CN113200570B - Mn based on MES system 3 O 4 Continuous production process - Google Patents

Mn based on MES system 3 O 4 Continuous production process Download PDF

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CN113200570B
CN113200570B CN202110557466.1A CN202110557466A CN113200570B CN 113200570 B CN113200570 B CN 113200570B CN 202110557466 A CN202110557466 A CN 202110557466A CN 113200570 B CN113200570 B CN 113200570B
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unit
reaction
production
conveying device
material conveying
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CN113200570A (en
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杨洋
王以存
丁晓锋
刘阿朋
田甜
费凡
王志鹏
王军伟
王金宝
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Sinosteel New Materials Co Ltd
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Sinosteel New Materials Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/02Oxides; Hydroxides
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B19/00Programme-control systems
    • G05B19/02Programme-control systems electric
    • G05B19/418Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM]
    • G05B19/41875Total factory control, i.e. centrally controlling a plurality of machines, e.g. direct or distributed numerical control [DNC], flexible manufacturing systems [FMS], integrated manufacturing systems [IMS] or computer integrated manufacturing [CIM] characterised by quality surveillance of production
    • GPHYSICS
    • G05CONTROLLING; REGULATING
    • G05BCONTROL OR REGULATING SYSTEMS IN GENERAL; FUNCTIONAL ELEMENTS OF SUCH SYSTEMS; MONITORING OR TESTING ARRANGEMENTS FOR SUCH SYSTEMS OR ELEMENTS
    • G05B2219/00Program-control systems
    • G05B2219/30Nc systems
    • G05B2219/32Operator till task planning
    • G05B2219/32368Quality control
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P90/00Enabling technologies with a potential contribution to greenhouse gas [GHG] emissions mitigation
    • Y02P90/02Total factory control, e.g. smart factories, flexible manufacturing systems [FMS] or integrated manufacturing systems [IMS]

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Quality & Reliability (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Automation & Control Theory (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses an MES system basedMn 3 O 4 A continuous production process. The process comprises the following steps: s1: modeling; s2: mixing materials; s3: reacting; s4: press filtration; s5: drying; s6: and (3) collecting: and (5) collecting the material obtained in the step S5 in a collecting unit. Mn based on MES system of the invention 3 O 4 Mn is realized by a continuous production process through an MES system 3 O 4 Can improve Mn 3 O 4 The production efficiency of the main quality characteristics of the product is improved, the process capability index cpk of the main quality characteristics of the product is improved, and the product is more stable and controllable.

Description

Mn based on MES system 3 O 4 Continuous production process
Technical Field
The invention belongs to the field of control of flow industrial production process, and more particularly relates to Mn based on an MES system 3 O 4 A continuous production process.
Background
The manganous-manganic oxide belongs to high-performance structural materials, is mainly used in the electronic industry, is one of important raw materials required for producing the soft magnetic ferrite, is also a high-quality raw material for preparing the manganese-zinc ferrite, and the prepared soft magnetic ferrite accounts for more than 60% of the total amount of the soft magnetic ferrite. After manganese oxide is used for replacing manganese carbonate as a manganese source to prepare the manganese zinc soft magnetic ferrite, the development of the manganese oxide is rapid; the soft magnetic ferrite is made by mixing oxides of manganese, zinc and iron according to a certain proportion, sintering and forming, has a narrow remanence induction curve, can be magnetized repeatedly, has high direct current resistivity, and can avoidEddy current losses. It can be used as magnetic core, magnetic disk and magnetic tape for storing information in electronic computer, telephone transformer and high-quality inductor, television flyback transformer, magnetic recording head, inductor, magnetic amplifier, saturated inductor and antenna rod. Through the development for over twenty years, the production scale of the manganous manganic oxide in China becomes the first world, the application of the manganous manganic oxide is more and more extensive, and the market demand is also increasing continuously. Therefore, there is a need to develop an intelligently produced Mn 3 O 4 Is a continuous production process of (3).
