CN111097747B - Device and method for circularly cleaning and dissolving chemicals - Google Patents
Device and method for circularly cleaning and dissolving chemicals Download PDFInfo
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- CN111097747B CN111097747B CN201911355629.7A CN201911355629A CN111097747B CN 111097747 B CN111097747 B CN 111097747B CN 201911355629 A CN201911355629 A CN 201911355629A CN 111097747 B CN111097747 B CN 111097747B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
- B01F31/83—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations comprising a supplementary stirring element
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B13/00—Accessories or details of general applicability for machines or apparatus for cleaning
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
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Abstract
The invention provides a device for circularly cleaning and dissolving chemicals and a method for circularly cleaning and dissolving chemicals. The device comprises: the cleaning solution secondary treatment unit is also connected with the chemical dissolving unit, and the chemical dissolving unit comprises an ultrasonic dispersion tank. The method comprises the following steps: 1) introducing the cleaning liquid produced by the cleaning liquid secondary treatment unit into each tank body, and starting ultrasound; 2) introducing the cleaning liquid in each tank body into a cleaning liquid primary treatment unit and then into a cleaning liquid storage unit; 3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment and recycling; 4) putting the chemicals into an ultrasonic dispersion tank, and opening the ultrasonic to accelerate dissolution. The device can effectively clear away the pollutant, realizes the cyclic utilization of water resource, can accelerate raw and other materials dissolution rate simultaneously, and the homogenization dispersion.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a device and a method for circularly cleaning and dissolving chemicals.
Background
The lithium ion battery has the advantages of high energy density, high working voltage, no memory response, small self-discharge, long cycle life and the like, and is widely applied to the fields of mobile phones, notebook computers, pure electric vehicles, mobile base stations, energy storage power stations and the like. The ternary precursor is used as a key material for producing the ternary anode of the lithium ion battery, and is prepared into the ternary anode by mixing and sintering with a lithium source, and the core physical and chemical properties of the ternary anode material are directly determined by the performance of the ternary precursor.
The synthesis method of the ternary material precursor is mainly a chemical coprecipitation method, generally, synthesis raw materials are mixed in a solution state, a complexing agent is added into an alkaline solution, the crystal nucleus of the precursor grows up, and after the granularity reaches a preset value, reaction slurry is filtered, washed and dried to obtain the ternary material precursor. In the process of the ternary material precursor synthesis reaction, the requirement on the content of impurities is very high. And often can remain a lot of impurity pollutants when equipment fixing, debugging in earlier stage, be difficult to obtain effectual washing, cause the waste of a large amount of water resources on the contrary to and increase the degree of difficulty of product debugging in earlier stage. The existing ternary material cleaning method is mostly aimed at the processes of filtering and washing ternary material reaction slurry.
CN109574356A discloses a zero discharge treatment method for ternary material cleaning wastewater, which adopts a process flow combining a ceramic membrane treatment system, an electrodialysis treatment system, an RO reverse osmosis system, an MVR evaporation crystallization system and a lithium carbonate recovery system, and comprises (1) filtering solid suspended matters in the wastewater and recovering solid oxides in the wastewater by passing ternary material cleaning water through a ceramic microfiltration membrane treatment system; (2) the wastewater filtered by the ceramic microfiltration membrane enters a coagulative precipitation tank; (3) the electrodialysis system is used for concentrating the effluent of the coagulating sedimentation tank; (4) the water produced by electrodialysis enters an RO reverse osmosis system, the water produced by the RO reverse osmosis system reaches the standard of reuse water, and RO concentrated water returns to the water fed by electrodialysis and is concentrated again; (5) adding a proper amount of saturated sodium carbonate solution into the electrodialysis concentrated water, crystallizing and separating out lithium carbonate, carrying out solid-liquid separation on the lithium carbonate by a centrifugal machine, and finally drying; (6) and (4) the mother liquor after lithium carbonate recovery enters an MVR evaporation system.
CN109713228A discloses a recyclable water-washing alkali-reducing method for ternary materials of lithium ion batteries, which comprises the following steps: putting the ternary positive electrode material and deionized water into a stirring barrel according to a certain proportion, stirring and washing, washing a filter cake by using a small amount of deionized water after primary solid-liquid separation, and performing solid-liquid separation again to obtain a powder material; and (3) the separated filtrate enters a circulating storage tank, an acidic solution is added to adjust the pH value, the obtained filtrate can be used for treating the next batch of ternary cathode materials, after the ternary cathode materials are circularly treated for a certain number of times, the filtrate is led into a wastewater treatment system, and lithium in the wastewater is recovered through a filtering and evaporating device.
