Iron phosphate yellow material low-water-consumption washing and membrane concentration integrated system
The integrated system of low-water-consumption washing and membrane concentration of iron phosphate yellow material solves the problems of high water consumption and high wastewater treatment costs in existing technologies, and achieves efficient washing and concentration, thereby improving production continuity and capacity.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-21
- Publication Date
- 2026-03-24
AI Technical Summary
The existing iron phosphate yellow washing process consumes a lot of water resources, generates a large amount of high-salinity wastewater, has high wastewater treatment costs, low washing efficiency, poor production continuity, and limited production capacity.
The system adopts an integrated washing and membrane concentration system with low water consumption using iron phosphate yellow material. It includes an n-stage washing and concentration unit. Through a pulping tank, membrane module, concentrate tank and desalination tank, combined with sensors and control devices, the membrane fouling status is monitored in real time and the backwashing frequency is dynamically adjusted to achieve efficient washing and concentration.
It significantly reduces water consumption, improves washing efficiency and capacity, lowers wastewater treatment costs, ensures process stability and continuity, and avoids water waste.
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Figure CN224024720U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to chemical equipment technical field especially relates to a kind of low water consumption washing and membrane concentration integration system of iron phosphate yellow material. BACKGROUND
[0002] As the key precursor of lithium-ion battery cathode material (such as lithium iron phosphate), the purity of iron phosphate has a decisive influence on the electrochemical performance (such as capacity, cycle life) of the battery. The traditional iron phosphate yellow material washing process mainly removes impurity ions (such as SO4 2- , Na + , etc.) by water washing, including primary water washing and multi-stage countercurrent washing.
[0003] When washing iron phosphate yellow material, ≥20 tons of washing water per ton of iron phosphate yellow material is required for washing, and multiple repeated water washing is required to meet the purity requirements (such as Na + content <50ppm). At the same time, a large amount of high-salinity wastewater (containing sulfate, sodium salt, etc.) is generated during washing, which is difficult to treat subsequently. Therefore, the existing iron phosphate yellow material washing process not only consumes a large amount of water resources, but also generates a large amount of high-salinity wastewater, resulting in high wastewater treatment costs and high environmental protection costs. In addition, the existing iron phosphate yellow material washing process requires conventional centrifugal or filter pressing equipment, and the washing cycle is as long as 8 hours or more, resulting in low solid-liquid separation efficiency, poor production continuity and limited production capacity.
[0004] The applicant believes that the existing iron phosphate yellow material washing process has at least the following defects:
[0005] 1. Not only consumes a large amount of water resources, but also generates a large amount of high-salinity wastewater, resulting in high wastewater treatment costs.
[0006] 2. Low washing efficiency, resulting in poor production continuity and limited production capacity. INVENTION CONTENTS
[0007] The utility model discloses a kind of low water consumption washing and membrane concentration integration system of iron phosphate yellow material to solve the technical problem that the existing technology in iron phosphate yellow material washing process exists water resource consumption is huge, also generates a large amount of high-salinity wastewater, wastewater treatment cost is high.
[0008] To solve the above problems, the utility model adopts the following technical solutions:
[0009] In the first aspect, the present application provides a kind of low water consumption washing and membrane concentration integration system of iron phosphate yellow material, characterized in that it includes control device and washing concentration device, the washing concentration device is n level, n ≥ 1, and n is natural number, the washing concentration device includes beating kettle, membrane component, concentrated water tank and fresh water tank;Wherein,
[0010] The beating kettle is provided with a feeding port of yellow iron phosphate material, and is connected with a water inlet pipe and a liquid outlet pipe, and the liquid outlet pipe is connected with a pressure sensor and a liquid outlet pump;
[0011] The membrane assembly has a concentrated chamber liquid inlet, a concentrated chamber liquid outlet, a dilute chamber liquid inlet and a dilute chamber liquid outlet; the concentrated chamber liquid inlet is connected with the liquid outlet pipe of the beating kettle;
[0012] The concentrated chamber liquid outlet is connected with a concentrated water tank through a first concentrated chamber liquid outlet pipeline, and the first concentrated chamber liquid outlet pipeline is connected with a first flow sensor; the dilute chamber liquid outlet is connected with a dilute water tank through a first dilute chamber liquid outlet pipeline, and the first dilute chamber liquid outlet pipeline is connected with a second flow sensor;
[0013] It also comprises a backwashing pipeline; the backwashing pipeline comprises a dilute chamber liquid inlet pipe, a second concentrated chamber liquid outlet pipeline and a second dilute chamber liquid outlet pipeline; the dilute chamber liquid inlet pipe is connected with the liquid outlet pipe of the beating kettle through a first valve; one end of the second concentrated chamber liquid outlet pipeline is connected with the first concentrated chamber liquid outlet pipeline through a second valve, and the other end of the second concentrated chamber liquid outlet pipeline is connected with the dilute water tank; the second dilute chamber liquid outlet pipeline is connected with the first dilute chamber liquid outlet pipeline through a third valve, and the other end of the second dilute chamber liquid outlet pipeline is connected with the concentrated water tank;
[0014] The pressure sensor, the liquid outlet pump, the first flow sensor, the second flow sensor, the first valve, the second valve and the third valve are electrically connected with the control device respectively.
