CN115403026A - Intelligent control system and method for preparing carbon-based material of negative electrode of energy storage battery - Google Patents
Intelligent control system and method for preparing carbon-based material of negative electrode of energy storage battery Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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- H—ELECTRICITY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/00—Electrodes
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
The application relates to an intelligent control system and method for preparing carbon-based materials of an anode of an energy storage battery, wherein the control system comprises at least one pretreatment device used for obtaining a pretreatment material; the crushing device is used for obtaining primary crushed materials; the grinding device is used for obtaining powder; the particle size measuring device is used for obtaining particle size parameters; the pickling device is used for pickling the powder to obtain a purified material; an ion concentration detection device for detecting the concentration of anions and the concentration of cations in the pickling solution during pickling; the control device is used for obtaining and adjusting the pickling amount and the pickling reaction temperature of the first pickling according to the particle size parameters, and adjusting the pickling amount and the pickling reaction temperature of the subsequent two-stage or multi-stage pickling according to the anion concentration and the cation concentration; and a high-temperature carbonization device. The processing that this application has different raw materials of adaptation reduces the work load of technology adjustment, promotes the effect of amorphous carbon-based negative pole material's quality.
Description
Technical Field
The application relates to the field of battery cathode material preparation control, in particular to an intelligent control system and method for preparing an energy storage battery cathode carbon-based material.
Background
The research on the cathode material plays an important role in promoting the commercialization of new energy batteries, and particularly in the energy storage industry, a suitable cathode material which is mainly represented by a sodium battery is not found, so that the industrialization breakthrough is not realized, and the cathode material which is not easy to precipitate sodium dendrite, low in cost and excellent in performance is not found.
The negative electrodes of energy storage batteries currently under study include carbon-based, titanium-based, organic, alloys, and the like. Among them, research on carbon-based materials has mainly focused on graphitic carbon materials, nanocarbon materials, and amorphous carbon materials. Due to thermodynamic reasons, sodium ions are difficult to be embedded into graphite layers and form stable intercalation compounds with carbon, so that the graphite is difficult to be used as a negative electrode material of the energy storage battery.
The nano carbon material mainly comprises graphene, a carbon nano tube and the like, and is mainly used for adsorbing and storing sodium on the surface to realize rapid charge and discharge, but the practical application of the nano carbon material is difficult to obtain due to the problems of low first-cycle coulomb efficiency, poor cycle performance and the like. The amorphous carbon-based negative electrode material with larger disorder degree has higher sodium storage specific capacity, lower sodium storage potential and excellent cycling stability, and is the sodium ion battery negative electrode material with the most application prospect.
In the microstructure of amorphous carbon, the arrangement of the curved carbon layered structure is messy and irregular, and has defects, and the crystal grains are tiny and contain a small amount of heteroatoms. The van der Waals force between the carbon layers is weak, random translation, bending and rotation can be generated in a disordered way, if the structure between the carbon layers can be changed into the disordered way to be ordered, a strong cross-linking effect is established, the carbon layers are prevented from sliding under the mechanical action, the amorphous carbon can be effectively pushed to serve as the material of the energy storage battery cathode, and the development of the energy storage battery industry is promoted.
The amorphous carbon-based negative electrode material can be prepared from anthracite, coke or petroleum coke as a raw material, or biomass materials such as coconut shells, peanut shells, straws and the like through crushing and purifying the raw materials, and then performing high-temperature carbonization and other processes. In order to improve the quality of the product, manufacturers need to accurately control various process parameters in the processing process.
In view of the above-mentioned related technologies, the inventors believe that the difficulty of process treatment is different due to the difference in carbon content and impurity content in different raw materials, so that the processes of crushing, purification and the like need frequent adjustment, the workload is large, and the change of the previous process affects the subsequent process, so that the quality of the final product is difficult to ensure.
Disclosure of Invention
First aspect, for the processing of the different raw materials of adaptation, reduce the work load of technology adjustment, promote amorphous carbon-based anode material's quality, this application provides an energy storage battery negative pole carbon-based material preparation intelligence control system.
The application provides a pair of energy storage battery negative pole carbon-based material preparation intelligence control system adopts following technical scheme:
an energy storage battery negative electrode carbon-based material preparation intelligent control system comprises:
at least one pretreatment device, which is used for performing at least one of the procedures of cleaning and dewatering on the raw materials and obtaining a pretreatment material;
the crushing device is used for crushing the pretreated material to obtain a primary crushed material;
the grinding device is used for grinding the primary crushed materials to obtain powder;
the particle size measuring device is used for performing particle size measurement on the powder and acquiring particle size parameters;
the pickling device is used for pickling the powder to obtain a purified material;
the ion concentration detection device is used for detecting the concentration of anions and the concentration of cations in the pickling solution during pickling;
the control device is connected with the particle size measuring device, the ion concentration detection device and the pickling device and is used for obtaining and adjusting the pickling amount and the pickling reaction temperature of primary pickling according to particle size parameters and adjusting the pickling amount and the pickling reaction temperature of subsequent two-stage or multi-stage pickling according to the anion concentration and the cation concentration; and
and the high-temperature carbonization device is used for carrying out high-temperature treatment on the purified material and generating a microstructure in the purified material.