The scheme adopts the filtering and washing procedures aiming at the ternary material reaction slurry, so that the problems of waste of a large amount of water resources and difficulty in product debugging in the early stage are solved.
The nickel-cobalt-manganese salt serving as the raw material of the ternary material precursor needs a large amount of time in a dissolving working section, and stirring and dissolving are usually adopted at present, so that the production efficiency is influenced by long time.
Disclosure of Invention
In view of the above-mentioned shortcomings in the prior art, the present invention provides an apparatus for circularly cleaning and dissolving chemicals and a method for circularly cleaning and dissolving chemicals. The device provided by the invention can effectively remove impurity pollutants such as mud dirt, salt dirt and the like remained in the installation and debugging of the equipment at the earlier stage, realizes the cyclic utilization of water resources, and can accelerate the dissolution rate of raw materials and homogenize and disperse.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides an apparatus for cyclically cleaning and dissolving chemicals, the apparatus comprising: the cleaning solution secondary treatment unit is also connected with the chemical dissolving unit, and the chemical dissolving unit comprises an ultrasonic dispersion tank.
The device provided by the invention can effectively remove impurity pollutants such as mud dirt, salt dirt and the like remained in the installation and debugging of the equipment at the earlier stage, realizes the cyclic utilization of water resources, and can accelerate the dissolution rate of raw materials and homogenize and disperse.
As a preferable technical scheme of the invention, the ultrasonic dispersion tank comprises a shell, ultrasonic transducer vibrating plates distributed on the inner wall of the shell, an ultrasonic generator arranged outside the shell and a stirrer driven by a motor and positioned in the shell.
Preferably, the agitator is a pitched blade agitator.
Preferably, 1 of the ultrasonic dispersion tanks contains 2-6 ultrasonic transducer vibrating plates, for example 2, 3, 4, 5 or 6.
Preferably, the ultrasonic transducer vibrating plate comprises a vibrating plate shell and an ultrasonic transducer vibrator arranged on one side of the vibrating plate shell.
Preferably, the 1 ultrasonic transducer vibrating plate comprises 14-18 ultrasonic transducer vibrators.
Preferably, the spacing between adjacent ultrasound transducer elements is 60-100mm, such as 60mm, 70mm, 80mm, 90mm or 100 mm. If the distance between the vibrators is too large, the vibrating plate can generate bending vibration, and meanwhile, the radiation surface is relatively reduced; if the distance between the vibrators is too small, partial sound waves can be counteracted mutually, the ultrasonic efficiency is reduced, meanwhile, the abrasion among all the elements is increased, and the maintenance cost is increased.
Preferably, the shell of the ultrasonic dispersion tank also comprises a liquid discharge pipe.
As a preferable embodiment of the present invention, the chemical dissolving unit includes 2 or more ultrasonic dispersion tanks.
Preferably, each of the ultrasonic dispersion tanks in the chemical dissolving unit is simultaneously connected with a cleaning solution primary treatment unit and a cleaning solution secondary treatment unit.
As a preferable technical scheme of the invention, the cleaning liquid primary treatment unit comprises a solid-liquid separation unit, a deamination unit and a pH regulation unit.
Preferably, the solid-liquid separation unit comprises a cross-flow ceramic filter.
As a preferable technical scheme of the invention, the cleaning solution secondary treatment unit comprises a multi-media filter, an activated carbon filter, a cation resin softener, a precision filter, a reverse osmosis system and ion exchange resin.
As a preferable technical scheme, the device further comprises a subsequent reaction unit, and each tank body in the subsequent reaction unit is simultaneously connected with the cleaning solution primary treatment unit and the cleaning solution secondary treatment unit.
In a second aspect, the present invention provides a method for cyclically cleaning and dissolving chemicals using the apparatus for cyclically cleaning and dissolving chemicals according to the first aspect, comprising the steps of:
(1) introducing the cleaning liquid produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting the ultrasound of the ultrasonic dispersion tank, and cleaning dirt in the tank;
(2) introducing the cleaning liquid in each tank body into a cleaning liquid primary treatment unit, and introducing the cleaning liquid into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling after treatment;
(4) and (3) placing the chemical into an ultrasonic dispersion tank in a chemical dissolving unit, and opening the ultrasonic to accelerate dissolving.