The MES system is a production informatization management system facing the workshop execution layer of a manufacturing enterprise. The whole production process from order to product completion can be optimally managed through information transmission. The MES system has been found to be useful in the production of ceramics (CN 108706963A), semiconductors (CN 110233122A), formulas (CN 112258053A), and the like. However, the prior art does not disclose Mn 3 O 4 Is combined with MES system.
There are many preparation methods of manganous oxide, and the preparation methods can be divided into the following steps from the aspects of reaction property and process characteristics: reduction, calcination, electrolysis and oxidation. The method for producing the manganous-manganic oxide in China mostly adopts an electrolytic metal manganese powder sheet suspension oxidation method, the raw materials of the method are electrolytic metal manganese sheets, firstly, the metal manganese sheets are crushed into suspension, and the manganous-manganic oxide is prepared under certain conditions by using an oxidant, and the basic process flow is as follows: pulping, oxidizing, drying and obtaining the finished product of the electrolytic manganese metal sheet. The key of the technology is an oxidation tank, a washing tower and water treatment and drying equipment. Wherein reverse osmosis equipment and ion exchange equipment are generally adopted in water treatment; the oxidation tank usually utilizes a titanium-lined plate high-efficiency stirring tank or rubber lining; the scrubber typically utilizes a multi-stage countercurrent scrubber; the drying equipment adopts pressure spray type, centrifugal spray type and box type drying.
However, in the prior art Mn 3 O 4 The production process of the device adopts a discontinuous circulation mode, manual operation is needed, and a one-to-one mode is adopted among the processes, so that the production efficiency and the equipment utilization rate are greatly reduced.
Disclosure of Invention
1. Problems to be solved
For the existing Mn 3 O 4 The invention provides Mn based on an MES system, which has the problems of low production efficiency and unstable quality 3 O 4 The system can feed back production information in real time according to intelligent control equipment of reaction process and improve Mn 3 O 4 Is characterized by high productivity and stable quality.
2. Technical proposal
In order to solve the problems, the invention adopts the following technical scheme:
mn based on MES system of the invention 3 O 4 The continuous production process comprises the following steps:
s1: modeling: inputting the production parameters into a control unit comprising an MES system database;
s2: mixing: selecting a designated mixing unit;
s3: the reaction: after the raw materials are processed by the mixing unit, the reaction unit and a material conveying device input into the reaction unit are matched according to the conditions required by the reaction, and the reaction is stopped after the reaction reaches the specified pH;
s4: and (3) filter pressing: the MES system determines that the filter pressing unit automatically feeds;
s5: and (3) drying: according to the equipment state, the material obtained by the S4 filter pressing is transmitted to a drying unit for drying;
s6: and (3) collecting: and (5) collecting the material obtained in the step S5 in a collecting unit.
Furthermore, the materials after the reaction flow into the storage unit, and according to the liquid level information of the storage unit, the MES system determines whether the materials can be discharged or not and conveys the materials to the filter pressing unit.
The production line matched with the continuous production process comprises a plurality of production units, each production unit is provided with respective identification information, and the system also comprises a control unit of an MES system database; at least one material conveying device is arranged between two adjacent production units, each material conveying device is provided with respective identification information, and the identification information of each material conveying device is associated with a material state; and an information acquisition device for acquiring the identification information of the production unit from each production unit and the identification information of the material conveying device from each material conveying device, wherein the control unit is connected with the information acquisition device and is used for binding the identification information of each material conveying device received from the information acquisition device with the identification information of the corresponding production unit through an MES system database, and the corresponding production unit is a production unit for receiving all materials associated with the identification information of the material conveying device.
Still further, the production unit comprises a mixing unit, a reaction unit, a filter pressing unit, a drying unit and a collecting unit, wherein a material conveying device between the mixing unit and the reaction unit comprises at least two first conveying pipes, and an electromagnetic ball valve is arranged on each first conveying pipe; the material conveying device between the reaction unit and the filter pressing unit comprises at least two second conveying pipes, and an electromagnetic ball valve is arranged on each second conveying pipe; the material conveying device between the filter pressing unit and the drying unit comprises at least one feeder; the material conveying device between the drying unit and the collecting unit comprises at least one third conveying pipe.