By adopting the technical scheme, the raw materials are pretreated and then crushed; and then grinding the mixture to form powder particles, removing impurities such as metals, oxides and the like after multistage acid washing to obtain a purified material, and performing high-temperature carbonization and other steps to obtain the amorphous carbon-based negative electrode material. The particle sizes of the crushed and ground powder are different, and generally comprise D10, D50, D90, D99 and the like, the particle size of the raw material with higher hardness is larger, the particle size of the raw material with lower hardness is smaller, the impurity components and the content in the powder can influence the hardness of the raw material, and the particles with the same quality are smaller, the larger the integral surface area is, the larger the contact area with the pickling solution is, the larger the pickling amount required for the first time is, the anion concentration and the cation concentration can measure the completion degree of the first pickling, whether the impurities are completely removed or not, and whether the pickling is required to be continued or not, so that the control device can determine the pickling amount, the pickling frequency and the like required by the powder according to the particle size parameters, thereby improving the pickling efficiency, improving the resource utilization rate, adapting to the processing of different raw materials, reducing the workload of process adjustment, and improving the quality of the amorphous carbon-based negative electrode material.
Preferably, the screening device is further included, and is used for filtering the primary crushed aggregates to obtain a first screened material with a particle size smaller than a first set particle size and a second screened material with a particle size not smaller than the first set particle size, and performing secondary crushing or multiple crushing on the second screened material to obtain secondary crushed aggregates;
the grinding device is used for grinding the first screened material to obtain primary selected powder, and grinding the secondary crushed material to obtain secondary selected powder;
the sampling device is used for collecting samples of primary selection powder and secondary selection powder according to a set sampling proportion, wherein the set sampling proportion adopts a mass ratio, a volume ratio or a quantity ratio; and
the impurity analysis device is used for analyzing the components of the samples of the primary selection powder and the secondary selection powder;
the control device is connected with the impurity analysis device and used for adjusting the total amount of pickling solution for pickling and the pickling reaction temperature according to the component composition of the impurities.
By adopting the technical scheme, the sampling device can sample the second screened material, so that the workload of measurement and data analysis is reduced, meanwhile, the real conditions of the first screened material and the secondary crushed material can be simulated as accurately as possible in a mass ratio, volume ratio or quantity ratio mode, and the precision of subsequent processes such as acid dosage prediction and the like is improved; the hardness of raw materials can be reflected to the broken condition, and hardness generally receives factors such as impurity to influence, therefore accessible crushing technology and crocus technology divide into at least two kinds with the raw materials, and the roughly composition of impurity is analyzed by impurity analysis device again, and different compositions need the acid of different ratios to corrode to be furnished with different reaction temperature, can regard as the important parameter of adjusting pickling volume and pickling reaction temperature to promote pickling efficiency.
Preferably, the system further comprises a water washing device, the water washing device is used for performing deionization operation on the purified material, and the control device is connected with the water washing device and is used for generating a water washing amount according to the acid washing amount and the concentrations of anions and cations in the waste liquid obtained by acid washing.
By adopting the technical scheme, redundant ions in the purification material can be removed through the deionized water, and the water washing amount is calculated through the hydrogen ion plasma concentration and the like of the waste liquid of the acid washing, so that the waste of the deionized water can be reduced, and the resource utilization rate is improved.
Preferably, the sieving device comprises a basic filtering piece and a grading filtering piece, wherein the basic filtering piece is used for filtering the primary crushed materials to obtain a first sieving material with a particle size smaller than a first set particle size and a second sieving material with a particle size not smaller than the first set particle size;
the grading filter piece is used for carrying out step screening on the second screened materials, the second screened materials of each step correspond to different particle size ranges, the second screened materials of each step correspond to different crushing technological parameters of two-stage crushing or multi-stage crushing respectively, the crushing technological parameters comprise crushing strength, the control device adjusts the corresponding crushing technological parameters according to the steps of the second screened materials, and the crushing technological parameters comprise the crushing strength.
By adopting the technical scheme, the second screened material is subjected to step screening, so that raw material particles with different particle size ranges are divided, and different crushing technological parameters are designated, so that the technological parameters of the crushing device are optimized, and the resource utilization rate is improved.
Preferably, the device further comprises a carbon content detection device and a specific surface area measurement device, the carbon content detection device is used for detecting the carbon content of the particles, the specific surface area measurement device is used for measuring the specific surface area of the purified material, and the control device is connected to the carbon content detection device and the specific surface area measurement device and is used for obtaining the carbon content and the specific surface area of the purified material after acid washing and judging whether the acid washing reaches the standard according to the change condition of the carbon content and the specific surface area of the purified material.
By adopting the technical scheme, the carbon content of the particles can be detected by the carbon content detection device, so that the content of impurities can be reversely judged according to the carbon content, the pickling amount can be adjusted according to the content of the impurities, the waste of hydrochloric acid and hydrofluoric acid can be reduced, and the resource utilization rate can be improved; the specific surface area of the purified material can be detected by a specific surface area measuring device, and in most cases, the larger the specific surface area change of the particles is, the more surface micropores are, the stronger the ion disintercalation capability is, so that the electrochemical performance of the final product can be improved; meanwhile, the purification material not only needs to meet the requirement of carbon purity, but also needs to meet the requirement of specific surface area, so that the purification material and the purification material are combined with each other, the strict control of links is realized, and the quality of a final product is improved.
Preferably, the device further comprises a waste recovery device, the waste recovery device is connected to the control device, the control device obtains the carbon content of the second sieved material of each step through the carbon content detection device, and when the carbon content is lower than a first set value, the control device controls the waste recovery device to recover the second sieved material of the step and return the second sieved material to the intermediate bin for treatment.
