CN112351953B - Method and device for preparing lithium chloride - Google Patents
Method and device for preparing lithium chloride Download PDFInfo
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- CN112351953B CN112351953B CN201880095143.1A CN201880095143A CN112351953B CN 112351953 B CN112351953 B CN 112351953B CN 201880095143 A CN201880095143 A CN 201880095143A CN 112351953 B CN112351953 B CN 112351953B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention relates to a preparation method of lithium chloride and a device thereof. One embodiment of the present invention provides a method for preparing lithium chloride, comprising: mixing the spodumene ore, coke and chlorine gas and then carrying out chlorination reaction; and a step of generating lithium chloride gas by the chlorination reaction and desublimating the gas.
Description
Technical Field
The invention relates to a preparation method of lithium chloride and a device thereof.
Background
As lithium is applied to various fields, attention is increasingly paid to methods and techniques for recovering lithium resources. For example, it can be prepared from spodumene (LiAlSi) 2 O 6 ) Mineral extraction of LiCl for use as Li 2 CO 3 The raw materials of (1).
At present, from spodumene (LiAlSi) 2 O 6 ) The ores were used to prepare LiCl using a wet process. The method specifically adopts the following process: oxidizing and roasting spodumene, leaching and neutralizing by sulfuric acid process, refining, evaporating and concentrating to prepare Li 2 CO 3 。
However, when lithium is extracted by a wet method using sulfuric acid, there is a problem that various costs such as labor costs, management costs, and the like are high due to a complicated process. Moreover, environmental problems due to waste residues also arise.
Therefore, development of an environmentally friendly lithium extraction technology is required by developing a simple process based on a dry process. The technology for extracting lithium by a dry method is simple in process, and no impurities exist in residues, so that profits are easily created, and the problem of environmental pollution can be solved.
Disclosure of Invention
One embodiment of the present invention relates to a method for preparing lithium chloride from spodumene ore using a dry flow chlorination process and an apparatus therefor.
Specifically, the present invention aims to extract lithium chloride by chlorination reaction after mixing coke and chlorine gas into spodumene ore.
The method for preparing lithium chloride according to an embodiment of the present invention may include a step of mixing spodumene and chlorine gas and then performing a chlorination reaction, and a step of generating lithium chloride gas through the chlorination reaction and desublimating the gas.
The step of chlorination reaction may be performed at a temperature range of 1100 ℃ or higher.
Specifically, the spodumene ore and chlorine gas may further contain coke.
The coke may be mixed to 0.3 wt% or less with respect to 100 wt% of the spodumene ore. More specifically, the coke may be mixed in a range of 0.01 to 0.3 wt% with respect to 100 wt% of the spodumene ore.
After the step of the chlorination reaction under the foregoing conditions, the amount of lithium element contained in 100 wt% of spodumene ore may be 2.8 wt% or less.
Further specifically, the step of chlorination reaction may be carried out at a temperature ranging from above 1100 ℃ to below 1200 ℃.
In the step of the chlorination reaction, the spodumene and chlorine gas may further include coke. At this time, the coke may be mixed to 0.01 to 0.2 wt% with respect to 100 wt% of the spodumene ore.
After the step of the chlorination reaction under the foregoing conditions, the amount of lithium element contained in 100 wt% of spodumene ore may be 1.5 wt% or less.
Still more specifically, the step of chlorination reaction may be carried out at a temperature in the range of 1200 ℃ to 1400 ℃.
In the step of the chlorination reaction, the spodumene ore and chlorine gas may further contain coke. At this time, the coke may be mixed to 0.04 wt% to 0.28 wt% with respect to 100 wt% of the spodumene ore.
After the step of the chlorination reaction under the foregoing conditions, the amount of lithium element contained in 100 wt% of the spodumene ore may be 1.0 wt% or less.
The step of the chlorination reaction may be performed under a pressure of 0.1 to 1atm.
In the chlorination step, the flow rate of chlorine gas can be 300sccm/min to 1500sccm/min.
The step of chlorination reaction may be performed for 5 minutes to 2 hours.
The desublimation step may cool the generated lithium chloride gas to 10 to 770 ℃. Specifically, by the desublimation step, lithium chloride in a solid state can be extracted and prepared.
The average particle diameter of the coke may be 100 to 400 μm.
An apparatus for preparing lithium chloride according to another embodiment of the present invention may comprise: a hopper for supplying spodumene ore, coke, or a combination thereof; a selective chlorinator connected to a lower portion of the hopper for causing a chlorination reaction; and a desublimation device connected to an upper portion of the selective chlorination device, for desublimating lithium chloride gas generated by the chlorination reaction.
The selective chlorinator also comprises a byproduct collector which is connected to the upper part of the selective chlorinator and is used for collecting byproducts generated by the chlorination reaction.