Further, the information acquisition device is a code scanning gun, the identification information is borne by the bar codes, and the corresponding bar codes are attached to the outer surfaces of the production unit and the material conveying device.
Still further, the compounding unit includes grinding mechanism and rabbling mechanism, grinding mechanism's discharge gate passes through pipe connection with rabbling mechanism's feed inlet, grinding mechanism includes vertical tower mill, ball mill or roller mill, can realize the grinding of material can, rabbling mechanism includes stirred tank, agitator tank or stirred tank, can realize the stirring of material can.
Still further, the reaction unit includes reation kettle and air pump, reation kettle's feed inlet is connected with rabbling mechanism's discharge gate, the air inlet of air pump is located the reation kettle lower extreme for provide the air for the reaction.
Further, the filter pressing unit comprises a plate-and-frame filter press, the plate-and-frame filter press is provided with a trolley in a matched mode and used for unloading plates, and a feeder is arranged below the plate-and-frame filter press and used for conveying filter cakes obtained by filter pressing to the drying unit; the filter press is a plate-and-frame filter press, and can realize the same function as the plate-and-frame filter press, and can also be reverse osmosis equipment, ion exchange equipment, a centrifuge or a filter.
Still further, drying unit includes flash dryer and combustion furnace, the drying body is cylindricly, and its bottom is equipped with high-speed rotatory sword, drying body one side below is equipped with feed inlet and feeder terminal and links up, drying body and combustion furnace's exit linkage intercommunication, drying body's opposite side top is equipped with the discharge gate, and after the material was exported from the discharge gate, get into the collection unit by the third conveyer pipe, stirring crushing mechanism includes high-speed rotatory sword or stirring tooth.
Still further, the collection unit includes the selection powder machine, the selection powder machine below is equipped with first discharge gate, the below of first discharge gate is equipped with highly-compressed air pump, the selection powder machine upper end is connected with dust removal mechanism A through the pipeline, dust removal mechanism A's end is equipped with extraction mechanism A, extraction mechanism A is driven by the motor, dust removal mechanism A below is equipped with the second discharge gate, the lower extreme of first discharge gate passes through the pipe connection with the lower extreme of second discharge gate, forms the air by highly-compressed air pump and send.
Furthermore, the control unit is provided with a control console and terminal equipment, the state of the equipment in the production process is provided with data by the information acquisition device, and the MES system regulates and controls according to the acquired data. The terminal equipment can be a computer, a mobile phone or a tablet, and can be provided with an MES system database.
Still further, still include the storage unit, the storage unit includes the stock chest, the stock chest is located the conveyer pipe of second conveyer pipe.
Still further, the exit of reation kettle inboard, burning furnace, the discharge gate of dry body opposite side, dust removal mechanism A's air intake are equipped with temperature sensor respectively, the exit of burning furnace, dust removal mechanism A's exit punishment do not is equipped with pressure sensor, reation kettle inboard and storage tank inboard are equipped with level sensor respectively, the reation kettle inboard is equipped with pH sensor, first conveyer pipe between rabbling mechanism and the reation kettle is equipped with the flowmeter, and the second conveyer pipe between reation kettle and storage tank, storage tank and the plate-and-frame filter press is equipped with the flowmeter, and the pipeline between reation kettle and the air pump is equipped with the flowmeter, temperature sensor, pressure sensor, level sensor, pH sensor and flowmeter all are connected with terminal equipment electricity.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
mn based on MES system of the invention 3 O 4 Mn is realized by a continuous production process through an MES system 3 O 4 Can improve Mn 3 O 4 The production efficiency of the main quality characteristics of the product is improved, the process capability index cpk of the main quality characteristics of the product is improved, and the product is more stable and controllable.
Drawings
The technical solution of the present invention will be described in further detail below with reference to the accompanying drawings and examples, but it should be understood that these drawings are designed for the purpose of illustration only and thus are not limiting the scope of the present invention. Moreover, unless specifically indicated otherwise, the drawings are intended to conceptually illustrate the structural configurations described herein and are not necessarily drawn to scale.