By adopting the technical scheme, the secondary powder which is difficult to crush and has larger particle size often contains more impurities and lower carbon content, the acid dosage, the deionized water dosage, the energy consumption and the like required by the treatment process are correspondingly increased, and even the resource consumption is possibly higher than the value of the secondary powder, so that the raw material particles with overhigh purification cost are screened out by a carbon content detection mode, and the effects of reducing the cost and saving energy are achieved.
Preferably, the high temperature carbonization device includes the carbide furnace, be provided with at least two temperature control districts that are used for carrying out the high temperature carbonization to the purification material in the carbide furnace, every temperature control district is provided with at least one temperature detector, temperature detector is used for gathering the temperature of purification material in real time, controlling means includes processing module, processing module is used for calculating the temperature rate of change and according to the current temperature rate of change real-time calculation arrive appointed temperature's estimated time, outputs alarm signal when estimated time exceeds the settlement duration.
Through adopting above-mentioned technical scheme, realize the subregion temperature control to the purification material through the temperature control district, the inside and outside difference in temperature of avoiding purification material centralized heating or cooling to lead to is too big, but thermodetector real-time supervision purification material's temperature variation, especially in the intensification stage, for guaranteeing graphite's quality, need strictly control each intensification and the length of heat preservation stage, consequently judge through temperature variation rate whether the purification material intensifies or cools down too fast, whether can guarantee abundant heat preservation time, thereby promote graphite finished product's quality.
Preferably, each temperature control area is provided with a temperature regulator, the temperature regulator is connected to the control device and is used for regulating heating efficiency or cooling efficiency, the control device receives and responds to the alarm signal to start temperature compensation, and the heating efficiency or cooling efficiency of the temperature regulator is adjusted according to the difference between the estimated time and the set time.
By adopting the technical scheme, the temperature of the purification material can be adjusted through the temperature regulator, the higher the heating/cooling efficiency is, the faster the temperature change of the purification material is, the temperature to be compensated can be estimated according to the difference between the estimated time and the set time, the heating/cooling efficiency is changed along with the temperature change of the purification material, the phenomena that the temperature of the purification material exceeds the expected temperature and the like caused by the time lag of temperature conduction are reduced, and the quality of the purification material is improved.
Preferably, the high-temperature carbonization device further comprises a partition temperature difference control module, wherein the partition temperature difference control module is used for acquiring temperature values of the purified materials in each temperature control area at the current moment, generating a reference temperature line according to the current set temperature, screening the purified materials with the temperature deviation from the reference temperature line, the difference value of which exceeds a preset limit value, collecting a temperature change curve of the purified materials, and generating an abnormal report according to the temperature change curve and a preset abnormal tracing standard.
By adopting the technical scheme, some impurities possibly exist in the purified material and can generate extra heat or absorb heat in the process of heating and carbonizing, and the abnormal tracing standard records the possible reaction or change of various impurities in each temperature stage, so that the actual condition of the abnormal temperature change of the purified material and the abnormal tracing standard can conveniently and timely reflect the carbonization condition of the purified material, the treatment is convenient and timely, the potential safety hazard is reduced, and the production quality of graphite is guaranteed.
In order to adapt to the processing of different raw materials, reduce the workload of process adjustment and improve the quality of the amorphous carbon-based anode material, the application provides a control method in the preparation process of the carbon-based material of the anode of the energy storage battery, which adopts the following technical scheme:
a control method in the preparation process of an anode carbon-based material of an energy storage battery applies the anode carbon-based material of the energy storage battery to prepare an intelligent control system, and comprises the following steps:
acquiring the particle size parameter of the powder after the milling process;
obtaining the anion concentration and the cation concentration in the pickling solution during pickling;
obtaining and adjusting the pickling amount and the pickling reaction temperature of the first pickling according to the particle size parameters;
and adjusting the pickling amount and the pickling reaction temperature of the subsequent two-stage or multi-stage pickling according to the anion concentration and the cation concentration.
By adopting the technical scheme, the particle with the same quality is smaller in particle size and larger in integral surface area, the larger the contact area with the pickling solution is, the larger the pickling amount required for the first time is, the finishing degree of the first pickling can be measured by the anion concentration and the cation concentration, whether impurities are completely removed or not, and whether pickling is required to be continued or not, so that the control device can determine the pickling amount, the pickling frequency and the like required by powder according to the particle size parameters, the pickling efficiency is improved, the resource utilization rate is improved, the processing of different raw materials is adapted, the workload of process adjustment is reduced, and the quality of the amorphous carbon-based negative electrode material is improved.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the control device can determine the pickling amount, the pickling times and the like required by the powder according to the particle size parameters, so that the pickling efficiency is improved, the resource utilization rate is improved, the control device is suitable for processing of different raw materials, the workload of process adjustment is reduced, and the quality of the amorphous carbon-based negative electrode material is improved;
2. the raw materials can be divided into at least two types through a crushing process and a grinding process, then an impurity analysis device is used for analyzing the approximate components of impurities, different components need different proportions of acid for corrosion, and different reaction temperatures are matched, so that the different components can be used as important parameters for adjusting the pickling amount and the pickling reaction temperature, and the pickling efficiency is improved;
3. realize the subregion temperature control to the purification material through the temperature control district, the inside and outside difference in temperature of avoiding purification material centralized heating or cooling to lead to is too big, but thermodetector real-time supervision purification material's temperature variation, especially in the intensification stage, for guaranteeing the quality of graphite, need strictly be long of each intensification and heat preservation stage of accuse, consequently judge through temperature variation rate that the purification material heaies up or cools down too fast, whether can guarantee abundant heat preservation time, thereby promote the off-the-shelf quality of graphite.