[0015] The technical scheme adopted by the utility model can achieve the following beneficial effects:
[0016] (1) The low-water-consumption washing and membrane concentration integrated system for yellow iron phosphate material in the application comprises an n-stage washing and concentration device, n≥1, n is a natural number, and the system is designed in a washing and concentration integrated manner and is suitable for efficient washing and concentration of iron phosphate-based materials in the fields of lithium battery materials and catalyst carriers. When the system in the application is used for washing and concentrating yellow iron phosphate material, a beating kettle is used to perform beating treatment through mechanical stirring, the agglomeration of iron phosphate particles is broken, uniform iron phosphate suspension is formed, local blockage during subsequent membrane assembly filtration is avoided, the solid content of the iron phosphate suspension is controlled to be 10% to 30%, and the flowability of the iron phosphate suspension is ensured, thereby facilitating subsequent processes.
[0017] (2) The low water consumption washing and membrane concentration integrated system of the iron phosphate yellow material in the application, in the application process, based on the first flow sensor, the second flow sensor and the pressure sensor, the membrane pollution state is judged in real time, and the frequency of backwashing is dynamically adjusted. Before the membrane module treatment, the concentration water and the fresh water flow variation threshold value are set, and the pressure sensor pressure variation threshold value is set, and the backwashing time is set. The process of membrane module treatment includes: ①Membrane concentration, the first valve, the second valve and the third valve are connected by the control device to control the membrane concentration pipeline, and the iron phosphate suspension is introduced from the concentration chamber inlet in the process of membrane concentration. The first flow sensor is used for monitoring the flow of the first concentration chamber outlet pipeline, and the second flow sensor is used for monitoring the flow of the first dilution chamber outlet pipeline. The first flow sensor and the second flow sensor send the monitoring signal to the control device, the control device receives the signal, the concentration water and the fresh water flow can be obtained, the membrane separation efficiency can be judged by the concentration water / fresh water flow ratio, the membrane surface concentration polarization is avoided, such as the sudden drop of fresh water flow may indicate membrane pollution, if the concentration water flow is significantly higher than the theoretical value, pipeline leakage or pressure imbalance should be checked. Through the first flow sensor and the second flow sensor in the membrane concentration process, the concentration water and fresh water flow can be monitored in real time to optimize the system operation and ensure the stability of the process; the pressure sensor is used for monitoring the inlet pressure of the iron phosphate suspension in the outlet pipe entering the membrane module, and the pressure sensor sends the monitoring signal to the control device, and the control device receives the signal and obtains the inlet pressure of the iron phosphate suspension entering the membrane module. Then, the concentration water flow, fresh water flow and inlet pressure are obtained to judge the degree of membrane pollution, when the set threshold value is reached, the backwashing is started by the control device. ②Backwashing, the first valve, the second valve and the third valve are connected by the control device to control the backwashing pipeline, the membrane module is backwashed by the iron phosphate suspension in the beater, in the process of backwashing, the iron phosphate suspension enters from the dilution chamber inlet, at this time, the outlet of the concentration chamber is fresh water and the outlet of the dilution chamber is concentrated water, the first flow sensor and the second flow sensor are still used to monitor the flow of fresh water and concentrated water, and the first flow sensor and the second flow sensor send the monitoring signal to the control device, and the control device receives the signal and obtains the flow of fresh water and concentrated water. Before the set backwashing time is reached, the recovery of membrane pollution can be judged by the control device to obtain the fresh water flow and the concentrated water flow, if the recovery requirement is reached, the backwashing is stopped by the control device when the backwashing time reaches the set backwashing time, and the membrane concentration is switched to; if the recovery requirement of membrane pollution is not reached when the backwashing time reaches the set backwashing time, the backwashing is considered to be continued or the pressure is increased for backwashing until the recovery requirement of membrane pollution is reached. The switching of the membrane concentration pipeline is realized by the control device to control the first valve, the second valve and the third valve to connect the membrane concentration pipeline, and the membrane concentration is continued.Since the backwashing uses the iron phosphate suspension in the beater to backwash the membrane module, the process of backwashing the membrane module is also the process of solid-liquid separation and concentration purification, and the backwashing of the membrane module by the iron phosphate suspension further avoids waste of water resources.
[0018] (3) The low-water consumption washing and membrane concentration integrated system for the iron phosphate yellow material in the application can continuously wash and concentrate the iron phosphate yellow material through the multi-stage washing and concentrating device, thereby improving the washing efficiency and production capacity of the iron phosphate yellow material. BRIEF DESCRIPTION OF DRAWINGS
[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the following embodiment or prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.
[0020] Figure 1 is a connection diagram of the first-stage washing and concentrating device in the embodiment of the application;
[0021] Figure 2 is a connection diagram of the third-stage washing and concentrating device in the embodiment of the application.
