CN212893947U - Intelligent production system of battery-grade aluminum sulfate - Google Patents

Intelligent production system of battery-grade aluminum sulfate Download PDF

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Publication number
CN212893947U
CN212893947U CN202022162847.3U CN202022162847U CN212893947U CN 212893947 U CN212893947 U CN 212893947U CN 202022162847 U CN202022162847 U CN 202022162847U CN 212893947 U CN212893947 U CN 212893947U
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unit
reaction
tail gas
aluminum sulfate
production system
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司东峰
司思
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Zibo Boshan Win Win Chemical Co ltd
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Zibo Boshan Win Win Chemical Co ltd
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Abstract

The utility model discloses an intelligent production system of battery-grade aluminum sulfate, which comprises a material mixing unit, a reaction unit, a crystallization unit, a crushing unit and a drying unit which are connected in sequence, wherein the crushing unit is also connected with the reaction unit to realize the pre-crushing of reaction raw materials; the reaction unit is also connected with a tail gas condensation recovery unit, and the tail gas condensation recovery unit is respectively connected with a tail gas treatment unit and the reaction unit; the material mixing unit, the reaction unit, the crystallization unit, the crushing unit, the drying unit, the tail gas condensation and recovery unit and the tail gas treatment unit are all in communication connection with and controlled by a PLC control module. The production period of the battery-grade aluminum sulfate prepared by the intelligent production system is reduced by more than half at least, the purity of the finally obtained battery-grade aluminum sulfate is up to 99.9 percent, and the iron content is lower than 50 ppm.

Description

Intelligent production system of battery-grade aluminum sulfate
Technical Field
The utility model relates to an aluminum sulfate production technical field, concretely relates to intelligent production system of battery level aluminum sulfate.
Background
The iron-free aluminum sulfate is widely applied to the fields of high-grade paper, high-grade fabrics, food leavening agents, batteries, rubber and the like. At present, the annual production capacity of the iron-free aluminum sulfate in China reaches over 100 million tons, but the demand of international and domestic markets can not be met. The industrial preparation method of the iron-free aluminum sulfate is that the bauxite and the sulfuric acid are pressurized to react to obtain liquid aluminum sulfate, and the liquid aluminum sulfate is crystallized after iron is removed to obtain hydrated aluminum sulfate crystals; slowly heating the hydrated aluminum sulfate crystals to gradually dehydrate the hydrated aluminum sulfate crystals, cooling, solidifying and crushing the hydrated aluminum sulfate crystals after complete dehydration to obtain the finished product. The reaction mode has harsh conditions, high requirements on a reaction kettle and large loss. In addition, the iron removal process generally adopts the following 3 modes: 1) the iron is removed by adopting the ion exchange resin, but the ion exchange resin poisoning caused by iron ions is difficult to regenerate at present; 2) the iron is removed by adopting potassium ferrocyanide and potassium ferricyanide, but the method has larger environmental pollution problem and potential safety hazard; 3) the solvent extraction method is adopted for removing iron, but the problems of complex process operation, large loss, poor iron removal efficiency and the like exist. In addition, most of reaction equipment adopted by the existing process is more traditional, the automation degree is low, the labor cost is high, and the production efficiency is low, so that the reaction equipment is a key factor which seriously restricts the production capacity of the non-iron aluminum sulfate. Therefore, it is urgent to further develop new production technology of iron-free aluminum sulfate to match the development status thereof in various fields.
SUMMERY OF THE UTILITY MODEL
In view of the above-mentioned problem that prior art exists, the utility model provides a battery grade aluminum sulfate's intelligent production system. The technical scheme of the utility model is that:
the intelligent production system of the battery-grade aluminum sulfate comprises a material mixing unit, a reaction unit, a crystallization unit, a crushing unit and a drying unit which are sequentially connected, wherein the crushing unit is also connected with the reaction unit to realize the pre-crushing of reaction raw materials; the reaction unit is also connected with a tail gas condensation recovery unit, and the tail gas condensation recovery unit is respectively connected with a tail gas treatment unit and the reaction unit; the material mixing unit, the reaction unit, the crystallization unit, the crushing unit, the drying unit, the tail gas condensation and recovery unit and the tail gas treatment unit are all in communication connection with and controlled by a PLC control module.