In the method provided by the invention, ultrasonic cavitation impact effect is utilized to generate ultrasonic beams which are radially and linearly transmitted in a pulse mode, thousands of small negative pressure bubbles are generated when the ultrasonic beams advance in a medium, the bubbles form a series of dense expansion explosions in liquid under certain pressure, instantaneous pressure generated when a vacuum cavity is exploded can reach thousands to ten thousands of atmospheric pressures, and solid particles are smashed and split. The micro-bubbles in the liquid keep vibrating under the action of the ultrasonic beam, so that the solid and liquid collide with each other or rub against the wall of the container, the homogenization and dispersion effects are achieved, and the purposes of accelerating the dissolution rate and removing the bonding impurities are achieved.
In a preferred embodiment of the present invention, the cleaning liquid is water.
Preferably, the operating frequency of the ultrasound in step (1) and step (4) is independently 25-130kHz, such as 25kHz, 50kHz, 100kHz or 130 kHz.
Preferably, the output power of the ultrasound in step (1) and step (4) is independently 600-3000W, such as 600W, 1000W, 2000W or 3000W.
Preferably, in the step (2), the conductivity of the cleaning solution treated by the cleaning solution one-time treatment unit is 3000-.
Preferably, in the step (2), the pH of the cleaning solution after the treatment of the cleaning solution primary treatment unit is 7-8, such as 7, 7.2, 7.5, 7.8 or 8. The pH value which is slightly alkaline is adopted because the alkaline environment needs to be maintained in the reaction stage of the synthesis of the ternary precursor, and the cost is reduced as far as possible while the dissolution process of the ternary precursor raw material is not influenced.
In the present invention, the cleaning solution primary treatment unit may adjust the pH with an acid.
Preferably, the acid comprises any one or a combination of at least two of sulfuric acid, phosphoric acid, hydrochloric acid, boric acid, acetic acid, or oxalic acid.
Preferably, in the step (3), the conductivity of the cleaning solution after the treatment by the cleaning solution secondary treatment unit is 0.5-1.0. mu.s/cm, such as 0.5. mu.s/cm, 0.6. mu.s/cm, 0.7. mu.s/cm, 0.8. mu.s/cm, 0.9. mu.s/cm or 1.0. mu.s/cm.
Preferably, step (1) further comprises: starting the stirring of the ultrasonic dispersion tank to clean dirt in the tank.
As a preferable technical scheme of the invention, the chemicals in the step (4) comprise ternary material raw materials.
Preferably, the ternary material raw materials are nickel salt, cobalt salt and manganese salt, or the ternary material raw materials are nickel salt, manganese salt and aluminum salt.
Preferably, three salts composing the ternary material raw material are respectively placed in 3 ultrasonic dispersion tanks for accelerated dissolution.
Preferably, the time for accelerating the dissolution in step (4) is 3-6h, such as 3h, 4h, 5h or 6 h.
Preferably, the temperature for accelerating the dissolution in step (4) is 20-40 ℃, such as 20 ℃, 25 ℃, 30 ℃, 35 ℃ or 40 ℃, etc.
Preferably, step (4) further comprises: starting the stirring of the ultrasonic dispersion tank.
Preferably, the stirring speed is 1.5-3m/s, such as 1.5m/s, 2m/s, 2.5m/s or 3m/s, etc.
As a preferred technical scheme of the invention, the method comprises the following steps:
(1) introducing water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank;
wherein the working frequency of the ultrasound is 25-130kHz, and the output power of the ultrasound is 600-3000W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7-8 and the conductivity of 3000-;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the water with the conductivity of 0.5-1.0 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and performing accelerated dissolution at 20-40 ℃ for 3-6 h;
wherein the working frequency of the ultrasound is 25-130kHz, the output power of the ultrasound is 600-3000W, and the stirring speed is 1.5-3 m/s.
Compared with the prior art, the invention has the following beneficial effects:
(1) the device provided by the invention can effectively remove impurity pollutants such as mud dirt, salt dirt and the like remained in the installation and debugging of the equipment at the early stage, realizes the recycling of water resources, can accelerate the dissolution rate of raw materials by utilizing the matching of ultrasound and stirring, homogenizes and disperses, and is particularly suitable for the dissolution of the raw materials in the ternary material precursor synthesis method.
(2) The method provided by the invention utilizes the ultrasonic cavitation impact effect, is matched with stirring, accelerates the dissolution rate, realizes the circulation of the washing liquid and saves resources.
