Preparation method and preparation system of rod-like nano-manganese dioxide by taking manganese ore leachate as raw material

Abstract

The invention provides a preparation method and a preparation system of rodlike nano-manganese dioxide by taking manganese ore leachate as a raw material. The preparation method comprises the following steps that manganese oxide ore powder and a reducing agent are subjected to a leaching reaction in a sulfuric acid solution, and manganese oxide ore leaching liquid is obtained; adding hydrogen peroxide, manganese carbonate and potassium sulfate, and carrying out oxidation reaction at 90 DEG C to obtain filtrate; fixing the volume of the filtrate, adding potassium permanganate, and carrying out stirring reaction at 85 DEG C to obtain a target mixed solution; and carrying out suction filtration and drying treatment on the target mixed solution to obtain the rod-like nano manganese dioxide. The preparation system comprises a leaching reaction module, an oxidation reaction module and a retreatment module which are used for achieving all the steps, by optimizing the technological process and the system structure, the preparation efficiency is improved, the operation complexity is reduced, the raw material cost and the energy consumption cost are reduced, and the method is suitable for large-scale production of the rod-shaped nano manganese dioxide.

Description

Technical Field

[0001] The invention relates to the technical field of inorganic chemical industry, and in particular to a system for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as a raw material. Background Art

[0002] With the gradual consumption and exhaustion of petrochemical resources, clean energy materials have become a research hotspot in the field of materials. Nano manganese dioxide is widely used in supercapacitors and other fields due to its superior electrochemical properties and low cost. In existing studies, most analytically pure manganese salts: manganese chloride, manganese sulfate or potassium permanganate are used as raw materials to prepare nano manganese dioxide by hydrothermal synthesis, microwave radiation and other methods. However, the cost of analytically pure reagents is high, the preparation method is complicated and the energy consumption is large. In order to solve this problem, the present invention proposes a new method for preparing nano manganese dioxide, using common manganese ores in nature: manganese oxide ore or manganese carbonate ore as raw materials, and obtaining a mixed solution mainly composed of manganese sulfate solution by smelting. After the solution is treated with iron removal and filtration, an oxidant: permanganate, chromate or ammonium nitrate is directly added to carry out redox reaction, and a rod-shaped nano manganese dioxide material is synthesized in situ. This method not only reduces the cost of raw materials, but also simplifies the preparation process, and has higher economy and operability.

[0003] This experimental team has been browsing and studying a large number of relevant records and materials on the relevant technologies for the preparation of manganese dioxide for a long time. At the same time, relying on relevant resources and conducting a large number of relevant experiments, after a large number of searches, it was found that the existing prior art, such as CN113088997B, CN107265505B, CN103153870B, and CN116605910B disclosed in the prior art, is a method for preparing high-purity manganese dioxide disclosed in the prior art, which has the following steps: selecting pyrolusite, mixing it with coal powder after crushing, beneficiation, and impurity removal, and reducing and roasting to obtain manganese monoxide; leaching the product with nitric acid solution, filtering and purifying to obtain manganese nitrate solution; concentrating the product, and using a continuous pyrolysis device to pyrolyze the manganese nitrate concentrate to obtain manganese dioxide, and the continuous pyrolysis device can collect by-product nitrogen oxides; inputting it into a post-processing device, refining it with nitric acid, activating it with sulfuric acid, washing it with water, and drying it to obtain a high-purity manganese dioxide product; treating the by-product nitrogen oxides to obtain a nitric acid solution for recycling. The continuous pyrolysis device can continuously process manganese nitrate concentrate, improve the thermal decomposition efficiency and effectively collect nitrogen oxide by-products. The post-treatment device can continuously purify, activate and wash manganese dioxide.

[0004] The present invention is made to solve the common problems in the art, such as high raw material cost, complex preparation process, high energy consumption, serious environmental pollution, etc. Summary of the invention

[0005] The purpose of the present invention is to address the deficiencies in the current art and to propose a rod-shaped nano manganese dioxide preparation system using manganese ore leaching solution as a raw material.