Drawings
Fig. 1 is a system block diagram of an intelligent control system for preparing carbon-based materials of an anode of an energy storage battery according to an embodiment of the application.
Fig. 2 is a flow chart of the preparation of the carbon-based material for the anode of the energy storage battery according to the example of the application.
FIG. 3 is a flow chart of the crushing process parameter adjustment step according to an embodiment of the present application.
Fig. 4 is a flow diagram of the screen recovery of the second screened material of an embodiment of the present application.
FIG. 5 is a flow chart of the estimation of the total amount of pickling solution and the amount of first pickling solution in the examples of the present application.
Fig. 6 is a flowchart of temperature control of the purified material in the high-temperature carbonization process according to the example of the present application.
Fig. 7 is a flowchart for tracing back a temperature abnormality in the high-temperature carbonization step of the purified material according to the example of the present application.
Detailed Description
The present application is described in further detail below with reference to the accompanying drawings.
The embodiment of the application discloses an intelligent control system for preparing a carbon-based material of an anode of an energy storage battery. Referring to fig. 1, the intelligent control system for preparing the carbon-based material of the anode of the energy storage battery comprises:
the pretreatment device can adopt a dryer, a cleaning machine and the like, is used for performing cleaning, dehydration and other procedures on the raw materials, reduces impurities, moisture and the like on the surface of the raw materials, facilitates subsequent processing, and finally obtains a pretreatment material after the raw materials are pretreated;
the crushing device can adopt a jaw crusher and the like and is used for crushing the pretreated material to obtain primary crushed material with uniform particle size;
the sieving device is used for filtering the primary crushed aggregates to obtain first sieved materials with the particle size smaller than a first set particle size and second sieved materials with the particle size not smaller than the first set particle size, and crushing the second sieved materials for two times or multiple times to obtain secondary crushed aggregates;
the powder grinding device can adopt mechanical powder grinding or airflow powder grinding, the embodiment adopts a combined type, the mechanical powder grinding is firstly carried out on the first sieved material and the second crushed material through a ball mill, then airflow powder grinding is carried out through an airflow mill, the first sieved material and the second crushed material can be ground to 10-100 micrometers, and the materials are collected through a cyclone dust collector to obtain powder;
the pickling device adopts a pickling tank and is used for pickling powder to obtain a purified material, the pickling can adopt mixed acid of hydrochloric acid, hydrofluoric acid and the like, impurities in most of the powder can be corroded and dissolved, high-purity carbon is obtained, meanwhile, a large number of micropores are formed on powder particles, the ion desorption in the charging and discharging process is facilitated, and the electrochemical performance of the powder is improved.
The water washing device adopts a water washing pool, and carries out deionization operation on the purified material through deionized water to remove redundant anions and cations;
and the high-temperature carbonization device is used for carrying out high-temperature treatment on the purified material to generate a microstructure in the purified material so as to generate the amorphous carbon-based negative electrode material.
Specifically, the raw materials are sequentially subjected to pretreatment, crushing, screening, grinding, acid washing, water washing and high-temperature carbonization to finally form the amorphous carbon-based negative electrode material, wherein the acid washing and the water washing are alternately performed and are performed in multiple stages.
In the crushing process, because the hardness of partial impurities in the raw materials is higher, the impurities are not easy to be converted into particles with small particle sizes through a simple crushing mode, the crushing degree difference of the raw material particles after one-time crushing is large, and the particle size difference is large.
Referring to fig. 1 and 2, the sieving device includes a basic filtering element and a classifying filtering element, both of which employ a classifier, such as an air classifier, a jet classifier, etc., for filtering the primary crushed material to obtain a first sieved material smaller than a first set particle size and a second sieved material not smaller than the first set particle size, wherein the first set particle size may take any value of 5-10 mm.
Referring to fig. 1 and 3, the first material is generally a raw material with less impurities or lower impurity hardness due to smaller particle size, while the second material is generally a raw material with more impurities or higher impurity hardness due to larger particle size, and the overall carbon content and impurity content are greatly different. And the grading filter element is used for carrying out step screening on the second screened materials, and the second screened materials of each step correspond to different particle size ranges. For example, the material is divided into a first stage below 5mm, a second stage below 5mm to 10mm, a third stage below 10mm to 15mm, and so on, wherein the second material of each step corresponds to different crushing process parameters of the second-stage crushing or the multi-stage crushing, and the crushing process parameters comprise crushing strength.
The crushing device is connected with a control device, the control device adopts a computer, an industrial personal computer and the like and is used for adjusting corresponding crushing technological parameters according to the steps of the second screened materials, for example, the first group of crushing technological parameters of the 5mm-10mm steps are adopted, the second group of crushing technological parameters of the 10 mm-15 mm steps are adopted, and the specific crushing technological parameters can be adjusted in the process or the result feedback after the process, so that the particle size of the secondary crushed materials can reach the standard of the first screened materials after the crushing, and meanwhile, the working load of the crushing device can be reduced to the minimum, thereby improving the crushing efficiency.