FIG. 1 shows Mn of the present invention 3 O 4 Schematic diagram of continuous production process;
FIG. 2 is Mn of the present invention 3 O 4 A structural schematic diagram of a continuous production system;
FIG. 3 is a schematic diagram of a mixing unit according to the present invention;
FIG. 4 is a schematic diagram of a reaction unit according to the present invention;
FIG. 5 is a schematic view of a storage unit according to the present invention;
FIG. 6 is a schematic diagram of a filter press unit according to the present invention;
FIG. 7 is a schematic diagram of a drying unit according to the present invention;
FIG. 8 is a schematic diagram of a collection unit according to the present invention;
FIG. 9 is a schematic diagram of a steering unit according to the present invention;
FIG. 10 is a schematic view of a material conveying process according to the present invention;
in the figure:
200. a mixing unit; 210. a grinding mechanism; 220. a stirring mechanism;
300. a reaction unit; 310. a reaction kettle; 320. an air pump;
400. a storage unit; 410. a storage tank;
500. a filter pressing unit; 510. a filter press; 520. a trolley; 530. a feeder;
600. a drying unit; 610. a dryer; 620. drying the body; 630. a combustion furnace; 640. a stirring and crushing mechanism;
700. a collection unit; 710. a powder selecting machine; 720. a first discharge port; 730. a second discharge port; 740. a dust remover A; 750. extraction mechanism A; 760. a high pressure air pump;
900. a manipulation unit; 910. a console; 920. and a display screen.
Detailed Description
The following detailed description and example embodiments of the invention may be better understood when read in conjunction with the accompanying drawings, in which elements and features of the invention are identified by reference numerals.
Example 1
As shown in FIG. 1, the Mn based MES system of the present embodiment 3 O 4 The continuous production process comprises the following steps:
s1: modeling: inputting the production parameters into a control unit 900 comprising an MES system database, and establishing the MES system database;
s2: mixing: selecting a designated mixing unit 200, conveying the materials to a tower mill 210 after entering the mixing unit 200, and conveying the materials to a stirring tank 220 for material mixing after grinding to designated parameters;
s3: the reaction: after the raw materials are processed by the mixing unit 200, matching the reaction kettle 310 and a material conveying device input into the reaction kettle 310 according to the reaction required conditions, and stopping the reaction after the reaction reaches the specified pH;
s4: and (3) material storage: after the reaction is finished, the MES system determines whether discharging can be performed according to the liquid level information of the storage tank 410;
s5: and (3) filter pressing: according to the liquid level information of the storage tank 410, the MES system determines that the filter pressing unit 500 automatically feeds, and the materials are conveyed to the flash dryer 610 by the feeder 530 after being processed by the plate-and-frame filter press 510;
s6: and (3) drying: according to the equipment state, the material obtained by the S5 filter pressing is transmitted to a flash dryer 610 for drying;
s7: and (3) collecting: the materials obtained in S6 are collected in the collecting unit 700, and the materials may be collected directly or after being processed by the powder concentrator 710.
As shown in fig. 2 to 9, a production line used in cooperation with a continuous production process includes a plurality of production units, each of which has respective identification information; at least one material conveying device is arranged between two adjacent production units, each material conveying device is provided with respective identification information, and the identification information of each material conveying device is associated with a material state (slurry, wet material and powder exist in the invention); and an information acquisition device for acquiring the identification information of the production unit from each production unit and the identification information of the material conveying device from each material conveying device, wherein the control unit 900 is connected with the information acquisition device and performs information matching on the identification information of each material conveying device received from the information acquisition device and the identification information of the corresponding production unit through the MES system database, and the corresponding production unit is a production unit for receiving all materials associated with the identification information of the material conveying device.