[0022] In the drawings:
[0023] 1-beater; 101-vessel body; 102-vessel cover; 103-variable frequency motor; 104-variable frequency device; 105-stirring shaft; 106-stirring paddle; 107-heating jacket; 2-feed inlet; 3-water inlet pipe; 4-liquid outlet pipe; 5-membrane module; 501-concentrate chamber liquid inlet; 502-concentrate chamber liquid outlet; 503-dilute chamber liquid inlet; 504-dilute chamber liquid outlet; 6-concentrate tank; 601-stirring motor; 602-stirring rod; 603-stirring blade; 7-dilute water tank; 8-first concentrate chamber liquid outlet pipeline; 9-first flow sensor; 10-first dilute chamber liquid outlet pipeline; 11-second flow sensor; 12-first valve; 13-second valve; 14-third valve; 15-pressure sensor; 16-concentrate water pipeline; 17-dilute water pipeline; 18-liquid outlet pump; 19-first liquid level sensor; 20-second liquid level sensor; 21-third liquid level sensor; 22-second concentrate chamber liquid outlet pipeline; 23-second dilute chamber liquid outlet pipeline; 24-dilute chamber liquid inlet pipe; 25-concentrate water pump; 26-fourth valve; 27-fifth valve; 28-sixth valve; 29-one-way valve; 30-seventh valve; 31-gas discharge pipeline; 32-gas discharge valve; 33-dilute water pump. DETAILED DESCRIPTION
[0024] It should be apparent that the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of the present application.
[0025] The terms "first", "second", and the like in the specification and claims of the present application are used to distinguish similar objects, and are not used to describe a specific order or sequence. It should be understood that the data used in this way can be interchanged under appropriate circumstances, so that the embodiments of the present application can be implemented in an order other than those illustrated or described herein, and the objects distinguished by "first", "second", etc. are generally of a kind and do not limit the number of objects, for example, the first object can be one or more. In addition, "and / or" in the specification and claims indicates at least one of the connected objects, and the character " / ", generally indicates that the front and rear associated objects are in a "or" relationship.
[0026] In the prior art, when washing the yellow iron phosphate material, ≥20 tons of washing water are consumed per ton of yellow iron phosphate material, and multiple repeated water washing is required to meet the purity requirement (such as Na + content < 50 ppm), at the same time, a large amount of high-salinity wastewater (containing sulfate, sodium salt, etc.) is generated during washing, which is difficult to treat subsequently. Therefore, the existing yellow iron phosphate material washing process removes impurity ions by water washing, which not only consumes a large amount of water resources, but also generates a large amount of high-salinity wastewater, resulting in high wastewater treatment cost and high environmental protection cost accounting for a high proportion of production cost. Moreover, the existing yellow iron phosphate material washing process needs to rely on conventional centrifugal or filter pressing equipment, and the washing period is as long as 8 hours or more, and the solid-liquid separation efficiency is low, resulting in poor production continuity and limited production capacity.
[0027] To solve the above problems in the related art, the present application provides a yellow iron phosphate material low-water-consumption washing and membrane concentration integrated system, which will be described in detail below in combination with Figure 1 and Figure 2 The yellow iron phosphate material low-water-consumption washing and membrane concentration integrated system provided by the present application will be described in detail through specific embodiments and application scenarios.
[0028] A yellow iron phosphate material low-water-consumption washing and membrane concentration integrated system, comprising a control device and a washing and concentration device, the washing and concentration device is n stages, n ≥ 1, and n is a natural number, the washing and concentration device comprises a beating kettle 1, a membrane assembly 5, a concentrated water tank 6 and a fresh water tank 7; wherein,
[0029] The beating kettle 1 is provided with a feed inlet 2 of yellow iron phosphate material, the beating kettle 1 is connected with a water inlet pipe 3 and a liquid outlet pipe 4, and the liquid outlet pipe 4 is connected with a pressure sensor 15 and a liquid outlet pump 18;
[0030] The membrane module 5 has a concentrated chamber liquid inlet 501, a concentrated chamber liquid outlet 502, a dilute chamber liquid inlet 503 and a dilute chamber liquid outlet 504; the concentrated chamber liquid inlet 501 is connected with the liquid outlet pipe 4 of the beating kettle 1;
[0031] The concentrated chamber liquid outlet 502 is connected with the concentrated water tank 6 through a first concentrated chamber liquid outlet pipeline 8, and the first concentrated chamber liquid outlet pipeline 8 is connected with a first flow sensor 9; the dilute chamber liquid outlet 504 is connected with the dilute water tank 7 through a first dilute chamber liquid outlet pipeline 10, and the first dilute chamber liquid outlet pipeline 10 is connected with a second flow sensor 11;
[0032] The system further comprises a backwashing pipeline; the backwashing pipeline comprises a dilute chamber liquid inlet pipe 24, a second concentrated chamber liquid outlet pipeline 22 and a second dilute chamber liquid outlet pipeline 23; the dilute chamber liquid inlet pipe 24 is connected with the liquid outlet pipe 4 of the beating kettle 1 through a first valve 12; one end of the second concentrated chamber liquid outlet pipeline 22 is connected with the first concentrated chamber liquid outlet pipeline 8 through a second valve 13, and the other end of the second concentrated chamber liquid outlet pipeline 22 is connected with the dilute water tank 7; the second dilute chamber liquid outlet pipeline 23 is connected with the first dilute chamber liquid outlet pipeline 10 through a third valve 14, and the other end of the second dilute chamber liquid outlet pipeline 23 is connected with the concentrated water tank 6;
[0033] The pressure sensor 15, the liquid outlet pump 18, the first flow sensor 9, the second flow sensor 11, the first valve 12, the second valve 13 and the third valve 14 are electrically connected with a control device respectively.