Referring to fig. 1 and 4, the control device is connected with a sampling device, a waste recovery device and a carbon content detection device, the sampling device can adopt a manipulator for sampling according to a set sampling proportion, and the set sampling proportion adopts a mass ratio, a volume ratio or a quantity ratio. The sampling device randomly grabs a small part of samples from the second sieving materials of each step, the samples are subjected to steps of grinding and the like, then the carbon content of each sample is detected through the carbon content detection device, the carbon content detection device can adopt a chromatograph and the like, the carbon content in the samples is detected through chromatography, the control device judges whether the second sieving materials of the step reach the standard or not according to the average carbon content of the samples, when the carbon content is lower than a first set value, the actually obtained amorphous carbon-based negative electrode material after acid washing and high-temperature carbonization is lower than the paid process cost, the control device controls the waste material recovery device to recover the second sieving materials of the step and return the second sieving materials to the intermediate bin for treatment, and the materials in the intermediate bin can be used for other purposes.
The waste recovery device can adopt a conveyer belt and is used for receiving a second sieved material with unqualified carbon content after sieving by the grader, wherein the value of the first set value is obtained according to a simulation algorithm, the consumption of pickling solution and deionized water can be calculated according to the carbon content, the impurity content and the impurity components, the process consumption basic value obtained by an experiment is combined, the subsequent rough process cost of the second sieved material can be estimated, and the cost difference required by different process precision requirements is large, so that the process is not particularly expanded and described herein.
First sifting material and the second sifting material that remains up to standard are in the crocus technology, and milling equipment carries out the crocus to first sifting material, obtains the primary election powder, carries out the crocus to the secondary crushed aggregates, obtains the secondary selection powder, because the carbon content and the impurity composition of primary election powder and secondary selection powder generally differ great, consequently separately preserve and handle, adopt different technological parameters.
In order to sample and analyze the powder material, the purified material and the like conveniently and determine subsequent process steps and process parameters, the control device is also connected with a sampling device, a particle size measuring device, an ion concentration detecting device, an impurity analyzing device and a specific surface area measuring device. The impurity analyzer may be an analyzer such as a chromatograph or a scanning electron microscope, or may be a chemical test method for analyzing the approximate components of a sample of the secondary powder.
Referring to fig. 1 and 5, the sampling device further includes a vacuum feeder, which can dispersedly sample the primary powder and the secondary powder, analyze the components of the sample by the impurity analyzer, detect the approximate components, such as calcium carbonate, e.g., metal oxide, etc., and then detect the proportion of the components, and then adjust the reaction chemical formula of the components and the mixed acid to calculate the proportion of the mixed acid to be consumed with the same mass, thereby estimating the required mixed acid consumption with the same mass of the primary powder and the secondary powder, reducing the waste of the mixed acid, and simultaneously improving the impurity removal rate and the carbon purity as much as possible.
Because different impurities react with the mixed acid at different temperatures, the temperature range in the pickling process needs to be defined according to the composition of the components detected in the primary selected powder and the secondary selected powder, the temperature range of the pickling reaction temperature is determined according to the components of the impurities, the impurities react with the mixed acid most fully in the determined temperature range, and the reaction product is easy to dissolve and separate, so that the impurity removal rate is improved.
For example, the proportion of the impurity a is a%, the proportion of the impurity B is B%, the mixed acid required for each gram of the impurity a is x G, the mixed acid required for each gram of the impurity B is y G, the impurity a and the impurity B achieve the maximum degree of acid washing reaction at 80 ℃, and are easy to separate, the acid washing reaction temperature is controlled to be about 80 ℃, the total consumption of acid washing liquid is V = M (a% × x + B% × y) + M G, M is the mass of the primary powder or the secondary powder, G is a constant, and M G is used as redundant quantity to compensate the error of the estimation result.
The above is the pickling dosage required by the whole of the primary selection powder and the secondary selection powder, and in the pickling process, insoluble reaction products may cover the surface of the particles to form a protective layer, so that the primary pickling cannot reach the maximum degree, and therefore, the multistage pickling is required. The particle size measuring device is needed, and can adopt a laser particle size analyzer and be used for performing particle size measurement on the powder and obtaining particle size parameters, wherein the particle size parameters comprise roundness, average diameter and the like. The particle size of the particles with the same mass is smaller, the whole surface area is larger, the contact area with the pickling solution is larger, and therefore the pickling amount required for the first time is larger, the particle size parameters of samples in the primary selection powder and the secondary selection powder are collected through the particle size measuring device, the smaller the particle size is, the higher the pickling amount ratio of the first pickling is, and conversely, the larger the particle size is, the lower the pickling amount ratio of the first pickling is. For example, the first pickling solution usage = V x F arc (K/N)%, K is a constant, N is the average diameter of the particles, K and F are both constants, V is the total pickling solution usage, and the total formula is: the amount of the first pickling solution is = [ M (a%. X + b%. Y) + M.G ]. F.arctan (K/N)%.
The control device obtains the whole pickling solution consumption according to the impurity analysis data given by the impurity analysis device, generates the pickling solution consumption of primary pickling according to the particle size parameters, and then needs to adopt the ion concentration detection device to carry out ion concentration detection on the mixed acid waste liquid after pickling to determine the specific pickling reaction condition and reaction degree. The ion concentration detection device can adopt a liquid chromatograph and is used for detecting the anion concentration and the cation concentration in the pickling solution during pickling and simultaneously detecting the anion concentration and the cation concentration in the waste liquid after pickling.
