided by the factory as raw materials and the rare earth neutralization liquid reactor developed by our company, wherein the rare earth liquid and magnesium oxide slurry were taken from the workshop. The rare earth neutralization liquid reactor consists of a microchannel reactor, a primary diaphragm reactor, a secondary diaphragm reactor and a surface filter. In order to ensure the stability and repeatability of the experiment, the rare earth liquid and magnesium oxide slurry are both provided with a buffer tank, and then pumped to the microchannel reactor via an electric diaphragm pump, wherein the rare earth liquid flow remains unchanged, and the magnesium oxide slurry flow is adjusted to adjust the pH value. In order to ensure the scientific nature of the experiment, a sampling valve and a pressure gauge are provided at the rear end of each level of equipment, so as to timely analyze the experiment through the experimental feedback data while optimizing and improving the experimental equipment. After a series of continuous experiments, the pH at the rear end of each level of equipment is stable and controllable. It occupies a small area, does not require a large number of stirring devices, the reaction is continuously automatically controlled, has a high degree of intelligence, and has low labor costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] The accompanying drawings are used to provide a further understanding of the present invention and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention and do not constitute a limitation of the present invention. In the accompanying drawings:

[0013] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0014] Figure 2 It is the experimental data table of this utility model;

[0015] Figure 3 It is a schematic diagram of the utility model process.

[0016] In the figure: 10, microchannel reactor; 101, rare earth liquid feed port; 102, magnesium oxide slurry feed port; 20, first level diaphragm reactor; 30, second level diaphragm reactor; 40, second level diaphragm reactor; 50, surface filter; 70, distribution pipe. DETAILED DESCRIPTION

[0017] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0018] Example: Figures 1 to 3As shown, the utility model is a rare earth production water leaching neutralization production equipment, including a microchannel reactor 10, the microchannel reactor 10 is connected to a primary diaphragm reactor through a pipeline, the primary diaphragm reactor is provided with two groups, the two groups of primary diaphragm reactors are fixedly connected to a secondary diaphragm reactor 40 through a pipeline, and the secondary diaphragm reactor 40 is fixedly connected to a surface filter 50 through a pipeline.

[0019] By feeding the rare earth feed liquid and the magnesium oxide slurry into the microchannel reactor 10 and then utilizing its efficient heat transfer and mixing performance, the microchannel reactor 10 can achieve sufficient mixing of the rare earth feed liquid and the magnesium oxide slurry.

[0020] The two groups of primary diaphragm reactors include a first primary diaphragm reactor 20 and a second primary diaphragm reactor 30. Both the first primary diaphragm reactor 20 and the second primary diaphragm reactor 30 are fixedly connected with a feed distribution pipe 70, and the discharge ends of the feed distribution pipe 70 are connected to the secondary diaphragm reactor 40.

[0021] A connecting valve is fixedly connected to the microchannel reactor 10 , and the connecting valve is fixedly connected to the feed end of the material distribution pipe 70 .

[0022] A rare earth liquid feed inlet 101 is fixedly connected to one side of the top of the microchannel reactor 10, and a magnesium oxide slurry feed inlet 102 is fixedly connected to the other side of the rare earth liquid feed inlet 101. Buffer tanks are arranged above the rare earth liquid feed inlet 101 and the magnesium oxide slurry feed inlet 102, and an electric diaphragm pump is fixedly connected inside the buffer tank, and the electric diaphragm pump is arranged above the rare earth liquid feed inlet 101 and the magnesium oxide slurry feed inlet 102.

[0023] By setting the rare earth liquid feed inlet 101 and the magnesium oxide slurry feed inlet 102 at the top of the microchannel reactor 10, it is easier to add the initial raw materials. At the same time, by using the buffer tanks set above the rare earth liquid feed inlet 101 and the magnesium oxide slurry feed inlet 102, the stability and repeatability of the experiment can be further guaranteed, making it more convenient to use.

[0024] The ends of the microchannel reactor 10, the first primary membrane reactor 20, the second primary membrane reactor 30, the secondary membrane reactor 40 and the surface filter 50 are all fixedly connected with sampling valves and pressure gauges.

[0025] By using sampling valves and pressure gauges at the back end of each stage of equipment, the scientific nature of the experiment can be further guaranteed, and the experimental equipment can be optimized and improved while timely analyzing the experiment through experimental feedback data. After a series of continuous experiments, the pH at the back end of each stage of equipment is stable and controllable.

[0026] During operation: 1. Rare earth liquid and magnesium oxide slurry are pumped into the microchannel reactor for full mixing, and then fully reacted through the secondary diaphragm reactor.

[0027] 2. A pH meter is set at the end point to provide real-time feedback to the control system to adjust the frequency of the variable frequency pump to feed liquid, thereby achieving automatic control of the system.

[0028] 3. The pH stability of the effluent can be ensured by adding a multi-stage diaphragm reactor or a stirring tank at the back end.

[0029] Take the experimental data table as an example:

[0030] Rare earth liquid = rare earth solution = lanthanum cerium liquid (ReCl3 (RE = La, Ce)); seed slurry = seed solution (Rex (CO3) y (RE = La, Ce)) which is also the product of the reaction; seed bottom water = tap water; ammonium carbonate = ammonium bicarbonate solution

[0031] (1) First, 267.04 (g / L) of ammonium carbonate solution and 100 (g / L) of seed slurry (rare earth carbonate solution (lanthanum, cerium)) are fully mixed by a high-efficiency mixer. Only mixing is performed. The seed slurry here is the product reflux at the back end of the overall process.