[0034] The low-water-consumption washing and membrane concentration integrated system for yellow iron phosphate material in the application comprises an n-stage washing and concentration device, n≥1, and n is a natural number, and is suitable for efficient washing and concentration of iron phosphate-based materials in the fields of lithium battery materials and catalyst carriers, etc. When the system in the application is used for washing and concentrating yellow iron phosphate material, a beating kettle 1 is used to perform beating treatment through mechanical stirring, the agglomeration of iron phosphate particles is broken, a uniform iron phosphate suspension is formed, local blockage during subsequent membrane module filtration is avoided, the solid content of the iron phosphate suspension is controlled to be 10%~30%, the flowability of the iron phosphate suspension is ensured, and the subsequent process is facilitated.
[0035] The low water consumption washing and membrane concentration integrated system of the iron phosphate yellow material in the application, in the application process, based on the first flow sensor 9, the second flow sensor 11 and the pressure sensor 15, the membrane pollution state is judged in real time, and the frequency of backwashing is dynamically adjusted. Before the treatment of the membrane assembly 5, the flow variation threshold of the concentrated water and the fresh water is set, and the pressure variation threshold of the pressure sensor 15 is set, and the length of time of backwashing is set. The process of the treatment of the membrane assembly 5 includes: ①membrane concentration, the first valve 12, the second valve 13 and the third valve 14 are connected by the control device to control the membrane concentration pipeline, and in the process of membrane concentration, the iron phosphate suspension is entered from the concentrated chamber inlet 501. The first flow sensor 9 is used for monitoring the flow of the first concentrated chamber outlet pipeline 8, and the second flow sensor 11 is used for monitoring the flow of the first fresh water outlet pipeline 10. The first flow sensor 9 and the second flow sensor 11 send the monitoring signals to the control device, the control device receives the signals, the flow of the concentrated water and the fresh water can be obtained, the membrane separation efficiency can be judged by the flow ratio of the concentrated water / fresh water, the membrane surface concentration polarization is avoided, for example, if the fresh water flow suddenly drops, it may indicate that the membrane is polluted, if the concentrated water flow is significantly higher than the theoretical value, pipeline leakage or pressure imbalance needs to be checked; in the membrane concentration process, the first flow sensor 9 and the second flow sensor 11 are used for monitoring the flow of the concentrated water and the fresh water in real time, which can optimize the system operation and ensure the stability of the process; the pressure sensor 15 is used for monitoring the inlet pressure of the iron phosphate suspension in the outlet pipe 4 entering the membrane assembly 5, the pressure sensor 15 sends the monitoring signal value to the control device, and the control device receives the signal, and the inlet pressure of the iron phosphate suspension entering the membrane assembly 5 is obtained; then the degree of membrane pollution is judged by the obtained concentrated water flow, fresh water flow and inlet pressure, when the set threshold is reached, backwashing is started by the control device. ②backwashing, the first valve 12, the second valve 13 and the third valve 14 are connected by the control device to control the backwashing pipeline, the membrane assembly 5 is backwashed by the iron phosphate suspension in the beater 1, in the process of backwashing, the iron phosphate suspension enters from the fresh water inlet 503 because the backwashing pipeline is connected, at this time, the concentrated water outlet 502 of the concentrated chamber is fresh water, and the fresh water outlet 504 of the fresh water chamber is concentrated water, the first flow sensor 9 and the second flow sensor 11 are still used for monitoring the flow of the fresh water and the concentrated water, the signal values monitored by the first flow sensor 9 and the second flow sensor 11 are sent to the control device, and the flow of the fresh water and the concentrated water is obtained by the control device receiving the signals.Before the time length of backwashing reaches the set time length, the recovery of membrane pollution can be judged by the control device to obtain the fresh water flow and the concentrated water flow, if the recovery requirement has been reached, the backwashing is stopped by the control device when the time length of backwashing reaches the set time length, and the membrane concentration is switched to; if the recovery requirement of membrane pollution has not been reached when the time length of backwashing reaches the set time length, the backwashing is continued or the backwashing is increased by pressure until the recovery requirement of membrane pollution is reached. The switching of the membrane concentration pipeline is to control the first valve 12, the second valve 13 and the third valve 14 to communicate the membrane concentration pipeline by the control device, and the membrane concentration is continued. Since the backwashing of the membrane assembly 5 is carried out by the phosphoric acid iron suspension in the beater 1, the process of backwashing of the membrane assembly 5 is also the process of solid-liquid separation and concentration purification, and the backwashing of the membrane assembly 5 is carried out by the phosphoric acid iron suspension, which further avoids the waste of water resources.
[0036] The low-water consumption washing and membrane concentration integrated system of phosphoric acid iron yellow material in the application can continuously carry out the washing-concentration of the phosphoric acid iron yellow material through the multi-stage washing and concentrating device, thereby improving the washing efficiency and production capacity of the phosphoric acid iron yellow material.