[0006] In order to overcome the shortcomings of the prior art, the present invention adopts the following technical solutions:

[0007] A method for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as a raw material, the method comprising:

[0008] Step 1: taking manganese oxide ore powder and a reducing agent to carry out a leaching reaction in a sulfuric acid solution, the leaching temperature is 90° C., the time is 2 hours, and after the leaching reaction is completed, the solid-liquid separation is carried out to obtain a manganese oxide ore leachate, wherein the reducing agent includes sodium thiosulfate, walnut shells, glucose or iron powder;

[0009] Step 2: Take the manganese oxide ore leachate, add 36% hydrogen peroxide by mass, add manganese carbonate to adjust the pH to 2.5-3.5, add potassium sulfate, and perform oxidation reaction at 90° C. for 2 hours. After the reaction is completed, filter to obtain a filtrate, wherein the hydrogen peroxide is 2% by volume of the manganese oxide ore leachate, and the amount of potassium sulfate is 10% by mass of the manganese oxide ore leachate;

[0010] Step 3: After the filtrate is cooled, deionized water is gradually added to dilute the filtrate to 2.5 times of the original volume to obtain a fixed volume solution, and potassium permanganate is gradually added to the fixed volume solution according to a molar ratio of manganese to potassium permanganate of 3:2 in the fixed volume solution, and stirred at 85°C and 200 r / min for 4 hours. After the reaction is completed, the target mixed solution is obtained, and the target mixed solution is filtered to obtain a black powdery solid, wherein the molar number of manganese in the fixed volume solution is obtained by atomic absorption spectrometry, redox titration or inductively coupled ion emission spectrometry;

[0011] Step 4: Dry the black powdery solid at 60° C. for 3 h to obtain rod-shaped nano manganese dioxide.

[0012] A preparation system for realizing the preparation method of rod-shaped nano manganese dioxide, comprising a leaching reaction module for receiving manganese oxide ore powder and a reducing agent in a sulfuric acid solution for leaching reaction, an oxidation reaction module for carrying out oxidation reaction on the manganese oxide ore leachate with hydrogen peroxide, manganese carbonate and potassium sulfate, and a reprocessing module for adding potassium permanganate to the filtrate to obtain a target mixed solution and continuing to filter the target mixed solution to obtain a black powdery solid and drying the black powdery solid to obtain rod-shaped nano manganese dioxide.

[0013] Furthermore, the reprocessing module includes a reaction vessel with an open top structure, a liquid level sensor for monitoring the liquid level in the reaction vessel, a supporting base plate fixed around the outer wall of the reaction vessel, a sealing cover for covering the opening at the top of the reaction vessel, a movable opening arranged in the middle of the sealing cover, a rotating shaft arranged vertically through the movable opening, a stirring blade sleeved on the rotating shaft, a driving motor connected to the top of the rotating shaft through a coupling, a fixed base for fixing the top of the driving motor, a plurality of electric push rods respectively fixedly connected to the fixed base at the top and fixedly connected to the sealing cover at the bottom, a driving mechanism for driving the sealing cover to close the reaction vessel, a heating strip evenly laid on the outer wall of the reaction vessel, and a filtration unit for filtration treatment of the target mixed liquid in the reprocessing module.

[0014] The reaction vessel is a cubic structure, and the electric push rod is used to drive the fixed base to move up and down relative to the sealing cover, thereby synchronously driving the stirring shaft and the stirring blade to move up and down in the reaction vessel.

[0015] Furthermore, the driving mechanism includes a plurality of telescopic driving rods, one end of which is fixed to the sealing cover through a corresponding fixing piece and the other end of which is fixed to the supporting base plate through a fixing seat.

[0016] Furthermore, the filtration unit includes a plurality of through ports respectively arranged at the top of the sealing cover, through pipes arranged to penetrate the through ports in sequence, pumps respectively arranged to be connected to the through pipes, a suction component arranged to be connected to the bottom of the through pipes, a transfer port arranged on the side wall of the reaction vessel, a matching door that can be airtightly matched with the transfer port, a door handle arranged on the matching door, an intercepting component matched to the bottom of the reaction vessel and partially fixed to the matching door, a discharge port respectively arranged at the bottom of the reaction vessel, an electrically controlled closing valve for controlling the closing of the discharge port, a discharge pipe for driving the liquid phase of the target mixed liquid in the reaction vessel to be discharged from the discharge port, and a filtration pump respectively arranged to be connected to the discharge pipe.

[0017] Furthermore, the suction component includes a vertically arranged plate body, a cavity arranged inside the plate body, suction holes evenly distributed on the outer wall of the plate body and capable of communicating with the cavity, and an interface arranged on the top of the plate body and communicating with the cavity. The through pipe and the interface are airtightly connected by welding, threading or flange connection.