In this embodiment, the production unit includes a mixing unit 200, a reaction unit 300, a filter pressing unit 500, a drying unit 600, and a collecting unit 700, where a material conveying device between the mixing unit 200 and the reaction unit 300 includes at least two first conveying pipes, and an electromagnetic ball valve is disposed on each first conveying pipe; the material conveying device between the reaction unit 300 and the filter pressing unit 500 comprises at least two second conveying pipes, and an electromagnetic ball valve is arranged on each second conveying pipe; the material conveying device between the filter pressing unit 500 and the drying unit 600 comprises at least one feeder; the material conveying means between the drying unit 600 and the collecting unit 700 comprises at least one third conveying pipe. The three-way valve is arranged at the discharge ports of the mixing unit and the reaction unit, and the first conveying pipe and the second conveying pipe can be connected to the three-way valve and then are communicated in a control way through the electromagnetic ball valve. Furthermore, in some cases, it is also possible to connect the corresponding transport pipe to the corresponding production unit manually.
1) Mixing unit 200: the mixing unit 200 comprises a vertical tower mill, a horizontal ball mill, a roller mill and three matched stirring tanks, wherein a discharge hole of the vertical tower mill is connected with a feed hole of the stirring tanks through pipelines;
2) Reaction unit 300: the reaction unit 300 comprises three reaction kettles 310 and an air pump 320, wherein a feed inlet of the reaction kettles 310 is connected with a discharge outlet of a stirring tank, and an air inlet of the air pump 320 is positioned at the lower end of the reaction kettles 310;
3) Storage unit 400: the storage unit 400 comprises three storage tanks 410, wherein the storage tanks 410 are positioned on a conveying pipeline of the second conveying pipe;
4) Filter pressing unit 500: the filter pressing unit 500 comprises a three-platen frame filter press 510, wherein a trolley 520 is arranged above the plate frame filter press 510, and a feeder 530 is arranged below the plate frame filter press 510 and is used for conveying a filter cake obtained by filter pressing to the drying unit 600;
5) Drying unit 600: the drying unit 600 comprises three flash evaporation dryers 610, the flash evaporation dryers 610 comprise a drying body 620 and a combustion furnace 630, the drying body 620 is cylindrical, a high-speed rotary knife 640 is arranged at the bottom of the drying body, a feeding port is arranged below one side of the drying body 620 and is connected with the terminal of the feeder 530, the drying body 620 is communicated with an outlet of the combustion furnace 630, a discharging port is arranged above the other side of the drying body 620, and materials enter the collecting unit 700 through a third conveying pipe after being output from the discharging port;
6) The collection unit 700: the collecting unit 700 comprises a powder concentrator 710, a first discharge hole 720 is arranged below the powder concentrator 710, a high-pressure air pump 760 is arranged below the first discharge hole 720, the upper end of the powder concentrator 710 is connected with a dust removing mechanism A740 through a pipeline, the dust removing mechanism A740 is connected with an extracting mechanism A750 through a pipeline, the extracting mechanism A750 is driven by a motor, a second discharge hole 730 is arranged below the dust removing mechanism A740, the lower end of the first discharge hole 720 is connected with the lower end of the second discharge hole 730 through a pipeline, and air is sent by the high-pressure air pump 760;
7) The manipulation unit 900: the control unit 900 is provided with a control console 910 and a computer 920, the status of the equipment in the production process is provided with data by the information acquisition device, and the MES system regulates and controls according to the acquired data.
It should be noted that in the actual production process, the number of production units may be greater to meet the actual production requirement. Mn in the prior art 3 O 4 The circulation among the working procedures is discontinuous, manual operation is needed, the production efficiency and the equipment utilization rate are greatly reduced, and based on the fact, the inventor of the invention connects production equipment of the working procedures one by utilizing pipelines, and material circulation is realized. But based on different Mn 3 O 4 For Mn of 3 O 4 The production equipment and the reaction condition requirements of the process are different, for example, when the grinding mechanism is a vertical mill, the obtained material is thicker, when the ball mill is adopted, the obtained material is thinner, and when the reaction is carried out, the materials with different fineness are respectively conveyed to different reaction kettles for reaction, so that Mn is obtained 3 O 4 . The production line needs many-to-many production procedures, and a one-to-one conveying mode cannot meet production requirements, so that the inventor combines the production procedures with an MES system, and performs information matching between the identification information of each material conveying device received by the information acquisition device and the identification information of a corresponding production unit through an MES system database to realize Mn 3 O 4 Is suitable for the continuous production of many-to-many cross production, as shown in fig. 10.
