CN110898516B - Device for removing magnetic substances from lithium carbonate slurry - Google Patents
Device for removing magnetic substances from lithium carbonate slurry Download PDFInfo
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- CN110898516B CN110898516B CN201911228692.4A CN201911228692A CN110898516B CN 110898516 B CN110898516 B CN 110898516B CN 201911228692 A CN201911228692 A CN 201911228692A CN 110898516 B CN110898516 B CN 110898516B
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
Abstract
The invention relates to a device for removing magnetic substances from lithium carbonate slurry, which comprises a slurry washing and demagnetizing system, wherein the slurry washing and demagnetizing system comprises: filtering mechanism, filtration retrieve mechanism, thick liquid wash mechanism, steam filtering mechanism, rubbing crusher construct, remove magnetism mechanism, wherein filtering mechanism is connected to thick liquid wash the mechanism, thick liquid wash the mechanism rubbing crusher construct with remove magnetism mechanism and form circulation circuit, filtering mechanism still is connected with filter and retrieve the mechanism, thick liquid wash the mechanism still be connected with steam filtering mechanism. The device provided by the invention can obviously reduce the magnetic substances in the lithium carbonate slurry, and is a key production device for producing battery-grade lithium carbonate.
Description
Technical Field
The invention relates to the field of lithium carbonate production, in particular to a device for removing a magnetic substance from lithium carbonate slurry.
Background
In recent years, with the hot trend of global new energy development, the market of downstream lithium carbonate applications including electric vehicles, TMTs, energy storage batteries and the like is rapidly expanding, and the demand of battery-grade lithium carbonate is vigorous. The battery grade lithium carbonate has very strict requirements on the content of impurities, and the magnetic substance has very great influence on the safety of the ion battery and is an important index of the battery grade lithium carbonate. Therefore, for upstream lithium carbonate production enterprises, the content of the magnetic substance in the lithium carbonate must be strictly controlled, and the electromagnetic safety is ensured from the source.
In the production process of the lithium carbonate, the content of the magnetic substance is far higher than the standard value required by national standards and battery enterprises due to the magnetic substance existing in the raw material and the magnetic substance introduced in the subsequent process flow and equipment. How to remove magnetic impurities in lithium carbonate materials by using an efficient magnetic removal device is still a difficulty.
Disclosure of Invention
Technical problem
The invention aims to solve the technical problems and provides a device for efficiently demagnetizing in the lithium carbonate production process, which can effectively remove magnetic substances in lithium carbonate and is a key production device for producing battery-grade lithium carbonate.
Technical scheme
Specifically, the invention relates to a device for removing magnetic substances from lithium carbonate slurry, which comprises a slurry washing and demagnetizing system, wherein the slurry washing and demagnetizing system comprises: a filtering mechanism, a filtering and recycling mechanism, a pulp washing mechanism, a steam filtering mechanism, a crushing mechanism and a demagnetizing mechanism,
wherein the filter mechanism is connected to the slurry wash mechanism,
the pulp washing mechanism, the crushing mechanism and the demagnetizing mechanism form a circulation loop,
the filtering mechanism is also connected with the filtering and recovering mechanism,
the slurry washing mechanism is also connected with the steam filtering mechanism.
In one embodiment, the filtration mechanism is a plate and frame filter press.
In one embodiment, the filtration recovery mechanism comprises a bag filter, a filtrate storage tank, and a transfer pump.
In one embodiment, the slurry wash mechanism includes a wash slurry tank and an agitation member.
In one embodiment, the vapor filtration mechanism is a vapor filter.
In one embodiment, the comminuting mechanism is a high-speed shear pump.
In one embodiment, the demagnetizing mechanism is a deironing device.
In one embodiment, the apparatus includes two or more stages of slurry magnetic removal systems connected in series with each other, wherein the slurry washing mechanism in the slurry magnetic removal system of a preceding stage is connected to the filtering mechanism in the slurry magnetic removal system of a subsequent stage.
Advantageous effects
The device has high demagnetization efficiency and obvious effect, well solves the problems of high impurity content of magnetic substances and difficult efficient removal in the lithium carbonate production process, and is a key device for enabling the quality of lithium carbonate to reach above a battery level.
The apparatus of the present invention may use two or three stage pulp washing degaussing systems, each of which may be set to the same or different process parameters. After the materials are demagnetized for 2-3 times step by step, most of magnetic substances mixed in the initial materials can be efficiently processed, and the content of the magnetic substances can be reduced from more than 1000PPb to less than 400 PPb. In addition, the device reduces the demagnetizing pressure of the subsequent working section, and is favorable for stably controlling the content of magnetic substances in the lithium carbonate finished product.