Drawings
FIG. 1 is a schematic view of the apparatus for cyclically cleaning and dissolving chemicals provided in example 1;
FIG. 2 is a schematic view showing the structure of an ultrasonic dispersion tank in the apparatus for circularly cleaning and dissolving chemicals provided in example 1;
FIG. 3 is a schematic diagram of a vibrating plate structure of an ultrasonic transducer of the ultrasonic dispersion tank provided in example 1;
the ultrasonic vibration testing device comprises a shell 1, an ultrasonic transducer vibrating plate 2, an ultrasonic generator 3, a stirrer 4, a liquid discharge pipe 5, a bottom support 6, a motor 7, an ultrasonic transducer vibrator 8 and a vibrating plate shell 9.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
The following are typical but non-limiting examples of the invention:
example 1
This example provides an apparatus for cyclically cleaning and dissolving chemicals, the apparatus being schematically shown in fig. 1. The device comprises: the cleaning solution treatment device comprises a chemical dissolving unit, a cleaning solution primary treatment unit, a cleaning solution storage unit (namely a cleaning water storage tank in figure 1) and a cleaning solution secondary treatment unit which are sequentially connected, wherein the cleaning solution secondary treatment unit is also connected with the chemical dissolving unit, and the chemical dissolving unit comprises an ultrasonic dispersing tank.
The chemical dissolving unit comprises 3 ultrasonic dispersing tanks including a nickel dissolving tank, a cobalt dissolving tank and a manganese dissolving tank, and the three ultrasonic dispersing tanks are connected with the cleaning liquid primary treatment unit and the cleaning liquid secondary treatment unit simultaneously.
The cleaning liquid primary treatment unit comprises a solid-liquid separation unit, a deamination unit and a pH adjusting unit, wherein the solid-liquid separation unit is a cross-flow ceramic filter, and the filtering precision is 1.5 mu m. The cleaning solution secondary treatment unit comprises a multi-media filter, an activated carbon filter, a cation resin softener, a precision filter, a reverse osmosis system and ion exchange resin.
The device also comprises a subsequent reaction unit, wherein each tank body in the subsequent reaction unit is simultaneously connected with the cleaning solution primary treatment unit and the cleaning solution secondary treatment unit.
The structure of ultrasonic wave dispersion jar is shown in fig. 2, the ultrasonic wave dispersion jar includes casing 1, distributes 4 ultrasonic transducer on the 1 inner wall of casing shakes board 2, sets up 1 outside supersonic generator 3 of casing and by motor 7 drive and be located the agitator 4 of casing 1, agitator 4 is oblique oar formula agitator. The shell 1 of the ultrasonic dispersion tank is also provided with a liquid discharge pipe 5 and a bottom bracket 6.
In the ultrasonic dispersion tank of the present embodiment, the structure of the ultrasonic transducer vibration plate 2 is as shown in fig. 3, and includes a vibration plate housing 9 and 16 ultrasonic transducer oscillators 8 disposed on one side of the vibration plate housing 9, and the distance between adjacent ultrasonic transducer oscillators 8 is 100 mm.
The embodiment also provides a method for circularly cleaning and dissolving the ternary material precursor raw material by using the device of the embodiment, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 25kHz, and the output power of the ultrasound is 600W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 8 and the conductivity of 5000 mus/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 1.0 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 6 hours to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 25kHz, the output power of the ultrasound is 600W, and the stirring speed is 1.5 m/s.
Example 2
This example provides an apparatus for cleaning and dissolving chemicals in a circulating manner, which is similar to the apparatus for cleaning and dissolving chemicals in a circulating manner provided in example 1, except that the number of ultrasonic transducer vibrators disposed on the vibrating plate housing side in the ultrasonic transducer vibrating plate is 14, and the interval between the adjacent ultrasonic transducer vibrators is 80 mm.
The embodiment also provides a method for circularly cleaning and dissolving the ternary material precursor raw material by using the device of the embodiment, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 25kHz, and the output power of the ultrasound is 1500W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7.6 and the conductivity of 4600 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.90 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 5.2h to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 25kHz, the output power of the ultrasound is 1500W, and the stirring speed is 1.5 m/s.