[0037] In some embodiments, when n≥2, the concentrated water tank 6 in the n-1 stage washing and concentrating device is connected with the feed inlet 2 of the beater 1 in the n stage washing and concentrating device; the fresh water tank 7 in the n+1 stage washing and concentrating device is connected with the water inlet pipe 3 of the beater 1 in the n stage washing and concentrating device. It can be understood that when the washing and concentrating device is multi-stage, the concentrated water tank 6 in the n-1 stage washing and concentrating device is connected with the feed inlet 2 of the beater 1 in the n stage washing and concentrating device, that is, the phosphoric acid iron yellow material can be sequentially washed through the multi-stage washing and concentrating device until the phosphoric acid iron reaches the purity standard, the multi-stage washing and concentrating device can continuously carry out the washing-concentration of the phosphoric acid iron yellow material, thereby improving the washing efficiency and production capacity. Moreover, the fresh water collected by the second stage washing and concentrating device and the subsequent washing and concentrating devices can be reused in the previous stage washing and concentrating device, which can avoid the waste of water resources and greatly save the water resources.
[0038] In some embodiments, the liquid outlet pipe 4 is further connected with a fourth valve 26, a fifth valve 27, a one-way valve 29, a sixth valve 28, a gas release pipe 31, and a seventh valve 30 in sequence along the flow direction of the ferric phosphate suspension; the fifth valve 27 is connected to the feed side of the liquid outlet pump 18, and the one-way valve 29 is connected to the discharge side of the liquid outlet pump 18; the gas release pipe 31 is connected with a gas release valve 32; the fourth valve 26, the fifth valve 27, the one-way valve 29, the sixth valve 28, the seventh valve 30, and the gas release valve 32 are electrically connected with the control device, respectively. It can be understood that the gas release pipe 31 is provided to cooperate with the use of the liquid outlet pump 18; when the liquid outlet pump 18 needs to be subjected to the gas release treatment, the seventh valve 30 can be closed, the gas release valve 32 can be opened, and the liquid outlet pump 18 can be subjected to the gas release through the gas release pipe 31.
[0039] In some embodiments, the fourth valve 26, the fifth valve 27, the one-way valve 29, the sixth valve 28, the seventh valve 30, and the gas release valve 32 are solenoid valves or pneumatic valves.
[0040] In some embodiments, when n≥2, the concentrated water tank 6 in the n-1th-stage washing and concentrating device is connected with the feed inlet 2 of the beater 1 in the nth-stage washing and concentrating device through a concentrated water pipe 16, and a concentrated water pump 25 is connected to the concentrated water pipe 16; the fresh water tank 7 in the n+1th-stage washing and concentrating device is connected with the water inlet pipe 3 of the beater 1 in the nth-stage washing and concentrating device through a fresh water pipe 17, the eighth valve 34 is connected to the water inlet pipe 3, and a fresh water pump 33 is connected to the fresh water pipe 17; the eighth valve 34, the fresh water pump 33, and the concentrated water pump 25 are electrically connected with the control device, respectively. It can be understood that the fresh water generated in the n+1th-stage washing and concentrating device can be used in the nth-stage washing and concentrating device to mix with the ferric phosphate yellow material and then subjected to the beating treatment, and at the same time, the external water source needs to be supplemented from the water inlet pipe 3 into the beater 1.
[0041] In some embodiments, the concentrated water pump 25 is a wear-resistant single screw pump. It can be understood that the concentrated water is the ferric phosphate suspension with high solid content, and the low shear characteristic can avoid the destruction of the ferric phosphate particle structure. Of course, the type of the concentrated water pump 25 is not limited to the type disclosed in the present application, and other types of pumps that meet the requirements can also be selected.
[0042] In some embodiments, the fresh water pump 33 is a corrosion-resistant centrifugal pump. It can be understood that the fresh water is a weak acid solution, and the corrosion-resistant centrifugal pump meets the conveying requirements. Of course, the type of the fresh water pump 33 is not limited to the type disclosed in the present application, and other types of pumps that meet the requirements can also be selected.
[0043] In some embodiments, the liquid outlet pump 18 is a liner diaphragm pump. It can be understood that the iron phosphate suspension is transported on the liquid outlet pipe 4 in the present application, and the pump body can be lined with polytetrafluoroethylene (PTFE), rubber or ceramic to resist the erosion and wear of iron phosphate particles in the suspension (the hardness of iron phosphate particles ≥5 Mohs), while it has acid and alkali resistance (pH 1-14) suitable for corrosive media such as chemical industry and metallurgy. Of course, the type of liquid outlet pump 18 is not limited to the type disclosed in the present application, and other types of pumps that meet the requirements can also be selected.
[0044] In some embodiments, the washing and concentrating device is 2-4 stages. It can be understood that the number of stages of the washing and concentrating device can be set as needed until the purity of the iron phosphate meets the requirements. The number of stages of the washing and concentrating device is not limited by the present application and can be set as needed to meet the washing requirements.
[0045] In some embodiments, the beater 1 includes a kettle body 101 and a kettle cover 102 matched with the kettle body 101, the outer side of the kettle body 101 is provided with a jacket heating device 107, and the beater 1 is also provided with a variable frequency stirring device; the jacket heating device 107 and the variable frequency stirring device are respectively electrically connected with the control device.
[0046] In some embodiments, the jacket heating device 107 is an electric heating jacket. It can be understood that the jacket heating device 107 is used to control the temperature of the material in the beater 1, such as the high impurity content of the raw material, which can promote the dissolution of impurities by increasing the washing temperature of the beater 1, and facilitate subsequent membrane concentration by the membrane assembly 5.
