A high-purity manganese chloride production impurity removal device

Abstract

The utility model belongs to the production technology field of manganese chloride, disclose a kind of impurity removal device for high-purity manganese chloride production, including the acidification reaction kettle, ceramic membrane filter, oxidizing reactor, settling tank, multistage countercurrent extraction device, ion exchange column and activated carbon adsorption tower that pass through pipeline, pump and valve are sequentially communicated;The discharge port of acidification reaction kettle is communicated to the feed inlet of ceramic membrane filter, the discharge port of ceramic membrane filter is communicated to the feed inlet of oxidizing reactor, the discharge port of oxidizing reactor is communicated to the feed inlet of settling tank, the discharge port of settling tank is communicated to the feed inlet of multistage countercurrent extraction device, the discharge port of multistage countercurrent extraction device is communicated to the feed inlet of ion exchange column, the discharge port of ion exchange column is communicated to the feed inlet of activated carbon adsorption tower.The utility model can effectively remove the impurity in manganese chloride raw material liquid, guarantee the purity of manganese chloride product, so that product can satisfy the manufacturing requirement of high-end product.

Description

Technical Field

[0001] This utility model relates to the field of manganese chloride production technology, specifically to a purification device for the production of high-purity manganese chloride. Background Technology

[0002] Manganese chloride, also known as manganese sulfide or manganese dichloride, is an inorganic compound. Its molecular formula is MnCl2, and anhydrous manganese chloride appears as pinkish-red crystals. High-purity manganese chloride, due to its high purity and consistent quality, is widely used in the production of pharmaceuticals, high-quality magnesium-manganese alloys, aluminum-manganese alloys, high-purity manganese metal powder catalytic systems, and manganese-based high-efficiency gasoline antiknock agents.

[0003] Manganese chloride solid prepared by conventional methods, or manganese chloride solid prepared by conventional methods using a manganese chloride solution obtained by leaching high-purity metallic manganese with hydrochloric acid, has very high levels of Ca, Mg, and heavy metal impurities (Co, Ni, Pb, etc.). The Ca and Mg content can reach approximately 1000 ppm, and the heavy metal impurity (Fe, Co, Ni, Pb, Cd, Cr, etc.) content can reach approximately 50–500 ppm. These impurity levels are far below the requirements for battery-grade / electronic-grade raw materials (Ca... 2+ It forms slightly soluble substances in the electrolyte, reducing battery cycle life; Fe 3+ Catalytic electrolyte decomposition poses a safety hazard; Co 2+ Ni affects the conductivity of semiconductor devices. 2+ (This can lead to uneven film deposition, etc.), therefore, in order to ensure that the product can meet the manufacturing requirements of high-end products, impurities in the manganese chloride raw material solution must be removed. Summary of the Invention

[0004] The technical problem to be solved by this utility model is to provide a purification device for the production of high-purity manganese chloride, which can effectively remove impurities from the manganese chloride raw material liquid, ensure the purity of the manganese chloride product, and enable the product to meet the manufacturing requirements of high-end products.

[0005] To solve the above-mentioned technical problems, the technical solution of this utility model is as follows:

[0006] A purification device for producing high-purity manganese chloride includes an acidification reactor, a ceramic membrane filter, an oxidation reactor, a settling tank, a multi-stage countercurrent extraction device, an ion exchange column, and an activated carbon adsorption tower, which are connected in sequence via pipes, pumps, and valves. The outlet of the acidification reactor is connected to the inlet of the ceramic membrane filter, the outlet of the ceramic membrane filter is connected to the inlet of the oxidation reactor, the outlet of the oxidation reactor is connected to the inlet of the settling tank, the outlet of the settling tank is connected to the inlet of the multi-stage countercurrent extraction device, the outlet of the multi-stage countercurrent extraction device is connected to the inlet of the ion exchange column, and the outlet of the ion exchange column is connected to the inlet of the activated carbon adsorption tower.

[0007] Preferably, the feed inlet of the acidification reactor is connected to the raw material supply device via a pipeline.

[0008] Preferably, the acidification reactor is an acidification reactor equipped with a mechanical stirring device, an ultrasonic disperser, and a pH detection device. The volume is 10m³. 3 The manufacturer is Jiangsu Yangyang Chemical Equipment Manufacturing Co., Ltd.

[0009] Preferably, the ceramic membrane filter is a 0.22μm silicon carbide ceramic membrane filter. The manufacturer is Shandong Tiancan Environmental Protection Technology Co., Ltd.

[0010] Preferably, the oxidation reactor is an oxidation reactor equipped with an aeration system. The volume is 8m³. 3 The manufacturer is Shanghai Sensong Pressure Vessel Co., Ltd.

[0011] Preferably, the settling tank is also connected to a plate and frame filter press. The settling tank pumps the clarified liquid to a multi-stage countercurrent extraction device, where the settled flocculent precipitate is filtered and then further processed.

[0012] Preferably, the multi-stage countercurrent extraction device is a three-stage countercurrent extraction device. The model is CWL450-M, and the manufacturer is Zhengzhou Tianyi Extraction Technology Co., Ltd.

[0013] Preferably, the ion exchange column is a strong acid cation exchange resin column. It has dimensions of φ800mm × 3000mm and is manufactured by Jiangsu Secos Resin Co., Ltd.

[0014] Preferably, the activated carbon adsorption tower is a granular activated carbon adsorption tower, and the outlet of the activated carbon adsorption tower is connected to a vacuum concentrator evaporator in the subsequent treatment unit via a pipeline. The volume is 5m³. 3 The manufacturer is Zhejiang Xinhui New Materials Co., Ltd.