Further, the reaction unit at least comprises a first reaction kettle and a second reaction kettle, wherein a CPU module, an input module and an output module are loaded on the first reaction kettle and the second reaction kettle, and the functions of the CPU module comprise: and sending feedback information from the input module and the output module to the CPU, receiving a control instruction from the CPU, and sending the feedback information to the input module and the output module respectively.
Preferably, the feed inlet and the discharge outlet of the first reaction kettle and the second reaction kettle are provided with electromagnetic valves, the electromagnetic valves are provided with alarm devices, the electromagnetic valves and the alarm devices are respectively connected with the CPU module, when the electromagnetic valves are not closed tightly, the electromagnetic valves can generate a feedback signal to be sent to the CPU module, and the CPU module controls the alarm devices to give out an alarm.
Furthermore, the mixing tank, the first reaction kettle and the second reaction kettle are also provided with pressure sensors on conveying pipelines, and the pressure sensors are connected with the PLC control module.
Preferably, the crystallizer is a steel strip crystallizer.
Further, the crushing unit at least comprises a crushing machine and a crusher which are sequentially connected, a first vibrating feeder is arranged on the crushing machine, a second vibrating feeder is arranged on the crusher, and a conveying mechanism is arranged between the crushing machine and the crusher.
Further, the tail gas treatment unit at least comprises a heat exchanger and a gas-liquid separator.
Preferably, the tail gas treatment unit comprises a spray tower, a neutralization tower and a brine separator which are connected in sequence, and a water outlet of the brine separator is connected with the tail gas condensation and recovery unit so as to use the waste water separated from the brine separator as the circulating water of the heat exchanger and the spray water of the spray tower.
Further, the production system also comprises a flow control unit, and a control valve and a control pump which correspond to the flow control unit, wherein the flow control unit at least comprises an acid flowmeter, a water flowmeter and a material flowmeter, the control valve at least comprises an acid valve, a water valve and a material valve, and the control pump at least comprises an acid pump, a water pump and a material pump.
By adopting the system, the intelligent production process of the battery-grade aluminum sulfate comprises the following steps:
(1) preparing alkali liquor in a mixing unit: introducing quantitative sodium hydroxide and water into a mixing unit and uniformly mixing;
(2) preparation of battery grade aluminium sulphate in the reaction unit: introducing the alkali liquor obtained in the step (1) into a reaction unit, introducing the ferro-aluminum ore into the reaction unit for reaction, and introducing a sulfuric acid solution for reaction after the reaction is finished; after the reaction is finished, continuously adding sodium diethyldithiocarbamate solution to carry out iron removal reaction;
(3) recovering and treating tail gas in a tail gas condensation and recovery unit and a tail gas treatment unit: introducing tail gas generated in the reaction process of introducing the sulfuric acid solution in the step (2) into a tail gas condensation recovery unit for condensation recovery, introducing partial condensed tail gas droplets into the reaction unit again for reaction, and introducing uncondensed tail gas into a tail gas treatment unit for treatment;
(4) the reaction product is crystallized in a crystallization unit: introducing the final product obtained from the reaction unit into a crystallization unit for crystallization;
(5) and respectively crushing and drying the crystallized product in a crushing unit and a drying unit to obtain the product.
Further, the final concentration of the sodium hydroxide solution in the step (1) is 20-25%.
Further, the concentration of the sulfuric acid solution in the step (2) is 45-50%.
Further, the concentration of the sodium diethyldithiocarbamate solution in the step (2) is 20-25%, and the molar ratio of the sodium diethyldithiocarbamate to iron in the ferro-aluminum ore is not lower than 2.
Preferably, the production process further comprises: and respectively using the waste water and the strong brine from the tail gas treatment unit as circulating water of the tail gas condensation and recovery unit and raw materials for preparing industrial salt.
In a third aspect, the utility model provides a battery grade aluminum sulfate, which is obtained by adopting the production process.