[0047] In some embodiments, the variable frequency stirring device includes a variable frequency motor 103, a frequency converter 104, and a stirring shaft 105; the variable frequency motor 103 is electrically connected with the frequency converter 104, and the variable frequency motor 103 and the frequency converter 104 are respectively electrically connected with the control device, one end of the stirring shaft 105 is connected to the output shaft of the variable frequency motor 103, the other end of the stirring shaft 105 extends into the beater 1, and the stirring shaft 105 is connected with a stirring paddle 106.
[0048] In some embodiments, the concentrated water tank 6 is provided with an anti-deposition device. It can be understood that the concentrated water is a concentrated solution with high solid content of iron phosphate, and the anti-deposition device is set to prevent the deposition of iron phosphate particles to avoid the deposition of iron phosphate in the concentrated solution.
[0049] In some embodiments, the anti-deposition device is a stirring device, which comprises a stirring motor 601 and a stirring rod 602 connected to the output shaft of the stirring motor 601, the stirring rod 602 extends into the concentrated water tank 6, and a stirring blade 603 is connected to the stirring rod 602. It can be understood that the stirring effect of the stirring device can prevent the deposition of iron phosphate particles. Of course, other anti-deposition devices can also be used to achieve the effect of preventing deposition, such as ultrasonic anti-deposition devices.
[0050] In some embodiments, the pulping kettle 1 is provided with a first liquid level sensor 19, and the first liquid level sensor 19 is electrically connected with the control device. It can be understood that the first liquid level sensor 19 is used to monitor the liquid level in the pulping kettle 1. First, the liquid level position of the pulping kettle 1 is set. When the liquid level reaches the set liquid level position, the first liquid level sensor 19 sends the monitored signal to the control device. The control device receives the signal and obtains the liquid level in the pulping kettle 1. Then, the control device is used to control the liquid level to remain at the position required by the process.
[0051] In some embodiments, the concentrated water tank 6 is provided with a second liquid level sensor 20, and the second liquid level sensor 20 is electrically connected with the control device. It can be understood that the second liquid level sensor 20 is used to monitor the liquid level in the concentrated water tank 6. First, the liquid level position of the concentrated water tank 6 is set. When the liquid level reaches the set liquid level position, the second liquid level sensor 20 sends the monitored signal to the control device. The control device receives the signal and obtains the liquid level in the concentrated water tank 6. Then, the control device is used to control the liquid level to remain at the position required by the process.
[0052] In some embodiments, the fresh water tank 7 is provided with a third liquid level sensor 21, and the third liquid level sensor 21 is electrically connected with the control device. It can be understood that the third liquid level sensor 21 is used to monitor the liquid level in the fresh water tank 7. First, the liquid level position of the fresh water tank 7 is set. When the liquid level reaches the set liquid level position, the third liquid level sensor 21 sends the monitored signal to the control device. The control device receives the signal and obtains the liquid level in the fresh water tank 7. Then, the control device is used to control the liquid level to remain at the position required by the process.
[0053] In some embodiments, the first valve 12 is an electromagnetic control three-way valve or a pneumatic three-way valve; the second valve 13 is an electromagnetic control three-way valve or a pneumatic three-way valve; the third valve 14 is an electromagnetic control three-way valve or a pneumatic three-way valve; and the eighth valve 34 is an electromagnetic control three-way valve or a pneumatic three-way valve. It can be understood that the first valve 12, the second valve 13 and the third valve 14 are all three-way valves for switching the membrane concentration pipeline and the backwashing pipeline, and the setting of the pneumatic three-way valve or the electromagnetic control three-way valve is to facilitate the control device to control the switching of the valve. The eighth valve 34 is a three-way valve for switching the water inlet of the water inlet pipe 3, and the setting of the pneumatic three-way valve or the electromagnetic control three-way valve is to facilitate the control device to control the switching of the valve.
[0054] When the membrane concentration is carried out, the through-hole control device controls the first valve 12, the second valve 13 and the third valve 14 to communicate the membrane concentration pipeline, and the ferric phosphate suspension is pumped from the liquid outlet pipe 4 of the beater 1 into the membrane assembly 5 through the lining diaphragm pump 18, enters the concentrated chamber inlet 501 of the membrane assembly 5, and the concentrated water at the concentrated chamber outlet 502 enters the concentrated water tank 6 through the first concentrated chamber outlet pipeline 8, and the dilute water at the dilute chamber outlet 504 enters the dilute water tank 7 through the first dilute chamber outlet pipeline 10;
[0055] When backwashing is needed, the first valve 12, the second valve 13 and the third valve 14 are switched by the control device to communicate the backwashing pipeline, and the ferric phosphate suspension is pumped into the membrane assembly 5 through the liquid outlet pipe 4 of the beater 1, the dilute chamber inlet pipe 24 and the dilute chamber inlet 503; at this time, the concentrated chamber outlet 502 is dilute water, the dilute chamber outlet 504 is concentrated water, and the dilute water at the concentrated water outlet enters the dilute water tank 7 through the second concentrated chamber outlet pipeline 22, and the dilute water at the dilute chamber outlet 504 enters the concentrated water tank 6 through the second dilute chamber outlet pipeline 23.
[0056] In some embodiments, the control device is a PLC.
[0057] In some embodiments, the membrane assembly 5 includes three groups of parallel flat sheet membranes.