Drawings
Fig. 1 is a process flow diagram of an apparatus for removing magnetic substances from lithium carbonate slurry according to an embodiment of the present invention.
Fig. 2 is a process flow diagram of an apparatus for removing magnetic substances from lithium carbonate slurry according to another embodiment of the present invention.
Reference numerals
1: conversion slurry
2: filtrate
3: deionized water
4: steam generating device
5: magnetic material
6: slurry washing demagnetizing product
100: slurry washing demagnetizing system
101: filtering mechanism
102: filtering and recycling mechanism
103: slurry washing mechanism
104: steam filtering mechanism
105: crushing mechanism
106: demagnetizing mechanism
11: first valve
12: second valve
Detailed Description
The terms or words used in the present specification and claims should not be construed restrictively as general or dictionary definitions, and should be construed as meanings and concepts corresponding to technical ideas of the present invention on the basis of the principle that the inventor can appropriately define concepts of the terms to describe the invention in the best possible manner.
1. Device for removing magnetic substances from lithium carbonate slurry
The invention relates to a device for removing magnetic substances from lithium carbonate slurry.
First embodiment
Fig. 1 shows a process flow according to an embodiment of the invention, and a lithium carbonate demagnetizing device used in the process flow comprises a primary slurry washing demagnetizing system.
As shown in fig. 1, the slurry washing and demagnetizing system 100 includes a filter mechanism 101, a filter recovery mechanism 102, a slurry washing mechanism 103, a steam filter mechanism 104, a pulverization mechanism 105, and a demagnetizing mechanism 106.
The filter mechanism 101 may comprise primarily a plate and frame filter press. The lithium carbonate slurry generated in the lithium conversion and precipitation working section is subjected to solid-liquid separation in the 1 st stage of slurry washing to obtain a filter cake and a filtrate containing impurities, wherein the filter cake enters the slurry washing mechanism 103 of the stage, and the filtrate containing impurities enters the filtration and recovery mechanism 102 and is recycled after being processed.
The filtering and recovering mechanism 102 may mainly comprise a filtrate storage tank, a bag filter and a transfer pump, and may store the filtrate from the plate and frame filter press, recover lithium carbonate remaining in the filtrate, and transfer the final remaining filtrate to an upstream process for recycling, thereby reducing water resource consumption. The recovery rate of lithium carbonate in the filtrate of the plate-and-frame filter press can reach more than 99 percent. The recovery rate is a ratio of lithium carbonate recovered from the filtrate of the plate and frame filter press to lithium carbonate contained in the filtrate.
The slurry wash mechanism 103 may include a wash slurry tank and an internal agitation member. Deionized water is previously fed from the top of the slurry washing mechanism 103. Then, adding the lithium carbonate filter cake from the filtering mechanism 101, stirring with a stirring member to obtain uniform lithium carbonate slurry, and primarily washing lithium carbonate; at the same time, steam is introduced from the bottom of the pulp washing mechanism 103 to maintain the material at a relatively constant temperature range, e.g., 80-90 ℃. The method increases the solubility of soluble impurities, is beneficial to filtering out the impurities after the impurities are dissolved in the deionized water, and is also beneficial to controlling the quality stability of the finished product after the impurities are removed.
The steam filtering mechanism 104 can be composed of a steam filter, and impurities in the pipeline brought along with the steam are filtered by an internal filter screen after the steam enters the steam filtering mechanism, so that the steam cleanliness is ensured; meanwhile, the condensed water is discharged from the bottom of the steam filter in time by the steam filter, and part of impurities in the pipeline are taken out and the steam temperature is kept. In one embodiment of the invention, the temperature of the steam may be 160 ℃.
The uniformly mixed lithium carbonate slurry from the bottom of the slurry washing mechanism 103 is continuously fed to the crushing mechanism 105 through the first valve 11.
The crushing mechanism 105 may be constituted by 1 high-speed shear pump. The high-speed shear pump can be matched with a 3-stage impeller, the maximum rotating speed can reach 2900r/min, and the maximum flow can be 30m3H, particle diameter D of the slurry after being crushed50May be 20-30 μm. Fully crushing the slurry, and breaking the peritectic crystal of the lithium carbonate and the false package formed by the lithium carbonate and air.