[0018] Furthermore, the outer layer of the plate body is provided with a filter element adapted to the shape of the plate body and a fixing clamp for reinforcing and fixing the filter element to the outside of the plate body. The filter element has an open bag-like structure, and the filter elements can be sequentially sleeved onto the plate body from the bottom of the plate body. The filter element is obtained by cutting and hot-pressing disposable filter paper or multi-layer composite filter membrane.

[0019] Furthermore, the intercepting component includes a collecting dish adapted to the bottom of the reaction dish, the bottom wall of the collecting dish is provided with a bottom opening for discharging the liquid phase, the side wall of the collecting dish is provided with a side opening, and filter sheets are respectively installed at the bottom opening and the side opening, the filter sheets intercept the solids of the target reaction liquid to ensure that the liquid phase is smoothly discharged from the reaction dish.

[0020] The beneficial effects achieved by the present invention are:

[0021] 1. The method for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as raw material of the present invention replaces the traditional high-cost analytical pure manganese salt raw material with manganese oxide ore powder, providing an innovative solution for the industrial production of rod-shaped nano manganese dioxide. At the same time, by using iron powder, walnut shell or glucose as a cheap and readily available reducing agent, the production cost of nano manganese dioxide is significantly reduced, providing feasibility for large-scale industrial production.

[0022] 2. The rod-shaped nano manganese dioxide preparation system of the present invention independently realizes the leaching reaction, oxidation reaction and reprocessing through a dedicated reaction tank and a reprocessing module, thereby avoiding cross-interference between reactions, thereby improving the reaction efficiency and process controllability, and improving the preparation purity and efficiency of rod-shaped nano manganese dioxide.

[0023] 3. The preparation system of the present invention realizes the preparation of the target mixed liquid, the filtration and drying of the black powdery solid through the integration of the reaction vessel. Combined with the sliding structure, the filter element fixing system and the airtight connection design of the high-precision limit groove and the sealing strip, the operation process from reaction to drying is completely closed and efficient, avoiding the complexity and efficiency loss caused by switching of multiple devices. At the same time, the convenient design of the door and the locking buckle further improves the reliability and ease of operation of the overall system, and improves the efficiency of the preparation of rod-shaped nano manganese dioxide. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The present invention can be further understood from the following description in conjunction with the accompanying drawings. The components in the figures are not necessarily drawn to scale, but the emphasis is placed on illustrating the principles of the embodiments. In different views, the same reference numerals designate corresponding parts.

[0025] Figure 1 This is a structural electron microscope image of the rod-shaped nano manganese dioxide obtained by using sodium thiosulfate as a reducing agent in the present invention when magnified 304200 times.

[0026] Figure 2 This is a structural electron microscope image of the rod-shaped nano manganese dioxide obtained by using walnut shell as a reducing agent of the present invention when magnified 304200 times.

[0027] Figure 3This is a structural electron microscope image of the rod-shaped nano manganese dioxide obtained by using iron powder as a reducing agent of the present invention when magnified 303130 times.

[0028] Figure 4 This is a structural electron microscope image of the rod-shaped nano manganese dioxide obtained by using glucose as a reducing agent of the present invention when magnified 301050 times.

[0029] Figure 5 It is a partial structural schematic diagram of the reprocessing module of the present invention.

[0030] Figure 6 This is another partial structural schematic diagram of the reprocessing module of the present invention.

[0031] Figure 7 It is a partial structural schematic diagram of the filter clamp of the present invention.

[0032] Figure 8 It is another partial structural schematic diagram of the filter clamp of the present invention.

[0033] Explanation of the accompanying numbers: 1-reaction dish; 2-intercepting component; 3-matching door; 4-stirring blade; 5-rotating shaft; 6-supporting base plate; 7-coupling; 8-electric push rod; 9-through tube; 10-driving motor; 11-fixed base; 12-telescopic driving rod; 13-drain pipe; 14-suction component; 15-sealing cover; 16-collecting dish; 17-side opening; 18-sliding structure; 19-door handle; 20-plate body; 21-filter element; 22-male clamp; 23-female clamp. DETAILED DESCRIPTION

[0034] In order to make the purpose, technical solutions and advantages of the present invention clearer, the present invention is further described in detail in combination with its embodiments below; it should be pointed out that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present case. For those skilled in the art, after reviewing the following detailed description, other systems, methods and / or features of this embodiment will become apparent. And the terms describing the positional relationship in the accompanying drawings are only used for illustrative purposes and cannot be understood as limitations on this patent. For those of ordinary skill in the art, the specific meanings of the above terms can be understood according to the specific circumstances.