For example, when the hydrogen ion concentration in the waste liquid is high, it means that the ratio of the amount of the pickling solution used for the first pickling is too high, and the amount of the pickling solution used for the subsequent pickling needs to be decreased, and when the hydrogen ion concentration in the waste liquid is low, it means that the ratio of the amount of the pickling solution used for the first pickling is too low, and the amount of the pickling solution used for the subsequent pickling needs to be increased. And if the concentration of the hydrogen ions in the waste liquid is higher than a preset value, the waste liquid can be recycled, so that the resource waste is reduced. The hydrogen ion concentration and the like can be used as feedback quantity for adjusting the G value and the like in a calculation formula of the total consumption of the pickling solution, and can also be used as a reference for adjusting the consumption of the pickling solution for subsequent pickling.
And after the acid washing process, a water washing process is needed, the detection result of the anion concentration and the cation concentration obtained by the detection of the ion concentration detection device can be used as the reference of deionization, and the higher the anion concentration and the cation concentration are, the higher the using amount of the deionized water is. Therefore, the control device generates the dosage of the deionized water according to the dosage of the pickling solution of the previous stage of pickling and the concentrations of the anions and the cations in the waste liquid obtained by pickling. And after the first washing, the ion concentration detection device can recheck, and the injection proportion of the deionized water is adjusted by taking the recheck result as feedback, so that the using amount of the deionized water is more accurate, the resource waste is reduced, and the separation and dehydration are convenient.
The primary selection powder and the secondary selection powder are subjected to acid washing and water washing to obtain a purified material, the purified material can enter a high-temperature carbonization process after being audited to reach the standard, otherwise, the acid washing and the water washing processes are continuously carried out, wherein in the auditing process, the purified material needs to be continuously sampled by a sampling device, the carbon content of a sample of the purified material is detected by a carbon content detection device, and meanwhile, the specific surface area of the sample of the purified material is measured by a specific surface area measurement device.
The specific surface area measuring device can adopt a BETA201B model full-automatic static volumetric method specific surface and pore size analysis tester for measuring the specific surface area of the particles, wherein the specific surface area refers to the surface area of the porous solid substance in unit mass, the larger the specific surface area is, the more micropores are formed on the surface of the particles, and the more micropores are, the ion can be conveniently desorbed, so that the electrochemical performance is stronger.
The control device is connected with the carbon content detection device and the specific surface area measurement device, is used for obtaining the carbon content and the specific surface area of the sample of the purified material, compares the carbon content and the specific surface area with preset set values respectively, and judges according to a comparison result:
if the carbon content and the specific surface area both reach the standard, judging that the acid washing is finished, and directly entering a high-temperature carbonization procedure;
if the carbon content reaches the standard and the specific surface area does not reach the standard, the carbon is used as an auxiliary material for selection, and the high-temperature carbonization process is not performed for the time;
if the carbon content does not reach the standard and the specific surface area reaches the standard, continuing to perform the steps of acid washing and water washing, and modifying the process parameters of subsequent acid washing and water washing according to the carbon content;
and if the carbon content and the specific surface area do not reach the standard, judging whether to continue to reserve or not according to the difference value between the carbon content and the specific surface area and the set target value, if the simulated purification cost is higher than a preset threshold value, recovering the carbon content and the specific surface area as waste materials, and if the simulated purification cost is lower than the preset threshold value, continuing to perform the steps of acid washing and water washing.
Referring to fig. 1 and 6, the powder material is subjected to acid washing and water washing and then enters a high-temperature carbonization process, the high-temperature carbonization process is completed by a high-temperature carbonization device, the high-temperature carbonization device comprises a carbonization furnace, the up-to-standard purified material can be placed in a high-temperature resistant container and then is placed in the carbonization furnace for high-temperature carbonization, and the interior of the carbonization furnace needs to be controlled to maintain an anaerobic environment during the period, so that the purified material is controlled to be uniformly heated and cooled. The temperature control process is as follows: room temperature to 600 ℃ for 3 hours; keeping the temperature at 600 ℃ for 1 hour; 600 to 850 ℃ for 1 hour; keeping the temperature at 850 ℃ for 1 hour; 850 to 1250 ℃ for 1.5 hours; keeping the temperature at 1250 ℃ for 1 hour; 1250 ℃ to 1400 ℃ for 0.5 hour; preserving the heat for 2 hours at 1400 ℃; finally, the temperature is reduced for about 6.9 hours.
The carbonization furnace is internally provided with at least two temperature control areas for carrying out high-temperature carbonization treatment on the purified materials, each temperature control area is provided with at least one temperature detector, and each temperature control area is provided with a temperature regulator, and the temperature detectors can adopt MARS series monochromatic infrared thermometers and are used for collecting the temperature of each purified material in real time. Temperature regulation ware, thermodetector all connect in controlling means, and controlling means includes processing module, and processing module is used for calculating the temperature change rate of purifying the material in every temperature control district, and temperature regulation ware, thermodetector all connect in processing module. The temperature regulator can adopt an electric heating mode or a microwave heating mode to heat the purified material.
When the purified material is in a heat preservation state, checking whether the temperature change rate is larger than a set normal value, if so, indicating that the heat preservation does not reach the standard, and outputting an alarm signal by the processing module; if not, the heat preservation is normal.