The pulverized slurry enters a degaussing mechanism 106, which degaussing mechanism 106 may be a de-ironing separator that may be used to remove magnetic material from the pipeline fluid. The iron remover comprises a shell and a magnetic rod. The magnetic force of the magnetic bar may be 8000 GS. The magnetic rod of the iron remover is directly and fully contacted with the lithium carbonate slurry, so that a large amount of magnetic impurities can be adsorbed. In addition, when the subsequent magnetic discharge operation is performed, the magnetic substance adsorbed by the surface of the magnetic rod can be discharged from the bottom of the iron remover and collected as the magnetic substance 5.
The demagnetized lithium carbonate slurry is circulated back to the slurry washing mechanism 103, the crushed and refined lithium carbonate in the slurry can be fully contacted with the deionized water, and soluble impurities are more easily dissolved in the deionized water. Thereby realizing continuous circulation pulp washing demagnetizing.
After a set period of time, the lithium carbonate slurry completes the repeated slurry washing and magnetic removing circulation process. Then, the first valve 11 is closed, the second valve 12 is opened, and all the lithium carbonate slurry is discharged through the second valve 12 via the output line at the bottom of the slurry washing mechanism 103, so as to obtain the slurry-washed demagnetized product 6 (slurry-washed demagnetized lithium carbonate slurry).
Further, the slurry-washed demagnetized product 6 can be conveyed to a subsequent section by a conveying mechanism (such as a centrifugal pump).
Second embodiment
Fig. 2 shows a process flow according to another embodiment of the invention, and the lithium carbonate demagnetizing device used in the process flow comprises a three-stage pulp washing demagnetizing system.
In fig. 2, the 2 nd and 3 rd stage slurry washing and magnetic removing systems are the same as the 1 st stage slurry washing and magnetic removing system, the adopted process flow is also the same, and the process parameters can be the same or different. The lithium carbonate slurry treated by the previous slurry washing and demagnetizing system is connected to the 2 nd and 3 rd filtering mechanisms, and the processes (filtering, slurry washing, crushing and demagnetizing) identical to those in the 1 st slurry washing and demagnetizing system are performed, so that the three-stage slurry washing and demagnetizing are realized, and a final slurry washing and demagnetizing product 6 (the lithium carbonate slurry subjected to slurry washing and demagnetizing) is obtained.
The slurry washing demagnetizing product 6 after the third-stage slurry washing demagnetizing is completed can be conveyed to the subsequent working section through a conveying mechanism (such as a centrifugal pump).
2. Method for removing magnetic substance from lithium carbonate slurry
The invention also relates to a method for removing magnetic substances from lithium carbonate slurry, which adopts batch treatment or batch treatment and mainly comprises the following steps.
(1) Preliminary filtration
In order to reduce the pressure of the subsequent washing procedure, a certain amount of lithium carbonate slurry generated in a conversion lithium deposition working section in the lithium carbonate production process is conveyed to a filtering mechanism for primary filtering, and water and other soluble impurities are filtered out to obtain a lithium carbonate mixture filter cake containing a certain amount of water and impurities.
(2) Deionized water is introduced and filter cake is added
And (3) introducing deionized water with a certain proportion into the slurry washing mechanism, and adding the obtained whole lithium carbonate mixture filter cake into the deionized water.
In order to increase the solubility of soluble impurities during the subsequent stirring washing and filter the impurities after the impurities are easily dissolved in the deionized water, the temperature of the introduced deionized water can be set to be 70-95 ℃, and preferably 80-90 ℃.
(3) Stirring washing, pulverizing and demagnetizing
And stirring and washing (slurry washing) the lithium carbonate mixture filter cake and deionized water in a slurry washing mechanism to prepare slurry, so as to obtain homogeneous lithium carbonate slurry.
In order to keep the temperature of the lithium carbonate slurry within a relatively constant temperature range (for example, 80-90 ℃) so as to be beneficial to controlling the quality stability of the finished product after impurity removal, the slurry is heated by purified steam while stirring and washing, and the steam temperature can be 150-180 ℃.
Steam enters from the bottom of the slurry washing tank and then directly contacts with the slurry, and the steam has longer contact time with the lithium carbonate slurry in the rising process, so that the heating efficiency is high; meanwhile, the lithium carbonate slurry is driven to turn over in the rising process, the longitudinal stirring effect is achieved, the circumferential stirring of the stirring member is combined, the washing efficiency is higher, and the effect is better.
Before entering, the steam is filtered to remove impurities in the steam through a separately arranged steam filtering mechanism and is subjected to water-vapor separation treatment, so that the cleanliness of the steam is ensured, and the impurities in a steam pipeline are prevented from being introduced into the material.