[0035] Embodiment 1: Combining with Figure 1 , Attachment Figure 2 , Attachment Figure 3 and attached Figure 4 This embodiment constructs a method for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as a raw material, and the method for preparing rod-shaped nano manganese dioxide comprises:

[0036] Step 1: taking manganese oxide ore powder and a reducing agent to carry out a leaching reaction in a sulfuric acid solution, the leaching temperature is 90° C., the time is 2 hours, and after the leaching reaction is completed, the solid-liquid separation is carried out to obtain a manganese oxide ore leachate, wherein the reducing agent includes sodium thiosulfate, walnut shells, glucose or iron powder;

[0037] Step 2: Take the manganese oxide ore leachate, add 36% hydrogen peroxide by mass, add manganese carbonate to adjust the pH to 2.5-3.5, add potassium sulfate, and perform oxidation reaction at 90° C. for 2 hours. After the reaction is completed, filter to obtain a filtrate, wherein the hydrogen peroxide is 2% by volume of the manganese oxide ore leachate, and the amount of potassium sulfate is 10% by mass of the manganese oxide ore leachate;

[0038] Step 3: After the filtrate is cooled, deionized water is gradually added to dilute the filtrate to 2.5 times of the original volume to obtain a fixed volume solution, and potassium permanganate is gradually added to the fixed volume solution according to a molar ratio of manganese to potassium permanganate of 3:2 in the fixed volume solution, and stirred at 85°C and 200 r / min for 4 hours. After the reaction is completed, the target mixed solution is obtained, and the target mixed solution is filtered to obtain a black powdery solid, wherein the molar number of manganese in the fixed volume solution is obtained by atomic absorption spectrometry, redox titration or inductively coupled ion emission spectrometry;

[0039] Step 4: Dry the black powdery solid at 60° C. for 3 h to obtain rod-shaped nano manganese dioxide.

[0040] Using sodium thiosulfate as a reducing agent, a rod-shaped nano manganese dioxide with a thickness of 20 nanometers and a length of 300 nanometers can be obtained. The structure of the rod-shaped nano manganese dioxide obtained by using sodium thiosulfate as a reducing agent is magnified 304200 times as shown in the electron microscope image. Figure 1 shown.

[0041] Using walnut shell as a reducing agent, a rod-shaped nano manganese dioxide with a length of 130 nanometers can be obtained. The structure of the rod-shaped nano manganese dioxide obtained by using walnut shell as a reducing agent is shown in the electron microscope image when it is magnified 304200 times. Figure 2 shown.

[0042] Using iron powder as a reducing agent, rod-shaped nano manganese dioxide with a length range of 150-400 nanometers can be obtained. The structure electron microscope image of the rod-shaped nano manganese dioxide obtained by using iron powder as a reducing agent when magnified 303130 times is as follows Figure 3 shown.

[0043] Using glucose as a reducing agent, a rod-shaped nano-manganese dioxide with a length of 130 nanometers can be obtained. The structure electron microscope image of the rod-shaped nano-manganese dioxide obtained by using glucose as a reducing agent when magnified 301050 times is as follows Figure 4 shown.

[0044] The method for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as a raw material of the present invention replaces the traditional high-cost analytical pure manganese salt raw material with manganese oxide ore powder, providing an innovative solution for the industrial production of rod-shaped nano manganese dioxide. At the same time, by using iron powder, walnut shells or glucose as a cheap and easily available reducing agent, the production cost of nano manganese dioxide is significantly reduced, providing feasibility for large-scale industrial production.

[0045] Embodiment 2: Combining with Figure 5 , Attachment Figure 6 , Attachment Figure 7 and attached Figure 8 In addition to the contents of the above embodiments, this embodiment also constructs a preparation system for the rod-shaped nano manganese dioxide preparation method, characterized in that the rod-shaped nano manganese dioxide preparation system includes a leaching reaction module for receiving manganese oxide ore powder and a reducing agent for leaching reaction in a sulfuric acid solution, an oxidation reaction module for oxidizing the manganese oxide ore leachate with hydrogen peroxide, manganese carbonate and potassium sulfate, and a reprocessing module for adding potassium permanganate to the filtrate to obtain a target mixed solution and continuing to filter the target mixed solution to obtain a black powdery solid and drying the black powdery solid to obtain rod-shaped nano manganese dioxide.