In addition, in the whole production process of the system, the material is changed from block materials into slurry, the slurry is changed into wet materials through pressure filtration, and the wet materials are changed into powder after being dried, so that the process can involve a slurry selecting pipeline and a pumping mode, a wet material selecting conveying mode and a powder selecting negative pressure and pipeline mode.
Further, the information acquisition device is a code scanning gun, the identification information is borne by the bar codes, and the corresponding bar codes are attached to the outer surfaces of the production unit and the material conveying device. The code scanning gun obtains the above information and matches the information of the material conveying device, if the information matching is successful, the material conveying device supplies the production unit, and continuous production is realized, thereby solving the independent working modes of a plurality of units at present.
In this embodiment, thermistor temperature sensors are respectively disposed on the inner side of the reaction kettle 310, the inner side of the drying body 620, the outlet of the combustion furnace 630, and the feed inlet of the dust removing mechanism a 740; siemens pressure sensors QBE9103-P25U are respectively arranged on a feed inlet of the dedusting mechanism A740 and a pipeline connected with the extracting mechanism A750, omron/ohm Long Yewei sensors are respectively arranged on the inner side of the reaction kettle 310 and the inner side of the storage tank 410, a Metrele-Toril multi-pH sensor is arranged on the inner side of the reaction kettle 310, a Nager anti-corrosion electromagnetic flowmeter is arranged on a first conveying pipe between the stirring mechanism 220 and the reaction kettle 310, a Nager anti-corrosion electromagnetic flowmeter is arranged on a second conveying pipe between the reaction kettle 310 and the storage tank 410 and a second conveying pipe between the storage tank 410 and the plate-and-frame filter press 510, a Nager anti-corrosion electromagnetic flowmeter is arranged on a pipeline between the reaction kettle 310 and the air pump 320, and the temperature sensor, the pressure sensor, the liquid level sensor, the pH sensor and the flowmeter are all electrically connected with the terminal equipment 920.
Working principle: mn is prepared by a manganese tablet method 3 O 4 When the method comprises the following steps:
(1) mixing: grinding manganese metal sheet (purity of 99.7% or more) to particle size (D) by tower mill 210 50 ) Manganese slurry with the particle size of 1-20 mu m can be detected by a laser particle analyzer, and the manganese slurry enters a stirring tank 220 for stirring, and when the ratio of balls to manganese sheets to pure water is (2-5): 1: (1-3), stirring at a rotation speed of 30-100 rpm for 1-2 h, and entering a reaction kettle 310 through a pipeline;
(2) reverse-rotationThe method comprises the following steps: under the condition that the reaction kettle 310 is started to be stirred, the stirring speed is 100-300 rpm, the ground slurry is pumped into the reaction kettle 310, pure water is added to the solid content of 10-40 wt%, ammonium salt is added, wherein the ammonium salt can be one or more of ammonium chloride, ammonium sulfate and ammonium nitrate, the dosage is 0.3-3 wt% of the weight of the manganese metal, and the manganese metal is converted into manganese hydroxide by utilizing the catalysis of the ammonium salt; air is introduced through the air pump 320, and the flow is 200-500m 3 And/h, oxidizing the manganese hydroxide into manganomanganic oxide by using air, controlling the pH value to be 6-8.5 in the reaction process, controlling the temperature to be 50-80 ℃, finishing the reaction after 10-18 h, monitoring the reaction pH value by a pH sensor, and in addition, in order to prevent abnormal reaction, alarming when the temperature exceeds 90 ℃ by a system;
(3) and (3) material storage: the reacted slurry is pumped into a storage tank 410 by a pump for storing the material to be filtered, a stirring device is arranged in the storage tank 410, the rotating speed is 60-150 rpm, the mixture is kept uniform, the sinking is avoided, and an alarm is given when the liquid level exceeds 85%;
(4) and (3) filter pressing: the mixture in the storage tank 410 is input into a plate-and-frame filter press 510 through a pump, a filter cake is obtained after the mixture is subjected to feeding, washing and squeezing treatment in the plate-and-frame filter press 510, a plate frame is removed by a trolley 520, the filter cake between the plate frames falls on a feeder 530 and is conveyed to a dryer 610 by the feeder 530, and the speed of the feeder 530 is 2-4 m/min;