Example 3
This example provides an apparatus for cleaning and dissolving chemicals in a circulating manner, which is similar to the apparatus for cleaning and dissolving chemicals in a circulating manner provided in example 1, except that the number of ultrasonic transducer vibrators disposed on the vibrating plate housing side in the ultrasonic transducer vibrating plate is 18, and the interval between the adjacent ultrasonic transducer vibrators is 60 mm.
The embodiment also provides a method for circularly cleaning and dissolving the ternary material precursor raw material by using the device of the embodiment, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 25kHz, and the output power of the ultrasound is 3000W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH value of 7.2 and the conductivity of 4200 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.8 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 4.8h to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 25kHz, the output power of the ultrasound is 3000W, and the stirring speed is 1.5 m/s.
Example 4
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 28kHz, and the output power of the ultrasound is 600W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7.8 and the conductivity of 4800 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.96 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 5.5h to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 28kHz, the output power of the ultrasound is 600W, and the stirring speed is 1.5 m/s.
Example 5
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 28kHz, and the output power of the ultrasound is 1500W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7.4 and the conductivity of 4400 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.89 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 4.7h to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 28kHz, the output power of the ultrasound is 1500W, and the stirring speed is 1.5 m/s.
Example 6
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 28kHz, and the output power of the ultrasound is 3000W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH value of 7.2 and the conductivity of 4200 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.81 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 4 hours to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 28kHz, the output power of the ultrasound is 3000W, and the stirring speed is 1.5 m/s.
Example 7
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 40kHz, and the output power of the ultrasound is 600W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7.7 and the conductivity of 4600 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.91 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 5.5h to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 40kHz, the output power of the ultrasound is 600W, and the stirring speed is 1.5 m/s.
Example 8
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 40kHz, and the output power of the ultrasound is 1500W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the obtained water with the pH of 7.3 and the conductivity of 3700 mu s/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.6 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 4 hours to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 40kHz, the output power of the ultrasound is 1500W, and the stirring speed is 1.5 m/s.
Example 9
The embodiment provides a method for circularly cleaning and dissolving a ternary material precursor raw material by using the device for circularly cleaning and dissolving chemicals in embodiment 1, which comprises the following specific steps:
(1) introducing deionized water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank, and removing salt dirt and mud dirt adhered to the bottom of the tank body and the wall of the tank;
wherein the working frequency of the ultrasound is 40kHz, and the output power of the ultrasound is 3000W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7 and the conductivity of 4000 mus/cm into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the deionized water with the conductivity of 0.5 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and carrying out accelerated dissolution at 40 ℃ for 3 hours to fully dissolve the nickel salt, the cobalt salt and the manganese salt;
wherein the working frequency of the ultrasound is 40kHz, the output power of the ultrasound is 3000W, and the stirring speed is 1.5 m/s.
Comparative example 1
This comparative example provides a method of cyclically cleaning and dissolving a ternary material precursor raw material using the apparatus for cyclically cleaning and dissolving chemicals of example 1, which is the same as the method of example 1 except that only stirring without sonication is performed in step (4).
This comparative example is that the nickel salt, cobalt salt and manganese salt were not sufficiently dissolved in the same dissolution time as in example 1.
Combining the above examples and comparative examples, it can be seen that:
the method provided by the embodiment utilizes the ultrasonic cavitation impact effect, is matched with stirring, accelerates the dissolution rate, realizes the circulation of the washing liquid and saves resources.
Comparative example 1 did not employ sonication, making the dissolution process less than ideal.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (23)
1. A method for cyclically cleaning and dissolving chemicals, said method using an apparatus for cyclically cleaning and dissolving chemicals, comprising the steps of:
(1) introducing the cleaning liquid produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting the ultrasound of the ultrasonic dispersion tank, and cleaning dirt in the tank;
(2) introducing the cleaning liquid in each tank body into a cleaning liquid primary treatment unit, and introducing the cleaning liquid into a cleaning liquid storage unit after treatment;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling after treatment;
(4) placing the chemicals in an ultrasonic dispersion tank in a chemical dissolving unit, and opening the ultrasonic to accelerate dissolving;
the device comprises: the cleaning solution secondary treatment unit is also connected with the chemical dissolving unit, and the chemical dissolving unit comprises an ultrasonic dispersion tank;
the ultrasonic dispersion tank comprises a shell, ultrasonic transducer vibrating plates distributed on the inner wall of the shell, an ultrasonic generator arranged outside the shell and a stirrer driven by a motor and positioned in the shell; the ultrasonic transducer vibrating plate comprises a vibrating plate shell and an ultrasonic transducer vibrator arranged on one side of the vibrating plate shell; the distance between adjacent ultrasonic transducer vibrators is 60-100 mm;
the cleaning solution primary treatment unit comprises a solid-liquid separation unit, a deamination unit and a pH regulation unit; the cleaning solution secondary treatment unit comprises a multi-media filter, an activated carbon filter, a cation resin softener, a precision filter, a reverse osmosis system and ion exchange resin;
the device also comprises a subsequent reaction unit, wherein each tank body in the subsequent reaction unit is simultaneously connected with the cleaning solution primary treatment unit and the cleaning solution secondary treatment unit.