[0046] Among them, the leaching reaction module and the oxidation reaction module are respectively realized by different reaction tanks, each of which includes a tank body, an agitator rotatably matched in the tank body, a constant temperature heater for constant temperature heating of the mixed liquid in the tank body, a filter plate horizontally arranged in the tank body, a feed port arranged on the tank body, a derivation pipe connected to the bottom wall of the tank body, an electric control valve for controlling the connection between the derivation pipe and the tank body, a pH monitor and a liquid pump for driving the liquid filtered through the filter plate out of the tank body from the derivation pipe.

[0047] The reaction tank for completing the leaching reaction module is the first reaction tank. The implementation process of the leaching reaction module in the first reaction tank includes: manganese oxide ore powder, reducing agent and sulfuric acid solution are sequentially fed into the tank body of the first reaction tank from the feed port of the first reaction tank, the agitator rotates at a set speed to ensure that the manganese oxide ore powder and the reducing agent are evenly dispersed in the sulfuric acid solution, the reaction rate and leaching efficiency are improved so that the manganese oxide ore and the reducing agent fully react to generate dissolved manganese ions, the constant temperature heater controls the temperature in the first reaction tank at 90°C for two hours, the leaching reaction is completed, and a manganese oxide ore leachate is formed, the solid-liquid mixture in the first reaction tank is separated into solid and liquid through a filter plate, the solid residue is retained on the filter plate, the liquid pump of the first reaction tank performs a suction operation, and the manganese oxide ore leachate filtered through the filter plate of the first reaction tank is discharged from the first reaction tank through a dewatering pipe.

[0048] The reaction tank that completes the oxidation reaction module is the second reaction tank, the outlet pipe of the first reaction tank is connected to the second reaction tank, and the implementation process of the oxidation reaction module in the second reaction tank includes: the manganese oxide ore leaching liquid discharged from the first reaction tank is sent into the tank body of the second reaction tank, hydrogen peroxide, manganese carbonate and potassium sulfate are added to the second reaction tank in sequence from the feeding port of the second reaction tank, the agitator in the second reaction tank rotates at a constant speed, and the constant temperature heater maintains the temperature in the second reaction tank at 90°C. After 2 hours, the solid-liquid mixture in the second reaction tank is separated by the filter plate, and the solid precipitate is retained on the filter plate. The liquid pump of the second reaction tank performs extraction operation, and the filtrate filtered out of the filter plate of the second reaction tank is discharged out of the second reaction tank through the outlet pipe.

[0049] The reprocessing module comprises a reaction vessel with an open top structure, a liquid level sensor for monitoring the liquid level in the reaction vessel, a supporting base plate fixed around the outer wall of the reaction vessel, a sealing cover for covering the opening at the top of the reaction vessel, a movable opening arranged in the middle of the sealing cover, a rotating shaft arranged vertically through the movable opening, a stirring blade sleeved on the rotating shaft, a driving motor connected to the top of the rotating shaft through a coupling, a fixed base for fixing the top of the driving motor, a plurality of electric push rods respectively fixedly connected to the fixed base at the top and fixedly connected to the sealing cover at the bottom, a driving mechanism for driving the sealing cover to close the reaction vessel, heating strips evenly laid on the outer wall of the reaction vessel, and a suction filtration unit for suction filtration of the target mixed liquid in the reprocessing module.

[0050] The reaction vessel is a cubic structure, and the electric push rod is used to drive the fixed base to move up and down relative to the sealing cover, thereby synchronously driving the stirring shaft and the stirring blade to move up and down in the reaction vessel.

[0051] The filtration unit includes a plurality of through ports respectively arranged at the top of the sealing cover, through pipes arranged to penetrate the through ports in sequence, pumps respectively arranged to be connected to the through pipes, a suction component arranged to be connected to the bottom of the through pipes, a transfer port arranged on the side wall of the reaction vessel, a matching door that can be airtightly matched with the transfer port, a door handle arranged on the matching door, an interception component matched to the bottom of the reaction vessel and partially fixed to the matching door, a liquid discharge port respectively arranged at the bottom of the reaction vessel, an electrically controlled closing valve for controlling the closing of the liquid discharge port, a liquid discharge pipe for driving the liquid phase of the target mixed liquid in the reaction vessel to be discharged from the liquid discharge port, and a filtration pump respectively arranged to be connected to the liquid discharge pipe.