[0058] The following describes the application of the phosphoric acid iron yellow material low water consumption washing and membrane concentration integrated system in the three-stage washing and concentration device:
[0059] S1, the first-stage washing and concentration device carries out washing and concentration:
[0060] S11, beating: add phosphoric acid iron yellow material (FePO4·2H2O, water content 30%) from the feed inlet 2 of the beater 1, add pure water from the water inlet according to the mass ratio of pure water: phosphoric acid iron yellow material = 5:1, start stirring, and heat to 60°C, and continue stirring at 60°C for 30 minutes; form a ferric phosphate suspension;
[0061] S12, membrane concentration: through the control device to connect the membrane concentration pipeline, the iron phosphate suspension from the outlet pipe 4 of the pulper 1 is pumped into the membrane module 5 by the lining diaphragm pump 18 at a pressure of 0.8 MPa, enters from the concentrated chamber inlet 501 of the membrane module 5, and the concentrated water at the concentrated chamber outlet 502 enters the concentrated water tank 6 through the first concentrated chamber outlet pipeline 8, and the dilute water at the dilute chamber outlet 504 enters the dilute water tank 7 through the first dilute chamber outlet pipeline 10;
[0062] S13, backwashing: when the pressure of the pressure sensor 15 rises by 0.1-0.2 MPa or the dilute water flow monitored by the second flow sensor 11 decreases by one-third, the control device controls the entry into backwashing (for example, when the initial flow is 3 m³ / h and it decreases to 2 m³ / h, the control device controls the closing of the membrane concentration pipeline and the connection of the backwashing pipeline to enter backwashing); through the control device to connect the backwashing pipeline, switch the first valve 12, the second valve 13 and the third valve 14 to carry out backwashing, the iron phosphate suspension from the outlet pipe 4 of the pulper 1 and the dilute chamber inlet pipe 24 is pumped into the membrane module 5 by the lining diaphragm pump 18 at a pressure of 1.0 MPa from the dilute chamber inlet 503; at this time, the concentrated chamber outlet 502 is dilute water, and the dilute chamber outlet 504 is concentrated water, the dilute water at the concentrated chamber outlet 502 enters the dilute water tank 7 through the second concentrated chamber outlet pipeline 22, and the concentrated water at the dilute chamber outlet 504 enters the concentrated water tank 6 through the second dilute chamber outlet pipeline 23; the backwashing time is 60 seconds; after backwashing, switch the first valve 12, the second valve 13 and the third valve 14 to continue membrane concentration,
[0063] Repeat steps S12 and S13;
[0064] The concentrated water tank 6 collects concentrated water, and the concentrated water enters the pulper 1 in the second-stage washing and concentrating device through the concentrated water pipeline 16 for further pulping;
[0065] The dilute water tank 7 collects dilute water, and the dilute water is reused for the synthesis of iron phosphate again;
[0066] S2, the second-stage washing and concentrating device carries out washing and concentration:
[0067] The concentrated water collected in the concentrated water tank 6 in the first-stage washing and concentrating device enters the pulper 1 in the second-stage washing and concentrating device, and the concentrated water collected in the first-stage washing and concentrating device is further washed and concentrated by the second-stage washing and concentrating device; the steps of the second-stage washing and concentrating device for washing and concentration are the same as those of the first-stage washing and concentrating device;
[0068] The concentrated water tank 6 collects concentrated water, and the concentrated water enters the pulper 1 in the third-stage washing and concentrating device through the concentrated water pipeline 16 for further pulping;
[0069] The fresh water tank 7 collects fresh water, which enters the beating chest 1 in the first-stage washing and concentrating device through the fresh water pipeline 17 to continue to be reused to mix with the yellow iron phosphate slurry, and at the same time, external water sources are supplemented through the water inlet pipe 3 of the beating chest 1 in the first-stage washing and concentrating device until the required water amount is reached.
[0070] S3, the third-stage washing and concentrating device performs washing and concentrating:
[0071] The concentrated water collected in the concentrated water tank 6 in the second-stage washing and concentrating device enters the beating chest 1 in the third-stage washing and concentrating device to continue to use the concentrated water collected in the second-stage washing and concentrating device to perform washing and concentrating by the third-stage washing and concentrating device; the steps of washing and concentrating performed by the third-stage washing and concentrating device are the same as those of the first-stage washing and concentrating device.
[0072] The concentrated water tank 6 collects concentrated water, and when it is detected that the concentrated water has reached the required purity, the concentrated water is obtained by spray drying to obtain battery-grade anhydrous iron phosphate (purity ≥ 99.2%). If the concentrated water does not reach the required purity, the washing and concentrating device can be continuously increased to continue to perform washing and concentrating until the required purity is reached.
[0073] The fresh water tank 7 collects fresh water, which enters the beating chest 1 in the second-stage washing and concentrating device to continue to be reused to mix with the yellow iron phosphate slurry, and at the same time, external water sources are supplemented through the water inlet pipe 3 of the beating chest 1 in the second-stage washing and concentrating device until the required water amount is reached.
[0074] It should be noted that the terms "comprising", "containing", or any other variant thereof are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements, but can also include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without more limitations, an element defined by the phrase "comprising a" does not exclude the presence of additional identical elements in the process, method, article, or apparatus that includes the element.
[0075] In addition, it should be noted that the scope of the methods and devices in the embodiments of the present application is not limited to performing functions in the order shown or discussed, but can also include performing functions in a substantially simultaneous manner or in the opposite order according to the functions involved, for example, the described method can be performed in an order different from that described, and various steps can also be added, omitted, or combined. In addition, the features described with reference to certain examples can be combined in other examples.