When the purified material is in a temperature rising or reducing stage, the estimated time of reaching the specified temperature is calculated in real time according to the current temperature change rate, and an alarm signal is output when the estimated time exceeds the set time. The alarm signal can prompt the staff to adjust the heating efficiency or the cooling efficiency of the carbonization furnace. To improve the control accuracy, the temperature-raising and temperature-lowering time can be limited to a time range, for example:
when the estimated time is shorter than a first set time, reducing the heating efficiency in a temperature-rising state and reducing the temperature-reducing efficiency in a temperature-reducing state;
when the estimated time is longer than the second set time, the heating efficiency is improved in a temperature rising state, and the cooling efficiency is improved in a temperature reducing state;
the second set duration is greater than the first set duration.
The processing module receives and responds to the alarm signal to start temperature compensation, adjusts the heating efficiency or the cooling efficiency of the temperature regulator according to the difference value between the predicted time and the set time, and the set time can be converted into a time range, for example, from a first set time to a second set time, as follows:
the regulating quantity of the heating efficiency can be subjected to PID control according to the difference value, namely when the estimated time is lower than the first set time length, the absolute value of the difference value between the estimated time and the first set time length is a reference quantity of the PID control; and when the estimated time is higher than the second set time length, the absolute value of the difference between the estimated time and the second set time length is a reference quantity of PID control.
Referring to fig. 1 and 7, the high-temperature carbonization device further includes a partition temperature difference control module, which may be a processor, for acquiring temperature values of the purified materials in each temperature control area at the current time, generating a reference temperature line according to the current set temperature, screening the purified materials whose temperature deviates from the reference temperature line by a difference value exceeding a preset limit value, collecting a temperature change curve of the purified materials, and generating an abnormal report according to the temperature change curve and a preset abnormal tracing standard.
Specifically, the anomaly tracing standard records chemical reactions or physical/chemical property changes of various impurities at various temperature stages, and partial impurities react at high temperature or are converted into other physical/molecular states to generate heat or absorb heat, so that the temperature of the purified material is locally changed. The current set temperature is a system set temperature value of each time node in the temperature rise control process of the carbonization furnace for processing the purification material, for example, the purification material needs to reach 300 ℃ in 90 minutes and 600 ℃ in 180 minutes when the purification material starts to rise in temperature, and the current set temperature is taken as a reference temperature line at the current moment.
The subregion difference in temperature control module is according to the difference of purification material and benchmark temperature line, the positive and negative and the temperature change curve of difference again, judges the reaction condition and the reaction intensity of purification material to this and unusual retrospective standard contrast, thereby the high temperature carbonization condition of automatic feedback purification material, early warning in advance makes things convenient for the suggestion staff in time to handle unusual condition, promotes the production security. The information of the abnormal purification material position, the abnormal temperature change condition, the possible impurities, the subsequent possible abnormal conditions, the reaction intensity, the hidden danger level and the like is mainly fed back in the abnormal report.
The impurity analysis device detects the component composition of impurities in the primary selection powder and the secondary selection powder, the impurity components possibly remain partially after acid washing and water washing, reaction can be generated in the high-temperature carbonization process and the overall temperature of the purification material is influenced, so the component composition of the impurities is obtained by the subarea temperature difference control module, the abnormal condition of the high-temperature carbonization process of the purification material is estimated according to the reaction of various impurities possibly generated at high temperature, and judgment conditions are formulated, for example, when the temperature abnormally rises, reverse temperature compensation is performed in advance through the temperature regulator, and the abnormal change of the temperature is inhibited. The temperature reverse compensation amount of the temperature regulator can be estimated according to the component content of the impurity. The residual amount of impurities after pickling was estimated as follows: the residual amount of impurities can be analyzed by an impurity analysis device, or the carbon content detected by a carbon content detection device can be used for reversely deducing the loss ratio of the impurities, namely, the components of the impurities are reduced in equal proportion, for example, the carbon content is purified from 97 percent to 99.5 percent, the total amount of the impurities is reduced by 1/6, the reduction ratio of each component in the impurities is approximately equal, so that the residual amount of each component of the impurities can be roughly estimated, and the temperature reverse compensation amount can be estimated according to the residual amount.
The implementation principle of the energy storage battery negative electrode carbon-based material preparation intelligent control system in the embodiment of the application is as follows: the crushing process is optimized by carrying out step screening on the primary crushed aggregates, the load on crushing equipment is reduced, the types of impurities are simply classified, and the subsequent targeted process parameter adjustment is facilitated. Through sampling in advance and detecting the carbon content of raw materials, in time reject the more raw materials of impurity and waste recovery, prevent further technology cost loss. Through impurity analysis's mode, carry out the accurate distribution of pickling solution to different raw materials to this waste that reduces the pickling solution promotes resource utilization, promotes the edulcoration rate and the carbon purity of purification material simultaneously. Realize the accurate temperature control of purification material through the high temperature carbonization device, in time carry out temperature compensation to the temperature abnormal change of purification material to carry out unusual traceing back and early warning to unusual object, promote production security and final product quality.