[0052] The suction component includes a vertically arranged plate body, a cavity arranged inside the plate body, suction holes evenly distributed on the outer wall of the plate body and capable of communicating with the cavity, and an interface arranged on the top of the plate body and communicating with the cavity. The through pipe and the interface are airtightly connected by welding, threading or flange connection.

[0053] The driving mechanism comprises a plurality of telescopic driving rods, one end of which is fixed to the sealing cover through a corresponding fixing piece and the other end of which is fixed to the supporting base plate through a fixing seat.

[0054] The specific operation steps of the reprocessing module include:

[0055] S101: the telescopic driving rod is in an extended state, the sealing cover is arranged away from the top of the reaction vessel, the potassium permanganate, deionized water and the filtrate discharged from the second reaction tank enter the reaction vessel from the opening at the top of the reaction vessel respectively, and the electric push rod drives the stirring blade to extend to the bottom of the reaction vessel to perform stirring operation by contraction, the liquid level sensor monitors the liquid level in the reaction vessel in real time, the heating strip heats the reaction vessel to 85° C., the driving motor drives the stirring blade to stir at 200 r / min, the reaction is carried out for 4 hours, and the target mixed solution is obtained after the reaction is completed;

[0056] S102: When the telescopic driving rod is in the retracted state, the sealing cover is closed on the top of the reaction vessel, and the suction components are sequentially extended to the bottom of the reaction vessel, and the driving motor stops working at the same time, the electric driving rod drives the stirring blade to move to the top of the target mixed liquid by extension, the electrically controlled closing valve is opened, and the suction pump and the suction pump perform suction operations to extract the liquid phase of the target mixed liquid out of the reaction vessel, and the liquid phase is discharged through the drain port, and the black powdery solid of the solid phase is intercepted by the interception component;

[0057] S103: The suction component at least partially extends into the black powder solid above the interception component, and the pump is driven at a preset frequency to generate a preset adsorption strength to suck the residual water molecules in the black powder solid. The heating strip heats the temperature in the reaction vessel to 60° C. and maintains the constant temperature for 3 hours, and dries to obtain rod-shaped nano manganese dioxide;

[0058] S104: The heating strip stops heating, the telescopic driving rod is driven to an extended state, the sealing cover is driven away from the top of the reaction vessel, and the suction component is moved away from the intercepting component, and the intercepting component and the dry rod-shaped nano manganese dioxide in the intercepting component are transferred out of the reaction vessel by opening the transfer door.

[0059] The rod-shaped nano manganese dioxide preparation system of the present invention independently realizes the leaching reaction, oxidation reaction and reprocessing through a dedicated reaction tank and a reprocessing module, thereby avoiding cross interference between reactions, thereby improving the reaction efficiency and process controllability, and improving the preparation purity and efficiency of the rod-shaped nano manganese dioxide.

[0060] Embodiment 3: Combining with Figure 5 , Attachment Figure 6 , Attachment Figure 7 and attached Figure 8 In addition to the contents of the above embodiments, the outer layer of the plate body is provided with a filter element adapted to the shape of the plate body and a fixing clamp for reinforcing and fixing the filter element to the outside of the plate body, the filter element has an open bag-like structure, and the filter element can be sequentially mounted on the plate body from the bottom of the plate body, and the filter element is obtained by cutting and pressing a disposable filter paper or a multi-layer composite filter membrane.

[0061] The intercepting component includes a collecting dish adapted to the bottom of the reaction dish, the bottom wall of the collecting dish is provided with a bottom opening for liquid discharge, the side wall of the collecting dish is provided with a side opening, and filter sheets are respectively installed at the bottom opening and the side opening, the filter sheets intercept the solids of the target reaction liquid to ensure that the liquid phase is smoothly discharged from the reaction dish.

[0062] Part of the side wall of the collecting dish is fixed by welding with the matching door through argon arc welding or laser welding technology, and a sliding structure of sliding matching is arranged between the outer wall of the collecting dish and the inner wall of the reaction dish. The sliding structure consists of a parallel slide groove on the inner wall of the reaction dish and a guide rail part corresponding to the outer wall of the collecting dish.

[0063] In the sliding operation, the collecting dish is pushed and pulled horizontally along the sliding groove by pulling and pulling the matching door, so that the rod-shaped nano manganese dioxide dried in the collecting dish is transferred out of the reaction dish.