[0015] Due to the adoption of the above technical solution, the beneficial effects of this utility model are:

[0016] This invention utilizes an acidification reactor to ensure the complete dissolution of manganese and other metal ions in the raw material solution, preventing the formation of hydroxides or basic salt precipitates in the initial stage, which could lead to manganese loss or pipeline blockage. A ceramic membrane is used to separate insoluble solid particles, filter out colloids, and retain organic matter in the solution. An oxidation reactor is used to remove Fe2+, a common element in the solution that is difficult to remove through extraction. + Oxidized to Fe3 +The process involves forming a flocculent colloid of ferric hydroxide (Fe(OH)3), which adsorbs other metal ions and forms a flocculent precipitate. The solution and the flocculent precipitate are separated by a settling tank, and the solution is then transported to a multi-stage countercurrent extraction device to remove most of the heavy metal impurity ions remaining in the aqueous phase (raffinate). Then, trace amounts of cationic impurities are removed by an ion exchange column, and trace amounts of organic impurities are removed by an activated carbon adsorption tower, thus obtaining a high-purity manganese chloride product. Attached Figure Description

[0017] Figure 1 This is a flowchart of an embodiment of the present utility model. Detailed Implementation

[0018] The present invention will be further described below with reference to the accompanying drawings and embodiments.

[0019] like Figure 1 As shown, a purification device for the production of high-purity manganese chloride includes an acidification reactor, a ceramic membrane filter, an oxidation reactor, a settling tank, a multi-stage countercurrent extraction device, an ion exchange column, and an activated carbon adsorption tower, which are connected in sequence by pipes, pumps, and valves. The outlet of the acidification reactor is connected to the inlet of the ceramic membrane filter, the outlet of the ceramic membrane filter is connected to the inlet of the oxidation reactor, the outlet of the oxidation reactor is connected to the inlet of the settling tank, the outlet of the settling tank is connected to the inlet of the multi-stage countercurrent extraction device, the outlet of the multi-stage countercurrent extraction device is connected to the inlet of the ion exchange column, and the outlet of the ion exchange column is connected to the inlet of the activated carbon adsorption tower.

[0020] In actual production, the raw material solution obtained from the previous process first enters the acidification reactor to adjust the pH to 1.5-2.0, ensuring that manganese and other metal ions in the solution are completely dissolved. Then, the solution is conveyed to a ceramic membrane filter, where cross-flow filtration is performed using the dense micropores on the ceramic membrane surface to separate insoluble solid particles from the solution. These substances include suspended solids (SS), colloids, diatomaceous earth, CaSO4·2H2O microcrystals, silt, and all other tiny solid particles insoluble in acid. The resulting clarified manganese-containing solution is then conveyed to the oxidation reactor, where hydrogen peroxide is used to oxidize iron ions, generating ferric hydroxide precipitate (a flocculent colloid with extremely strong adsorption properties). This precipitate adsorbs aluminum ions (Al3+) from the solution. + The oxidized material contains some arsenic (As) and residual trace suspended solids. After oxidation, the material enters a settling tank for separation. The flocculent precipitate is then filtered in a plate and frame filter press for further processing. The resulting clarified liquid is then fed into a multi-stage countercurrent extraction unit to remove most of the heavy metal impurities remaining in the aqueous phase (raffinate), such as copper (Cu2+). + ), cobalt (Co2) + ), nickel (Ni 2+ ), Zinc (Zn2) + ), lead (Pb)2+ ), cadmium (Cd 2+ The purified manganese chloride solution, obtained through back-extraction (using a back-extraction agent to rediscover manganese from the organic phase to the aqueous phase), is then fed into an ion exchange column for further removal of trace heavy metal ions and alkaline earth metal ions (Ca2+). + Mg2 + Then, an activated carbon adsorption tower is used to remove trace organic impurities, such as oil residues from the extractant, decomposition products of additives, and bacterial metabolites, to obtain a high-purity manganese chloride solution. Through subsequent processes such as vacuum concentration, spray drying, vacuum rotary drying, and finished product packaging, a high-purity manganese chloride product is obtained.

[0021] It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

Claims

1. A purification device for the production of high-purity manganese chloride, characterized in that: The system includes an acidification reactor, a ceramic membrane filter, an oxidation reactor, a settling tank, a multi-stage countercurrent extraction device, an ion exchange column, and an activated carbon adsorption tower, which are connected sequentially via pipes, pumps, and valves. The outlet of the acidification reactor is connected to the inlet of the ceramic membrane filter, the outlet of the ceramic membrane filter is connected to the inlet of the oxidation reactor, the outlet of the oxidation reactor is connected to the inlet of the settling tank, the outlet of the settling tank is connected to the inlet of the multi-stage countercurrent extraction device, the outlet of the multi-stage countercurrent extraction device is connected to the inlet of the ion exchange column, and the outlet of the ion exchange column is connected to the inlet of the activated carbon adsorption tower.

2. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The feed inlet of the acidification reactor is connected to the raw material supply device via a pipeline.

3. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The acidification reactor is equipped with a mechanical stirring device, an ultrasonic disperser, and a pH detection device.

4. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The ceramic membrane filter is a silicon carbide ceramic membrane filter.

5. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The oxidation reactor is an oxidation reactor equipped with an aeration system.

6. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The settling tank is also connected to a plate and frame filter press.

7. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The multi-stage countercurrent extraction device is a three-stage countercurrent extraction device.

8. The impurity removal device for high-purity manganese chloride production as described in claim 1, characterized in that: The ion exchange column is a strongly acidic cation exchange resin column.

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