Compared with the prior art, the beneficial effects of the utility model are that:
firstly, the intelligent production system of the utility model adopts a full-automatic production mode, all processes can be controlled and completed by the PLC control module, thereby greatly saving the labor cost and the time cost, and each link can be considered as thoroughly as possible, for example, a mixing unit is arranged in front of the reaction unit for preparing alkali liquor, so as to relieve the use pressure of the reaction kettle; and the tail gas condensation and recovery unit and the tail gas treatment unit are additionally arranged, and the tail gas generated in the reaction process is recycled and treated and then discharged, so that the harm to the environment is greatly reduced.
Secondly, the production process of the utility model adopts a two-step reaction mode that bauxite reacts with alkali liquor firstly and then reacts with sulfuric acid solution, and then removes iron through sodium diethyldithiocarbamate solution, finally battery-grade aluminum sulfate can be obtained, the purity is as high as 99.9%, and the iron content is lower than 50 ppm. The existing traditional production mode directly adopts the pressure reaction of bauxite and sulfuric acid to obtain bauxite, although the mode is completed in one step, the reaction condition is harsh, concentrated sulfuric acid and pressure are needed, the complexity and the danger degree in the operation are high, and the iron removal effect is not ideal.
Drawings
Fig. 1 is a schematic structural diagram of the intelligent production system of the present invention.
Fig. 2 is a schematic diagram of the structure control of the intelligent production system of the present invention.
In fig. 1 and 2, 1, a mixing tank, 2, a first reaction tank, 3, a second reaction tank, 4, a CPU module, 5, an input module, 6, an output module, 7, an alarm device, 8, a pressure sensor, 9, a crystallizer, 10, a solenoid valve at a discharge and feed position of the reaction tank, 11, a fragmenting machine, 12, a pulverizer, 13, a first vibrating feeder, 14, a second vibrating feeder, 15, a conveying mechanism, 16, a dryer, 17, a tubular heat exchanger, 18, a buffer tank, 19, a spray tower, 20, a neutralization tower, 21, a brine separator, 22, a PLC control module, 23, an acid flow meter, 24, a water flow meter, 25, a material flow meter, 26, an acid pump, 27, a water pump, 28, a material pump, 29, an acid valve, 30, a water valve, 31, a material valve, 32, other control valves, 33, a mixer on the mixing tank, 34, a gas-liquid separator, 35, and other pumps.
Detailed Description
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms 'mounted', 'connected' and 'connected' are to be construed broadly, e.g. as being fixedly connected, detachably connected or integrally connected; can be mechanically or electrically connected; the two elements may be directly connected or indirectly connected through an intermediate medium, or may be communicated with each other inside the two elements, or may be wirelessly connected or wired connected. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.
In the description of the present invention, it is to be noted that the specific conditions are not specified in the examples, and the description is made according to the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present invention will be further described with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
As shown in fig. 1 and 2, the present embodiment provides an intelligent production system for battery-grade aluminum sulfate, which includes a material mixing tank 1, a reaction unit, a crystallizer 9, a crushing unit and a dryer 16, which are connected in sequence, wherein the crushing unit is further connected to the reaction unit to implement pre-crushing of reaction raw materials; the reaction unit is also connected with a tail gas condensation recovery unit, and the tail gas condensation recovery unit is respectively connected with the tail gas treatment unit and the reaction unit. In addition, the mixing tank 1, the reaction unit, the crystallizer 9, the crushing unit, the dryer 16, the tail gas condensation and recovery unit and the tail gas treatment unit are all in communication connection with the PLC control module 22 and are controlled by the PLC control module 22. The structure of each unit is described in detail as follows:
the mixing tank 1 is used for preparing the sodium hydroxide solution in advance, and the mixing tank 1 is connected with a water pump 27 and a sodium hydroxide quantitative feeder 33 and is internally provided with a stirring device. The PLC control module 22 controls the opening and closing of corresponding electromagnetic valves on the sodium hydroxide conveying pipeline and the like in the feeding process of the mixing tank 1, and the quantitative feeding of the sodium hydroxide raw materials is automatically completed by combining the data of the weighing sensor. In order to monitor whether the conveying pipeline is blocked, a pressure sensor 8 and an alarm device 7 can be additionally arranged on the sodium hydroxide conveying pipeline. In addition, a piece crusher is sometimes used in the preparation process of the sodium hydroxide, so that a piece crusher can be arranged before the mixing tank as required, a conveying mechanism 15 is arranged between the piece crusher and the mixing tank, and the piece crusher is also connected with the reaction kettle for pre-crushing the ferro-aluminium ore.