Then, a lithium carbonate slurry containing lithium carbonate and deionized water is transferred from the slurry washing mechanism to the pulverizing mechanism. Under the action of strong shearing force of the crushing mechanismAnd then, the lithium carbonate slurry is fully crushed to break the lithium carbonate peritectic crystal and the false package formed by the lithium carbonate and the air, so that impurities are prevented from being wrapped in the lithium carbonate peritectic crystal and the false package of the air or adhered to the lithium carbonate peritectic crystal and the false package of the air, and soluble impurities are more easily and fully contacted with deionized water to be dissolved in the deionized water. The particle diameter D of the crushed lithium carbonate slurry50May be 20-30 μm. And then, inputting the crushed lithium carbonate slurry into a demagnetizing mechanism, so that the magnetic substance is adsorbed onto the demagnetizing mechanism, and obtaining the demagnetized lithium carbonate slurry.
In order to enhance the washing effect, the slurry after being demagnetized enters the slurry washing mechanism again to be stirred and washed so as to better dissolve soluble impurities.
Thus continuously and circularly carrying out the crushing, the demagnetization and the stirring washing until the corresponding process standard is reached. The total treatment time for the agitated washing may be 15-30 minutes.
(4) Multistage filtering, stirring washing, crushing and demagnetizing
Optionally, in order to perform more deep degaussing on the lithium carbonate slurry, the lithium carbonate slurry can be subjected to the steps (1), (2) and (3) which are relatively independent and connected in series one or more times so as to achieve the corresponding process index.
Examples
Hereinafter, the present invention will be described in detail with reference to examples to specifically describe the present invention. However, the embodiment of the present invention may be modified into various other forms and the scope of the present invention should not be construed as being limited to the embodiments described below. Embodiments of the present invention are provided to more fully describe the present invention to those of ordinary skill in the art.
The apparatus or materials in the following examples are commercially available from the general market or can be easily prepared by the self, unless otherwise specified.
Comparative example 1 lithium carbonate slurry (material before washing) produced in the conversion lithium precipitation stage
In the lithium precipitation section of the process for producing lithium carbonate, lithium-rich brine (10 cubic meters) after evaporation concentration is fed into a conversion reaction kettle, and a saturated sodium carbonate solution (20 cubic meters) is added into the conversion reaction kettle, so that lithium ions and carbonate ions are combined to generate lithium carbonate precipitate.
The reforming reaction kettle is provided with a steam heating jacket, and steam with the temperature of 160 ℃ is introduced into the steam heating jacket to keep the reaction temperature in the reforming reaction kettle at about 80 ℃. Meanwhile, a stirring member is arranged at the top of the conversion reaction kettle, and on one hand, the stirring member uniformly stirs the lithium-rich brine and the sodium carbonate solution to accelerate the lithium precipitation reaction; in another aspect, the stirring member reacts the formed lithium carbonate precipitate with the remainder of the Na-containing material after the reaction+、K+And the like, and finally forming lithium carbonate slurry (lithium deposition slurry).
Example 1
Referring to fig. 1, the lithium carbonate demagnetizing device in the present embodiment includes a primary slurry washing demagnetizing system.
First, lithium carbonate slurry (10 cubic meters) generated in the conversion lithium precipitation section of comparative example 1 was fed to a filtration mechanism. And (3) carrying out primary impurity filtration in a plate-and-frame filter press as a filtering mechanism, and carrying out solid-liquid separation to obtain a lithium carbonate mixture filter cake.
Deionized water (6 cubic meters) at 80 ℃ was fed into a slurry washing mechanism (which included a washing slurry tank and a stirring member provided therein) (Sichuan Red light mechanical Co., Ltd., DT2500 x 2500-7.5), and then the whole cake of the lithium carbonate mixture obtained was added to the deionized water.
Then, stirring and washing (slurry washing) the lithium carbonate mixture to obtain lithium carbonate slurry, and finishing slurry preparation; meanwhile, steam (160 ℃) purified by the steam filtering mechanism is introduced from the bottom of the washing slurry tank, the lithium carbonate slurry is heated, and the temperature of the lithium carbonate slurry is kept at 80 ℃.
The lithium carbonate slurry is then fed to a high speed shear pump (SRH-3-165-22 KW, special pump and valve works ltd, lixing) as a comminuting mechanism for comminuting the lithium carbonate particles therein.