[0076] The above merely describes a specific implementation of the present application, but the protection scope of the present application is not limited thereto, any skilled person in the art can easily think of changes or replacements within the technical range disclosed by the present application, which should be covered within the protection scope of the present application.
Claims
1. A low-water-consumption washing and membrane concentration integrated system for iron phosphate yellow pigment, characterized in that, It includes a control device and a washing and concentration device, wherein the washing and concentration device is n-stage, n≥1, and n is a natural number, and the washing and concentration device includes a pulping tank, a membrane module, a concentrate tank, and a desalination tank; wherein, The pulping kettle is equipped with an inlet for ferric phosphate yellow material, and the pulping kettle is connected to a water inlet pipe and a liquid outlet pipe. A pressure sensor and a liquid outlet pump are connected to the liquid outlet pipe. The membrane module has a concentration chamber inlet, a concentration chamber outlet, a dilute chamber inlet, and a dilute chamber outlet; the concentration chamber inlet is connected to the outlet pipe of the pulping vessel; The concentrated chamber outlet is connected to the concentrated water tank via a first concentrated chamber outlet pipeline, and a first flow sensor is connected to the first concentrated chamber outlet pipeline; the dilute chamber outlet is connected to the dilute water tank via a first dilute chamber outlet pipeline, and a second flow sensor is connected to the first dilute chamber outlet pipeline. It also includes a backwashing pipeline; the backwashing pipeline includes a dilute chamber inlet pipe, a second concentrate chamber outlet pipe, and a second dilute chamber outlet pipe; the dilute chamber inlet pipe is connected to the outlet pipe of the pulping kettle through a first valve; one end of the second concentrate chamber outlet pipe is connected to the first concentrate chamber outlet pipe through a second valve, and the other end of the second concentrate chamber outlet pipe is connected to the dilute water tank; the second dilute chamber outlet pipe is connected to the first dilute chamber outlet pipe through a third valve, and the other end of the second dilute chamber outlet pipe is connected to the concentrate water tank; The pressure sensor, liquid pump, first flow sensor, second flow sensor, first valve, second valve, and third valve are electrically connected to the control device.
2. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 1, characterized in that, When n≥2, the concentrated water tank in the n-1 stage washing and concentrating unit is connected to the feed inlet of the pulping kettle in the n-stage washing and concentrating unit; the fresh water tank in the n+1 stage washing and concentrating unit is connected to the water inlet pipe of the pulping kettle in the n-stage washing and concentrating unit.
3. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 2, characterized in that, When n≥2, the concentrated water tank in the (n-1)th stage washing and concentrating unit is connected to the feed inlet of the pulping kettle in the nth stage washing and concentrating unit through a concentrated water pipeline, and a concentrated water pump is connected to the concentrated water pipeline; the desalinated water tank in the (n+1)th stage washing and concentrating unit is connected to the inlet pipe of the pulping kettle in the nth stage washing and concentrating unit through a desalinated water pipeline, and a desalinated water pump is connected to the desalinated water pipeline; both the concentrated water pump and the desalinated water pump are electrically connected to the control device.
4. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 3, characterized in that, The concentrate pump is a wear-resistant single screw pump; And / or, the freshwater pump is a corrosion-resistant centrifugal pump; And / or, the discharge pump is a lined diaphragm pump; And / or, the membrane assembly comprises multiple sets of parallel flat sheet membranes.
5. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 4, characterized in that, The washing and concentration device is a 2-4 stage device.
6. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 5, characterized in that, The pulping kettle includes a kettle body and a kettle cover adapted to the kettle body. A jacketed heating device is provided on the outside of the kettle body, and a variable frequency stirring device is also provided on the pulping kettle. And / or, the concentrate tank is equipped with an anti-deposition device.
7. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 6, characterized in that, The variable frequency stirring device includes a variable frequency motor, a frequency converter, and a stirring shaft; the variable frequency motor and the frequency converter are electrically connected, and the variable frequency motor and the frequency converter are respectively electrically connected to a control device; one end of the stirring shaft is connected to the output shaft of the variable frequency motor, and the other end of the stirring shaft extends into the pulping kettle; a stirring paddle is connected to the stirring shaft. And / or, the anti-deposition device is a stirring device, which includes a stirring motor and a stirring rod connected to the output shaft of the stirring motor. The stirring rod extends into the concentrate tank and is connected to stirring blades.
8. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 1, characterized in that, The pulping kettle is equipped with a first liquid level sensor, which is electrically connected to the control device. And / or, the concentrate tank is equipped with a second liquid level sensor, which is electrically connected to the control device; And / or, the freshwater tank is equipped with a third liquid level sensor, which is electrically connected to the control device.
9. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to claim 1, characterized in that, The first valve is an electromagnetically controlled three-way valve or a pneumatic three-way valve; And / or, the second valve is an electromagnetically controlled three-way valve or a pneumatic three-way valve; And / or, the third valve is an electromagnetically controlled three-way valve or a pneumatic three-way valve.
10. The integrated system for low-water-consumption washing and membrane concentration of ferric phosphate yellow material according to any one of claims 1-9, characterized in that, The control device is a PLC.