(5) and (3) drying: the filter cake enters a dryer 610, and is dried by blowing through a combustion furnace 630 in the descending process, wherein the temperature of the combustion furnace 630 is 350-500 ℃, the filter cake dropped from the inlet air pressure at the mouth of the combustion furnace 630 is minus 500Pa to minus 100Pa is smashed by a high-speed rotating knife 640, the frequency of the high-speed rotating knife is 20-50 Hz, the smashed material is output upwards by a pipeline under the negative pressure effect of a dust remover 740, and the outlet temperature is 120-150 ℃;
(6) and (3) collecting: after the materials are output by the dryer 610, the materials are screened under the centrifugal action of the powder concentrator 710, the materials with larger mass are settled, the materials with smaller mass are output by the first discharge port 720, the materials with smaller mass are easily lifted under the negative pressure action and are output upwards by a pipeline, the materials are output by the second discharge port 730 under the action of the bag type dust collector A740 and are mixed with the materials of the first discharge port 720 through conveying equipment, wherein the air outlet temperature of the bag type dust collector A740 is 100-120 ℃, and the air outlet pressure is-3500 to-1500 Pa.
Mn preparation by manganese salt method 3 O 4 When compared with the manganese tablet method, the method does not contain the mixing materials in the step (1); in the reaction process of the step (2), under the condition of starting stirring, the manganese salt solution and the alkali liquor flow to the reaction kettle 310, and the rest steps are the same as those of the manganese flake method. The manganese salt solution comprises one of manganese sulfate, manganese chloride or manganese nitrate, and the concentration is 0.1-2.5 mol/L; the alkali solution comprises ammonia water, sodium hydroxide or potassium hydroxide solution with the concentration of 0.1-2.5 mol/L, in the embodiment, manganese sulfate solution with the concentration of 1.5mol/L is adopted as manganese salt solution, the ammonia water solution is alkali solution, and the ammonia water is prepared by adopting industrial ammonia water with the concentration of 10-22 wt%.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (2)

1. Mn based on MES system 3 O 4 A continuous production process, characterized in that the Mn 3 O 4 The preparation method adopts a manganese salt method, and comprises the following steps:
s1: modeling: inputting the production parameters into a control unit (900) comprising a MES system database;
s2: the reaction: matching a reaction unit (300) and a material conveying device input into the reaction unit (300) according to the reaction requirement, starting stirring, enabling manganese salt solution and alkali liquor to flow into a reaction kettle (310), and stopping the reaction after the reaction reaches a specified pH value; controlling the pH value to be 6-8.5 in the reaction process, controlling the temperature to be 50-80 ℃, finishing the reaction after 10-18 hours, monitoring the reaction pH value by a pH sensor, monitoring the temperature by a temperature sensor, and alarming when the temperature exceeds 90 ℃ by a system;
s3: and (3) filter pressing: the MES system determines that the filter pressing unit (500) automatically feeds;
s4: and (3) drying: according to the equipment state, the material obtained by the S3 filter pressing is transmitted to a drying unit (600) for drying;
s5: and (3) collecting: collecting the material obtained in the step S4 in a collecting unit (700);
the production line matched with the continuous production process comprises a plurality of production units, each production unit is provided with respective identification information, and the system also comprises a control unit of an MES system database; at least one material conveying device is arranged between two adjacent production units, each material conveying device is provided with respective identification information, and the identification information of each material conveying device is associated with a material state; and an information acquisition device for acquiring the identification information of the production unit from each production unit and the identification information of the material conveying device from each material conveying device, wherein the control unit is connected with the information acquisition device and binds the identification information of each material conveying device received from the information acquisition device with the identification information of the corresponding production unit through an MES system database, and the corresponding production unit is a production unit for receiving all materials associated with the identification information of the material conveying device;