[0064] The filter clamp includes a male clamp and a female clamp which are horizontally arranged and adapted to the top of the plate body, and the middle areas of the male clamp and the female clamp are respectively adapted to the outer wall of the plate body, and the two sides of the male clamp and the female clamp extend out of the two sides of the plate body respectively, and the two sides of the male clamp can be engaged and fixed with the two sides of the female clamp, thereby realizing the removal of the male clamp and the female clamp shell and being mounted on the plate body. At the same time, the filter clamp provides positioning and support for the filter element to ensure that the filter element is flatly attached to the surface of the plate body and that the filter element does not slide or fall off during use.

[0065] The bottom edge of the transfer port is adjacent to the bottom wall of the reaction dish. The transfer port is a rectangular opening. The inner wall of the transfer port opening is processed with high precision to form a smooth limiting groove. The outer periphery of the matching door is provided with a sealing strip made of a composite of fluororubber and polytetrafluoroethylene high temperature resistant and corrosion resistant materials. The sealing strip forms a seal by directly fitting with the limiting groove, and can provide reliable airtightness in high temperature and high corrosion environments. The limiting groove is used to limit the installation position of the sealing strip. The sealing strip forms an airtight connection by precisely fitting with the limiting groove, and can provide reliable sealing performance in high temperature and high corrosion environments.

[0066] The mating door is locked and fixed to the side wall of the reaction dish by a detachable locking buckle. The locking buckle applies uniform pressure to press the sealing strip onto the limiting groove of the transfer port. The locking buckle facilitates the operator to quickly open or close the mating door, while ensuring good pressure resistance and anti-leakage performance in a sealed state. The locking buckle is a spring lock buckle, a rotary pressure buckle or a lever-type lock buckle in the prior art.

[0067] The preparation system of the present invention realizes the preparation of the target mixed liquid, the filtration and drying of the black powdery solid through the integration of the reaction vessel, and combines the sliding structure, the filter element fixing system and the airtight connection design of the high-precision limit groove and the sealing strip, so that the operation process from reaction to drying is completely closed and efficient, avoiding the complexity and efficiency loss caused by switching of multiple devices. At the same time, the convenient design of the door and the locking buckle further improves the reliability and ease of operation of the overall system, and improves the efficiency of the preparation of rod-shaped nano manganese dioxide.

[0068] Although the present invention has been described above with reference to various embodiments, it should be understood that many changes and modifications may be made without departing from the scope of the present invention. That is, the methods, systems and devices discussed above are examples. Various configurations may appropriately omit, replace or add various processes or components. For example, in alternative configurations, the method may be performed in an order different from that described, and / or various components may be added, omitted and / or combined. Moreover, the features described with respect to certain configurations may be combined in various other configurations, such as different aspects and elements of the configuration may be combined in a similar manner. In addition, as technology develops, the elements therein may be updated, i.e., many elements are examples and do not limit the scope of the present disclosure or claims. And it should be understood that after reading the contents of the record of the present invention, the technician may make various changes or modifications to the present invention, and these equivalent changes and modifications also fall within the scope defined by the claims of the present invention.

Claims

1. A method for preparing rod-shaped nano manganese dioxide using manganese ore leaching solution as raw material, characterized in that: The method for preparing rod-shaped nano manganese dioxide comprises: Step 1: taking manganese oxide ore powder and a reducing agent to carry out a leaching reaction in a sulfuric acid solution, the leaching temperature is 90° C., the time is 2 hours, and after the leaching reaction is completed, the solid-liquid separation is carried out to obtain a manganese oxide ore leachate, wherein the reducing agent includes sodium thiosulfate, walnut shells, glucose or iron powder; Step 2: Take the manganese oxide ore leachate, add 36% hydrogen peroxide by mass, add manganese carbonate to adjust the pH to 2.5-3.5, add potassium sulfate, and perform oxidation reaction at 90° C. for 2 hours. After the reaction is completed, filter to obtain a filtrate, wherein the hydrogen peroxide is 2% by volume of the manganese oxide ore leachate, and the amount of potassium sulfate is 10% by mass of the manganese oxide ore leachate; Step 3: After the filtrate is cooled, deionized water is gradually added to dilute the filtrate to 2.5 times of the original volume to obtain a fixed volume solution, and potassium permanganate is gradually added to the fixed volume solution according to a molar ratio of manganese to potassium permanganate of 3:2 in the fixed volume solution, and stirred at 85°C and 200 r / min for 4 hours. After the reaction is completed, the target mixed solution is obtained, and the target mixed solution is filtered to obtain a black powdery solid, wherein the molar number of manganese in the fixed volume solution is obtained by atomic absorption spectrometry, redox titration or inductively coupled ion emission spectrometry; Step 4: Dry the black powdery solid at 60° C. for 3 h to obtain rod-shaped nano manganese dioxide.