The pulverized slurry was introduced into a degaussing mechanism (iron remover, Ningbo Seiko magnetic industries development Co., Ltd., 200/65) and was brought into full contact with a magnetic rod having a magnetic force of up to 8,000GS, and a magnetic substance was adsorbed on the surface of the magnetic rod.
And the slurry after the demagnetization enters the slurry washing mechanism again for stirring and washing. Continuously and circularly carrying out the processes of crushing, demagnetizing and stirring washing. The time for the whole agitation washing took 25 minutes, that is, the time interval from the start of the agitation washing to the discharge was set to 25 minutes.
And finally, discharging the obtained lithium carbonate slurry from the slurry washing mechanism.
Example 2
The lithium carbonate demagnetizing device in this embodiment includes a three-stage slurry demagnetizing system, and the slurry demagnetizing systems used in this embodiment are respectively the same as those used in embodiment 1.
Specifically, the procedure of the grade 1 slurry washing for removing magnetism was the same as in example 1, and the whole procedure took 25 minutes.
Then, all the slurry enters into the 2 nd and 3 rd slurry washing and demagnetizing systems in sequence. The technological process and mechanism of the 2 nd and 3 rd stage slurry washing and magnetic removing are completely consistent with those of the 1 st stage, the materials are subjected to treatment similar to the 1 st stage slurry washing and magnetic removing, and the total time of stirring and washing is only different, and is reduced by 5 minutes step by step, namely the total time of the 1 st stage stirring and washing process is 25 minutes, the total time of the 2 nd stage stirring and washing process is 20 minutes, and the total time of the 3 rd stage stirring and washing process is 15 minutes.
Finally, the obtained lithium carbonate slurry is discharged from the 3 rd stage slurry washing mechanism.
Experimental example 1 measurement of magnetic substance content
The main equipment used in the laboratory for determining the magnetic content was inductively coupled plasma atomic emission spectroscopy (Thermo Fisher, iCAP 7400 Duo). The total content of six elements of Cr, Mn, Fe, Co, Ni and Zn in the magnetic substance is measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination method specifically comprises the following steps: the lithium carbonate slurry obtained in each of comparative example 1, and example 2 was filtered by a suction filter (saint/Sciencetool, R300A) to obtain a lithium carbonate semi-dry solid. Then, 200g of a semi-dry solid sample of lithium carbonate was weighed each time for measurement.
The content of each element was calculated, wherein the arithmetic mean of the values of the two replicates was taken as the calculation result. The sum of the contents of all the elements is the content of the magnetic substance in the tested sample. The results are shown in Table 1 below.
TABLE 1
| Item | Comparative example 1 | Example 1 | Example 2 |
| Content of magnetic substance (PPb) | 1100 | 380 | 200 |
As can be seen from table 1, the magnetic substance content in the lithium carbonate slurry demagnetized according to examples 1 and 2 of the present invention is significantly lower than that in the lithium carbonate slurry of comparative example 1, which indicates that the apparatus of the present invention is capable of efficiently removing the magnetic substance.
Claims (8)
1. An apparatus for removing magnetic material from lithium carbonate slurry, the apparatus comprising a slurry magnetic removal system, the slurry magnetic removal system comprising:
a filtering mechanism, a filtering and recycling mechanism, a pulp washing mechanism, a steam filtering mechanism, a crushing mechanism and a demagnetizing mechanism,
wherein the filter mechanism is connected to the slurry wash mechanism,
the pulp washing mechanism, the crushing mechanism and the demagnetizing mechanism form a circulation loop,
the filtering mechanism is also connected with the filtering and recovering mechanism,
the slurry washing mechanism is also connected with the steam filtering mechanism.
2. The apparatus of claim 1, wherein the filtration mechanism is a plate and frame filter press.
3. The apparatus of any of claims 1-2, wherein the filtration recovery mechanism comprises a bag filter, a filtrate storage tank, and a transfer pump.
4. The apparatus of claim 1, wherein the slurry wash mechanism comprises a wash slurry tank and an agitation member.
5. The device of claim 1, wherein the vapor filtration mechanism is a vapor filter.
6. The apparatus of claim 1, wherein the comminution mechanism is a high-speed shear pump.
7. The device of claim 1, wherein the demagnetizing mechanism is a deironizer.
8. The apparatus of claim 1, wherein the apparatus comprises two or more stages of slurry magnetic removal systems connected in series with each other, wherein the slurry washing mechanism in the slurry magnetic removal system of a preceding stage is connected to the filtering mechanism in the slurry magnetic removal system of a subsequent stage.
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