2. The method of claim 1, wherein the agitator is a pitched blade agitator.
3. The method of claim 1, wherein 1 ultrasonic dispersion tank contains 2-6 ultrasonic transducer vibrating plates.
4. The method of claim 1, wherein 1 ultrasonic transducer vibrating plate comprises 14-18 ultrasonic transducer elements.
5. The method of claim 1, wherein the housing of the ultrasonic dispersion tank further comprises a drain on the housing.
6. The method of claim 1, wherein the chemical dissolving unit comprises more than 2 of the ultrasonic dispersion tanks.
7. The method as claimed in claim 1, wherein each of the ultrasonic dispersion tanks in the chemical dissolving unit is connected to a cleaning solution primary treatment unit and a cleaning solution secondary treatment unit at the same time.
8. The method according to claim 1, wherein the solid-liquid separation unit comprises a cross-flow ceramic filter.
9. The method of claim 1, wherein the cleaning fluid is water.
10. The method of claim 1, wherein the operating frequency of the ultrasound of step (1) and step (4) is independently 25-130 kHz.
11. The method as claimed in claim 1, wherein the output power of the ultrasound in step (1) and step (4) is independently 600-3000W.
12. The method as claimed in claim 1, wherein in the step (2), the conductivity of the cleaning solution treated by the cleaning solution primary treatment unit is 3000-.
13. The method according to claim 1, wherein in the step (2), the pH of the cleaning solution after the treatment in the cleaning solution primary treatment unit is 7.
14. The method as claimed in claim 1, wherein in the step (3), the conductivity of the cleaning solution after the treatment by the cleaning solution secondary treatment unit is 0.5 to 1.0 μ s/cm.
15. The method of claim 1, wherein step (1) further comprises: starting the stirring of the ultrasonic dispersion tank to clean dirt in the tank.
16. The method of claim 1, wherein the chemical of step (4) comprises a ternary material feedstock.
17. The method of claim 16, wherein the ternary material raw materials are nickel salts, cobalt salts, and manganese salts, or the ternary material raw materials are nickel salts, manganese salts, and aluminum salts.
18. The method of claim 17, wherein three salts constituting the ternary material raw material are respectively placed in 3 ultrasonic dispersion tanks for accelerated dissolution.
19. The method of claim 1, wherein the time for accelerating dissolution in step (4) is 3-6 hours.
20. The method of claim 1, wherein the temperature for accelerating dissolution in step (4) is 20-40 ℃.
21. The method of claim 1, wherein step (4) further comprises: starting the stirring of the ultrasonic dispersion tank.
22. The method of claim 21, wherein the stirring speed is 1.5-3 m/s.
23. Method according to claim 1, characterized in that it comprises the following steps:
(1) introducing water produced by the cleaning liquid secondary treatment unit into each tank body in the device for circularly cleaning and dissolving chemicals, starting ultrasound of the ultrasonic dispersion tank and starting stirring to clean dirt in the tank;
wherein the working frequency of the ultrasound is 25-130kHz, and the output power of the ultrasound is 600-3000W;
(2) introducing the cleaning water in each tank body into a cleaning liquid primary treatment unit, and introducing the water with the pH of 7-8 and the conductivity of 3000-;
(3) introducing the cleaning liquid in the cleaning liquid storage unit into a cleaning liquid secondary treatment unit for treatment, and recycling the water with the conductivity of 0.5-1.0 mu s/cm obtained after treatment;
(4) respectively placing nickel salt, cobalt salt and manganese salt in 3 ultrasonic dispersion tanks in a chemical dissolving unit, starting ultrasonic and starting stirring, and performing accelerated dissolution at 20-40 ℃ for 3-6 h;
wherein the working frequency of the ultrasound is 25-130kHz, the output power of the ultrasound is 600-3000W, and the stirring speed is 1.5-3 m/s.
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