The reaction unit comprises a first reaction kettle 2 and a second reaction kettle 3 which are connected with each other, wherein the first reaction kettle 2 is used for carrying out the reaction between the bauxite and the sodium hydroxide, and the second reaction kettle 3 is used for carrying out the reaction between the sodium metaaluminate and the sulfuric acid and removing iron. Reation kettle 2 and reation kettle two 3 all adopt acid and alkali-resistance's reation kettle, and the bottom is equipped with heating device, and there is agitating unit inside to all have on the reation kettle to reserve mouthful and be used for loading distillation plant and reflux unit. In addition, the first reaction kettle 2 and the second reaction kettle 3 are both provided with a CPU module 4, an input module 5 and an output module 6, and the connection mode between the CPU module and the input module is shown in FIG. 2. The CPU module 4 adopts Siemens 400 series, the feeding process of the reaction kettle is automatically completed by controlling the opening and closing of corresponding electromagnetic valves on a conveying pipeline and the like by the PLC control module 22 through the CPU module 4 and combining the data of a weighing sensor to realize the quantitative feeding of the raw materials. Similarly, in order to monitor whether the conveying pipeline is blocked, a pressure sensor 8 and an alarm device 7 can be additionally arranged on the conveying pipeline. In addition, the electromagnetic valves 10 are arranged at the feed inlets and the discharge outlets of the first reaction kettle 2 and the second reaction kettle 3, the electromagnetic valves 10 are also provided with alarm devices 7, the electromagnetic valves and the alarm devices are respectively connected with the CPU module 4, when the electromagnetic valves are not tightly closed, the electromagnetic valves can generate a feedback signal to be sent to the CPU module 4, the CPU module 4 controls the alarm devices 7 to send out an alarm, and then the safety monitoring effect on the reaction kettles is achieved.
The production system further comprises a flow control unit, and a control valve and a control pump corresponding to the flow control unit, in this embodiment, the flow control unit comprises an acid flow meter 23, a water flow meter 24, and a material flow meter 25 (specifically, reaction liquid from the first reaction kettle), which are respectively installed on the pipelines between the second reaction kettle 3, the mixing tank 1, the first reaction kettle 2, and the second reaction kettle 3, the control valve comprises an acid valve 29, a water valve 30, and a material valve 31, and the control pump at least comprises an acid pump 26, a water pump 27, and a material pump 28, which respectively correspond to the acid flow meter 23, the water flow meter 24, and the material flow meter 25.
The crystallizer 9 is preferably a steel band crystallizer, and the steel band crystallization technology has the advantages of high cooling efficiency and rapid and uniform crystallization, and has good effect on the crystallization process of aluminum sulfate.
In this embodiment, the crushing unit only adopts a two-stage crushing device, including the successively connected chipper 11 and crusher 12, the chipper 11 is provided with the first vibrating feeder 13, the crusher 12 is provided with the second vibrating feeder 14, and a conveying mechanism 15 is further provided between the chipper 11 and the crusher 12.
The drier is a common drying device sold in the market.
The tail gas condensation recovery unit comprises a tubular heat exchanger 17, a gas-liquid separator 34 and a buffer tank 18, wherein a feed inlet of the tubular heat exchanger 17 is connected with a gas outlet of a second reaction kettle 3, a circulating water inlet of the tubular heat exchanger 17 is connected with a water outlet of a brine separator 21 of the tail gas treatment unit, a circulating water outlet of the tubular heat exchanger 17 is connected with a water inlet of a spray tower 19 spray pipeline of the tail gas treatment unit, a discharge outlet of the tubular heat exchanger 17 is connected with an inlet of the gas-liquid separator 34, a gas outlet of the gas-liquid separator 34 is connected with a feed inlet of the spray tower 19 of the tail gas treatment unit, a liquid outlet of the gas-liquid separator 34 is connected with the buffer tank 18, and the buffer tank 18 is connected with.