[0032] (2) The rare earth solution used needs to be diluted to 100 g / L before use due to its high concentration. The clear liquid from the belt filter is used as a diluent to dilute the original concentration of 310 g / L to 100 g / L.

[0033] (3) The ammonium carbonate mixed solution (ammonium carbonate + seed crystals in step 1) and the rare earth solution are then simultaneously introduced into the primary carbon precipitation microchannel reactor for reaction. The dosage here is distributed in proportion of m ammonium carbonate: m rare earth feed solution = 1.5:1 (detailed data: ammonium carbonate solution: added continuously at a flow rate of 120 L / h for 5 min; rare earth feed solution: added continuously at a flow rate of 300 L / h for 5 min; seed slurry: 12 L, added within 3 min, ammonium carbonate + seed crystals have been mixed in step 1, only detailed data is reflected here), the flow rate is controlled by a regulating valve, and the pH value is detected to be about 5-6. The reacted liquid is then fully mixed in the diaphragm reactor before entering the primary negative pressure crystallizer.

[0034] (4) An ultrasonic device is installed in the negative pressure crystallizer to accelerate the reaction through vibration and enhance the reaction effect. A large amount of CO2 is discharged during the reaction. An exhaust port is provided on the top, which can be quickly discharged through a fan to maintain the stability of the product.

[0035] (5) According to experiments, the ammonium carbonate solution needs to be added at multiple points, so the liquid after the reaction enters the secondary carbon precipitation microchannel reactor, and at the same time, the ammonium carbonate solution continues to be added to the secondary carbon precipitation microchannel reactor (detailed data: continuous addition at a flow rate of 120L / h for 2min12s, at this time the measured pH is about 7, and the mixed liquid in the previous step is also added for 2min12s), and then enters the secondary negative pressure reactor through the secondary diaphragm reactor. Each negative pressure crystallization tank is equipped with a pH meter, and the amount of ammonium carbonate added is controlled by the pH, and the end pH is about 7.

[0036] (6) The liquid out of the secondary negative pressure crystallizer enters the stirring tank to consolidate the crystal shape again to meet the design requirements and enter the later stage of the process.

[0037] The 3-minute seed solution addition time is only experimental data. The actual situation should be consistent with the ammonium carbonate addition time, which should be changed to 5 minutes so that the seed solution enters the primary microchannel simultaneously with the ammonium carbonate.

[0038] The experimental design is a continuous reaction, with continuous addition and continuous output.

[0039] Experimental process: 1. Dilute the on-site lanthanum-cerium liquid to 31g / L, add seed slurry as bottom water in the reaction tank according to the proportion, add appropriate amount of seed slurry during the reaction, and slowly add ammonium carbonate solution. The reaction lasts for 5 minutes, and stirring is continuous during the reaction. After the addition of materials is completed, stirring is continued for 10 minutes. After the stirring is completed, the precipitate in the solution settles slowly, and the solid-liquid separation is not obvious, and the experiment is judged to have failed.

[0040] 2. Maintain the concentration of the lanthanum-cerium solution at 60 g / L, use the seed slurry as the bottom water, add the lanthanum-cerium solution, all the ammonium carbonate solution, and the seed slurry at the same time during the reaction. The reaction lasts for 5 minutes, and stirring is maintained throughout the process. After the addition is completed, stirring is continued for 10 minutes. After the stirring ends, the precipitate in the solution slowly settles, and the solid-liquid separation is not obvious, and the experiment fails.

[0041] Finally, it should be noted that the above description is only a preferred embodiment of the utility model and is not intended to limit the utility model. Although the utility model is described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions recorded in the above embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. A rare earth production water leaching neutralization production equipment, comprising a microchannel reactor (10), characterized in that: The microchannel reactor (10) is connected to a primary diaphragm reactor via a pipeline, and two groups of the primary diaphragm reactors are provided. The two groups of the primary diaphragm reactors are fixedly connected to a secondary diaphragm reactor (40) via pipelines, and the secondary diaphragm reactor (40) is fixedly connected to a surface filter (50) via pipelines.

2. A rare earth production water leaching neutralization production equipment according to claim 1, characterized in that: The two groups of the first-level diaphragm reactors include a first-level diaphragm reactor (20) and a second-level diaphragm reactor (30), and the first-level diaphragm reactor (20) and the second-level diaphragm reactor (30) are fixedly connected with a distribution pipe (70), and the discharge end of the distribution pipe (70) is connected to the second-level diaphragm reactor (40).

3. A rare earth production water leaching neutralization production equipment according to claim 2, characterized in that: A connecting valve is fixedly connected to the microchannel reactor (10), and the connecting valve is fixedly connected to the feed end of the material distribution pipe (70).

4. The rare earth production water leaching neutralization production equipment according to claim 1, characterized in that: A rare earth liquid feed inlet (101) is fixedly connected to one side of the top of the microchannel reactor (10), and a magnesium oxide slurry feed inlet (102) is fixedly connected to the other side of the rare earth liquid feed inlet (101).

5. A rare earth production water leaching neutralization production equipment according to claim 4, characterized in that: A buffer tank is disposed above the rare earth liquid feed inlet (101) and the magnesium oxide slurry feed inlet (102), and an electric diaphragm pump is fixedly connected inside the buffer tank. The electric diaphragm pump is disposed above the rare earth liquid feed inlet (101) and the magnesium oxide slurry feed inlet (102).

6. A rare earth production water leaching neutralization production equipment according to claim 5, characterized in that: The ends of the microchannel reactor (10), the first primary diaphragm reactor (20), the second primary diaphragm reactor (30), the secondary diaphragm reactor (40) and the surface filter (50) are all fixedly connected with a sampling valve and a pressure gauge.

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