2. A preparation system for implementing the preparation method of rod-shaped nano manganese dioxide according to claim 1, characterized in that: The rod-shaped nano manganese dioxide preparation system comprises a leaching reaction module for receiving manganese oxide ore powder and a reducing agent for leaching reaction in a sulfuric acid solution, an oxidation reaction module for carrying out an oxidation reaction on a manganese oxide ore leachate with hydrogen peroxide, manganese carbonate and potassium sulfate, and a reprocessing module for adding potassium permanganate to a fixed volume of a filtrate to obtain a target mixed solution and continuing to filter the target mixed solution to obtain a black powdery solid and drying the black powdery solid to obtain rod-shaped nano manganese dioxide.

3. The rod-shaped nano manganese dioxide preparation system according to claim 2, characterized in that: The reprocessing module comprises a reaction vessel with an open top structure, a liquid level sensor for monitoring the liquid level in the reaction vessel, a supporting base plate fixed around the outer wall of the reaction vessel, a sealing cover for covering the opening at the top of the reaction vessel, a movable opening arranged in the middle of the sealing cover, a rotating shaft arranged vertically through the movable opening, a stirring blade sleeved on the rotating shaft, a driving motor connected to the top of the rotating shaft through a coupling, a fixed base for fixing the top of the driving motor, a plurality of electric push rods respectively fixedly connected to the fixed base at the top and fixedly connected to the sealing cover at the bottom, a driving mechanism for driving the sealing cover to close the reaction vessel, a heating strip evenly laid on the outer wall of the reaction vessel, and a suction filtering unit for suction filtering the target mixed liquid in the reprocessing module. The reaction vessel is a cubic structure, and the electric push rod is used to drive the fixed base to move up and down relative to the sealing cover, thereby synchronously driving the stirring shaft and the stirring blade to move up and down in the reaction vessel.

4. The rod-shaped nano manganese dioxide preparation system according to claim 3, characterized in that: The driving mechanism comprises a plurality of telescopic driving rods, one end of which is fixed to the sealing cover through a corresponding fixing piece and the other end of which is fixed to the supporting base plate through a fixing seat.

5. The rod-shaped nano manganese dioxide preparation system according to claim 4, characterized in that: The filtration unit includes a plurality of through ports respectively arranged at the top of the sealing cover, through pipes arranged to penetrate the through ports in sequence, pumps respectively arranged to be connected to the through pipes, a suction component arranged to be connected to the bottom of the through pipes, a transfer port arranged on the side wall of the reaction vessel, a matching door that can be airtightly matched with the transfer port, a door handle arranged on the matching door, an interception component matched to the bottom of the reaction vessel and partially fixed to the matching door, a discharge port respectively arranged at the bottom of the reaction vessel, an electrically controlled closing valve for controlling the closing of the discharge port, a discharge pipe for driving the liquid phase of the target mixed liquid in the reaction vessel to be discharged from the discharge port, and a filtration pump respectively arranged to be connected to the discharge pipe.

6. The rod-shaped nano manganese dioxide preparation system according to claim 5, characterized in that: The suction component includes a vertically arranged plate body, a cavity arranged inside the plate body, suction holes evenly distributed on the outer wall of the plate body and capable of communicating with the cavity, and an interface arranged on the top of the plate body and communicating with the cavity. The through pipe and the interface are airtightly connected by welding, threading or flange connection.

7. The rod-shaped nano manganese dioxide preparation system according to claim 6, characterized in that: The outer layer of the plate body is sleeved with a filter element adapted to the shape of the plate body and a fixing clamp that strengthens and fixes the filter element to the outside of the plate body. The filter element has an open bag-like structure, and the filter elements can be sequentially sleeved on the plate body from the bottom of the plate body. The filter element is obtained by cutting and hot-pressing disposable filter paper or multi-layer composite filter membrane.

8. The rod-shaped nano manganese dioxide preparation system according to claim 7, characterized in that: The intercepting component includes a collecting dish adapted to the bottom of the reaction dish, the bottom wall of the collecting dish is provided with a bottom opening for liquid discharge, the side wall of the collecting dish is provided with a side opening, and filter sheets are respectively installed at the bottom opening and the side opening, the filter sheets intercept the solids of the target reaction liquid to ensure that the liquid phase is smoothly discharged from the reaction dish.

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