The tail gas treatment unit comprises a spray tower 19, a neutralization tower 20 and a brine separator 21 which are connected in sequence, the waste water separated by the brine separator 21 is used as circulating water of the tubular heat exchanger 17, the circulating water enters the spray tower 19 again to be used as spray water for removing waste gas, and the strong brine separated from the brine separator is used as a raw material for preparing industrial salt.
The PLC control module 22 adopts Siemens S7300 series, and the communication between the PLC control module and an upper computer is realized through an Ethernet switch.
Example 2
The embodiment provides an intelligent production process of battery-grade aluminum sulfate, which is used for pilot-scale production in zibo boshan win-win chemical limited company, and adopts the production system of the embodiment 1, and comprises the following steps:
(1) preparing alkali liquor in a mixing tank: introducing quantitative sodium hydroxide and water into a mixing tank, and uniformly mixing to obtain a sodium hydroxide solution with the final concentration of 22.3%;
(2) preparation of battery grade aluminium sulphate in the reaction unit: introducing the sodium hydroxide lye obtained in the step (1) into a first reaction kettle, and introducing pre-crushed ferro-aluminum ore into the first reaction kettle for reaction, wherein the molar ratio of sodium ions in the sodium hydroxide solution to aluminum ions in the ferro-aluminum ore is 1.5: 1, continuously evaporating moisture generated in the reaction process at the reaction temperature of about 100 ℃; after the reaction of the first reaction kettle is finished, introducing a second reaction kettle when the temperature is reduced to below 60 ℃, and then introducing a sulfuric acid solution for reaction, wherein the heating is not needed in the reaction process, the concentration of the sulfuric acid solution is 50%, and the adding amount of sulfuric acid is that the molar ratio of sulfate radical to aluminum ions in the aluminum-iron ore is 2: 1, counting; and after the reaction is finished, continuously adding a sodium diethyldithiocarbamate solution into a second reaction kettle to perform iron removal reaction, wherein the concentration of the sodium diethyldithiocarbamate solution is 23.5%, and the molar ratio of the sodium diethyldithiocarbamate to iron in the ferro-aluminum ore is 3.5.
(3) Recovering and treating tail gas in a tail gas condensation and recovery unit and a tail gas treatment unit: introducing tail gas generated in the reaction process of introducing the sulfuric acid solution in the step (2) into a tail gas condensation recovery unit for condensation recovery, introducing partial condensed tail gas droplets into the reaction unit again for reaction, and introducing uncondensed tail gas into a tail gas treatment unit for treatment;
(4) the reaction product is crystallized in a crystallization unit: introducing the final product obtained from the reaction unit into a crystallization unit for crystallization;
(5) and respectively crushing and drying the crystallized product in a crushing unit and a drying unit to obtain the product.
In addition, the waste water and the strong brine from the tail gas treatment unit are respectively used as circulating water of the tail gas condensation and recovery unit and raw materials for preparing industrial salt, and the circulating water can also be used as spray water of a spray tower.
By adopting the method of the embodiment to produce the multi-batch battery grade aluminum sulfate, the production period of the finally obtained aluminum sulfate product is reduced by at least half compared with the production period of the traditional process and device, the purity of the aluminum sulfate is up to 99.9 percent, wherein the iron content is below 50ppm, and the lowest iron content can reach 25 ppm. And the waste discharge amount of the process is low, and is reduced by at least more than 70 percent compared with the waste discharge amount of the traditional process.