The above are preferred embodiments of the present application, and the scope of protection of the present application is not limited thereto, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (10)
1. The utility model provides an energy storage battery negative pole carbon-based material preparation intelligence control system which characterized in that: at least one pretreatment device, which is used for performing at least one of the procedures of cleaning and dewatering on the raw materials and obtaining a pretreatment material;
the crushing device is used for crushing the pretreated material to obtain a primary crushed material;
the grinding device is used for grinding the primary crushed materials to obtain powder;
the particle size measuring device is used for performing particle size measurement on the powder and acquiring particle size parameters;
the pickling device is used for pickling the powder to obtain a purified material;
an ion concentration detection device for detecting the concentration of anions and the concentration of cations in the pickling solution during pickling;
the control device is connected with the particle size measuring device, the ion concentration detection device and the pickling device and is used for obtaining and adjusting the pickling amount and the pickling reaction temperature of primary pickling according to particle size parameters and adjusting the pickling amount and the pickling reaction temperature of subsequent two-stage or multi-stage pickling according to the anion concentration and the cation concentration; and
and the high-temperature carbonization device is used for carrying out high-temperature treatment on the purified material and generating a microstructure in the purified material.
2. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 1, wherein: the screening device is used for filtering the primary crushed aggregates to obtain first screened materials with the particle size smaller than a first set particle size and second screened materials with the particle size not smaller than the first set particle size, and performing secondary crushing or multiple crushing on the second screened materials to obtain secondary crushed aggregates;
the grinding device is used for grinding the first screened material to obtain primary selected powder, and grinding the secondary crushed material to obtain secondary selected powder;
the sampling device is used for collecting samples of primary powder and secondary powder according to a set sampling proportion, and the set sampling proportion adopts a mass ratio, a volume ratio or a quantity ratio; and
the impurity analysis device is used for analyzing the components of the samples of the primary selection powder and the secondary selection powder;
the control device is connected with the impurity analysis device and is used for adjusting the total amount of the pickling solution for pickling and the pickling reaction temperature according to the component composition of the impurities.
3. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 2, wherein: still include the washing device, the washing device is used for carrying out the deionization operation to the purification material, controlling means is connected with the washing device for anion and the cation concentration generation washing volume according to pickling volume and the pickling gained waste liquid.
4. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 3, wherein: the screening device comprises a basic filtering piece and a grading filtering piece, wherein the basic filtering piece is used for filtering primary crushed materials to obtain a first screened material with a particle size smaller than a first set particle size and a second screened material with a particle size not smaller than the first set particle size;
the grading filter piece is used for carrying out step screening on the second screened materials, the second screened materials of each step correspond to different particle size ranges, the second screened materials of each step correspond to different crushing technological parameters of two-stage crushing or multi-stage crushing respectively, the crushing technological parameters comprise crushing strength, the control device adjusts the corresponding crushing technological parameters according to the steps of the second screened materials, and the crushing technological parameters comprise the crushing strength.
5. The intelligent control system for preparing carbon-based materials of the anode of the energy storage battery according to claim 4, wherein: the device comprises a carbon content detection device and a specific surface area measurement device, wherein the carbon content detection device is used for detecting the carbon content of particles, the specific surface area measurement device is used for measuring the specific surface area of the purified material, and the control device is connected with the carbon content detection device and the specific surface area measurement device and is used for obtaining the carbon content and the specific surface area of the purified material after acid washing and judging whether the acid washing reaches the standard according to the change conditions of the carbon content and the specific surface area of the purified material.
6. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 5, wherein: the device further comprises a waste recovery device, the waste recovery device is connected to the control device, the control device obtains the carbon content of the second sieved material of each step through the carbon content detection device, and the control device controls the waste recovery device to recover the second sieved material of the step and return the second sieved material to the middle bin for treatment when the carbon content is lower than a first set value.
7. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 6, wherein: the high temperature carbonization device includes the carbide furnace, be provided with at least two temperature control districts that are used for carrying out the high temperature carbonization to the purification material in the carbide furnace, every temperature control district is provided with at least one thermodetector, thermodetector is used for gathering the temperature of purification material in real time, controlling means includes processing module, processing module is used for calculating the temperature rate of change and reaches the estimated time of appointed temperature according to current temperature rate of change real-time calculation, outputs alarm signal when estimated time exceeds the settlement duration.
8. The intelligent control system for preparing carbon-based materials of the anode of the energy storage battery as claimed in claim 7, wherein: every temperature control district is provided with temperature regulator, temperature regulator connects in controlling means for adjust heating efficiency or cooling efficiency, controlling means receives and starts temperature compensation in response to alarm signal, and according to estimated time and the difference adjustment temperature regulator's of length of setting for heating efficiency or cooling efficiency.
9. The intelligent control system for preparing the carbon-based material for the anode of the energy storage battery according to claim 8, wherein: the high-temperature carbonization device further comprises a partition temperature difference control module, wherein the partition temperature difference control module is used for acquiring the temperature values of the purified materials in each temperature control area at the current moment, generating a reference temperature line according to the current set temperature, screening the purified materials with the temperature deviation exceeding a preset limit value from the reference temperature line, acquiring the temperature change curve of the purified materials, and generating an abnormal report according to the temperature change curve and a preset abnormal tracing standard.
10. A control method in the preparation process of carbon-based materials of an anode of an energy storage battery is realized by applying the intelligent control system for the preparation of carbon-based materials of an anode of an energy storage battery according to claims 1 to 9, and is characterized by comprising the following steps:
acquiring the particle size parameter of the powder after the grinding process;
obtaining the anion concentration and the cation concentration in the pickling solution during pickling;
obtaining and adjusting the pickling amount and the pickling reaction temperature of primary pickling according to the particle size parameters;
and adjusting the pickling amount and the pickling reaction temperature of the subsequent two-stage or multi-stage pickling according to the anion concentration and the cation concentration.
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