the production unit comprises a reaction unit (300), a filter pressing unit (500), a drying unit (600) and a collecting unit (700), wherein a material conveying device between the reaction unit (300) and the filter pressing unit (500) comprises at least two second conveying pipes, and an electromagnetic ball valve is arranged on each second conveying pipe; the material conveying device between the filter pressing unit (500) and the drying unit (600) comprises at least one feeder; the material conveying device between the drying unit (600) and the collecting unit (700) comprises at least one third conveying pipe,
the reaction unit (300) comprises a reaction kettle (310) and an air pump (320), wherein an air inlet of the air pump (320) is positioned at the lower end of the reaction kettle (310); the filter-pressing unit (500) comprises a plate-and-frame filter press (510); the drying unit (600) comprises a flash dryer (610), a drying body (620) of the flash dryer (610) is communicated with an outlet of a combustion furnace (630), the collecting unit (700) comprises a dust removing mechanism A (740), the tail end of the dust removing mechanism A (740) is provided with an extracting mechanism A (750), the control unit (900) is provided with a control table (910) and a terminal device (920), the state of the device in the production process is provided with data by an information acquisition device, and an MES system is regulated and controlled according to the acquired data;
thermistor temperature sensors are respectively arranged at the inner side of the reaction kettle (310), the inner side of the drying body (620), the outlet of the combustion furnace (630) and the feed inlet of the dust removing mechanism A (740); siemens pressure sensor QBE9103-P25U is arranged on a feeding port of dust removing mechanism A (740) and a pipeline connected with pumping mechanism A (750) respectively, a liquid level sensor is arranged on the inner side of reaction kettle (310), a pH sensor is arranged on the inner side of reaction kettle (310), a flowmeter is arranged on a pipeline between reaction kettle (310) and air pump (320), and thermistor temperature sensor, siemens pressure sensor QBE9103-P25U, liquid level sensor, pH sensor and flowmeter are all electrically connected with terminal equipment (920).
2. Mn based on MES system according to claim 1 3 O 4 The continuous production process is characterized in that the materials after the reaction end flow into a storage unit (400), the storage unit (400) comprises a storage tank (410), a liquid level sensor is arranged on the inner side of the storage tank (410), according to the liquid level information of the storage unit (400), an MES system determines whether the materials can be discharged or not and conveys the materials to a filter pressing unit (500), and in the storage process, an alarm is given out when the liquid level exceeds 85%; the storage tank (410) is positioned on a conveying pipeline of the second conveying pipe, and a flowmeter is arranged on the second conveying pipe between the reaction kettle (310) and the storage tank (410) and between the storage tank (410) and the plate-and-frame filter press (510).
CN202110557466.1A 2021-05-21 2021-05-21 Mn based on MES system 3 O 4 Continuous production process Active CN113200570B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102701285A (en) * 2012-06-26 2012-10-03 贵州红星发展股份有限公司 Methods for preparing low specific surface area (BET) manganous manganic oxide and controlling granularity and manganous manganic oxide
CN111459105A (en) * 2020-03-31 2020-07-28 安徽山河药用辅料股份有限公司 Pharmaceutic adjuvant automation line control system
CN112573577A (en) * 2020-12-25 2021-03-30 中钢天源股份有限公司 High-quality manganous-manganic oxide and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102701285A (en) * 2012-06-26 2012-10-03 贵州红星发展股份有限公司 Methods for preparing low specific surface area (BET) manganous manganic oxide and controlling granularity and manganous manganic oxide
CN111459105A (en) * 2020-03-31 2020-07-28 安徽山河药用辅料股份有限公司 Pharmaceutic adjuvant automation line control system
CN112573577A (en) * 2020-12-25 2021-03-30 中钢天源股份有限公司 High-quality manganous-manganic oxide and preparation method thereof

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