To sum up, the utility model discloses an intelligent production system adopts full automated production mode, and all processes can all be accomplished through PLC control module control, have practiced thrift human cost and time cost widely to greatly reduced its harm to the environment. The utility model discloses a production technology passes through the bauxite and reacts with alkali liquor earlier and then reacts with sulphuric acid solution two-step reaction mode, later through the deironing of diethyl dithiocarbamate solution, finally can obtain battery grade aluminium sulfate, and purity is up to 99.9%, and iron content is less than 50 ppm.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be considered as the protection scope of the present invention.

Claims (9)

1. The utility model provides an intelligent production system of battery grade aluminum sulfate which characterized in that: the device comprises a material mixing unit, a reaction unit, a crystallization unit, a crushing unit and a drying unit which are connected in sequence, wherein the crushing unit is also connected with the reaction unit to realize the pre-crushing of reaction raw materials; the reaction unit is also connected with a tail gas condensation recovery unit, and the tail gas condensation recovery unit is respectively connected with a tail gas treatment unit and the reaction unit; the material mixing unit, the reaction unit, the crystallization unit, the crushing unit, the drying unit, the tail gas condensation recovery unit and the tail gas processing unit are all in communication connection with and controlled by the PLC control module.
2. The intelligent production system of battery grade aluminum sulfate according to claim 1, characterized in that: the reaction unit at least comprises a first reaction kettle and a second reaction kettle, wherein the first reaction kettle and the second reaction kettle are loaded with a CPU module, an input module and an output module, and the CPU module has the functions of: and sending feedback information from the input module and the output module to the CPU, receiving a control instruction from the CPU, and sending the feedback information to the input module and the output module respectively.
3. The intelligent production system of battery grade aluminum sulfate according to claim 2, characterized in that: the feeding port and the discharging port of the first reaction kettle and the second reaction kettle are respectively provided with an electromagnetic valve, the electromagnetic valves are provided with alarm devices, the electromagnetic valves and the alarm devices are respectively connected with the CPU module, when the electromagnetic valves are not closed tightly, the electromagnetic valves can generate a feedback signal to be sent to the CPU module, and the CPU module controls the alarm devices to give out an alarm.
4. The intelligent production system of battery grade aluminum sulfate according to claim 2 or 3, characterized in that: and the material mixing unit, the first reaction kettle and the second reaction kettle are also provided with pressure sensors on conveying pipelines, and the pressure sensors are connected with the PLC control module.
5. The intelligent production system of battery grade aluminum sulfate according to claim 1, characterized in that: the crystallization unit is a steel strip crystallizer.
6. The intelligent production system of battery grade aluminum sulfate according to claim 1, characterized in that: the crushing unit at least comprises a crushing machine and a crusher which are sequentially connected, a first vibrating feeder is arranged on the crushing machine, a second vibrating feeder is arranged on the crusher, and a conveying mechanism is arranged between the crushing machine and the crusher.
7. The intelligent production system of battery grade aluminum sulfate according to claim 1, characterized in that: the tail gas treatment unit at least comprises a heat exchanger and a gas-liquid separator.
8. The intelligent production system of battery grade aluminum sulfate according to claim 7, characterized in that: the tail gas treatment unit comprises a spray tower, a neutralization tower and a brine separator which are sequentially connected, wherein a water outlet of the brine separator is connected with the tail gas condensation recovery unit, so that waste water separated from the brine separator is used as circulating water of the heat exchanger and spray water of the spray tower.
9. The intelligent production system of battery grade aluminum sulfate according to claim 1, characterized in that: the production system also comprises a flow control unit, and a control valve and a control pump which correspond to the flow control unit, wherein the flow control unit at least comprises an acid flow meter, a water flow meter and a material flow meter, the control valve at least comprises an acid valve, a water valve and a material valve, and the control pump at least comprises an acid pump, a water pump and a material pump.
CN202022162847.3U 2020-09-28 2020-09-28 Intelligent production system of battery-grade aluminum sulfate Expired - Fee Related CN212893947U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111994933A (en) * 2020-09-28 2020-11-27 淄博市博山双赢化工有限公司 Intelligent production system and production process of battery-grade aluminum sulfate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111994933A (en) * 2020-09-28 2020-11-27 淄博市博山双赢化工有限公司 Intelligent production system and production process of battery-grade aluminum sulfate

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