According to one embodiment of the invention, lithium chloride (LiCl) can be continuously produced from the primary ore by a dry process. Specifically, lithium chloride can be easily prepared by omitting the step of pretreating the ore using a flow chlorination system.
Drawings
Fig. 1 is a schematic view of an apparatus for preparing lithium chloride according to an embodiment of the present invention.
Fig. 2 is a graph showing the amount of change in residual lithium in spodumene ore based on the chlorination reaction temperature and the coke addition amount of examples and comparative examples.
Detailed Description
The advantages, features and methods of accomplishing the same may be understood more clearly with reference to the drawings and the following detailed description of the embodiments. However, the present invention can be embodied in various different forms and is not limited to the embodiments disclosed below. The following examples are put forth so as to provide those skilled in the art with a complete and complete understanding of the present invention, and are to be construed as being afforded the full scope of the invention as defined by the appended claims. Like reference numerals denote like constituent elements throughout the specification.
Accordingly, in some embodiments, well-known techniques are not described in detail to avoid obscuring the present invention. Unless otherwise defined, all terms (including technical and scientific terms) used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In the following description, when a certain component is "included" in a certain portion, unless specifically stated to the contrary, it means that other components are further included, and other components are not excluded. The singular forms are also intended to include the plural forms unless otherwise specified.
The method for preparing lithium chloride according to an embodiment of the present invention may include a step of mixing spodumene and chlorine gas and then performing a chlorination reaction, and a step of generating lithium chloride gas through the chlorination reaction and desublimating the gas.
First, it is possible to carry out the process of calcining spodumene ore (LiAlSi) 2 O 6 ) And a step of performing chlorination reaction after mixing with chlorine.
The specific reaction is shown in the following reaction formula 1.
[ reaction formula 1]
LiAlSi 2 O 6 (s)+1/2Cl 2 (g)＝LiCl+1/4O 2 (g)+1/6Al 6 Si 2 O 13 (s)+5/3SiO 2
Specifically, after mixing spodumene ore with chlorine gas, the chlorination reaction is performed to extract lithium element contained in the spodumene ore as lithium chloride.
The chlorination reaction step may be carried out at a temperature in the range of 1100 ℃ or higher.
At the temperature range, the reaction of the reaction formula 1 as described above may be caused.
Specifically, in the chlorination reaction step, the spodumene ore and chlorine gas may further contain coke.
At this time, the coke may be mixed in a ratio of 0.3 wt% or less with respect to 100 wt% of spodumene ore.
More specifically, the coke may be mixed in a proportion of 0.01 to 0.3% with respect to 100% by weight of spodumene ore.
The reaction when coke is added is shown in the following reaction formula 2.
[ reaction formula 2]
2LiAlSi 2 O 6 (s)+Coke(s)+Cl 2 (g)＝2LiCl(g)+CO(g)+Al 2 Si 4 O 11 (s)
The coke has the function of increasing chlorine (Cl) in ore 2 ) The reaction rate of (2). Specifically, by mixing the coke in the above range, the effect of improving the production efficiency can be obtained.
Accordingly, after the chlorination reaction step is performed according to the conditions, the amount of lithium element contained in 100 wt% of spodumene ore may be 2.8 wt% or less. More specifically, it may be 2.5% by weight or less.
More specifically, the chlorination reaction step may be carried out at a temperature ranging from greater than 1100 ℃ to less than 1200 ℃.
At this time, the coke may be mixed in a ratio of 0.01 to 0.2 wt% with respect to 100 wt% of spodumene ore.
More specifically, when 0.01 to 0.2 wt% of coke is added with respect to 100 wt% of spodumene ore at the temperature range, lithium elements remaining in the spodumene ore can be easily extracted. Still more specifically, in the aforementioned temperature range, when coke is added in an amount higher than the ratio, chlorination of oxides other than lithium may be initiated to cause a decrease in the purity of lithium chloride.
Accordingly, the amount of lithium element contained in 100 wt% of spodumene ore after the chlorination reaction step may be 1.5 wt% or less.
Still more specifically, the chlorination reaction step may be carried out at a temperature in the range of 1200 ℃ to 1400 ℃.
At this time, the coke may be mixed in a range of 0.04 wt% to 0.28 wt% with respect to 100 wt% of the spodumene ore. Specifically, it may be mixed in a range of 0.04 to 0.25% by weight.
Specifically, when 0.04 wt% to 0.28 wt% of coke is added with respect to 100 wt% of spodumene ore at the temperature range, it is easier to extract lithium element remaining in the spodumene ore. Still more specifically, at the aforementioned temperature range, when coke is added in an amount higher than the ratio, it is possible that the chlorination reaction of oxides other than lithium leads to a decrease in the purity of lithium chloride.
In addition, if the chlorination reaction is performed at a temperature range higher than 1400 ℃, the preparation cost may be increased.
Therefore, by performing the chlorination reaction step at the aforementioned temperature range, the spodumene ore can be phase-transformed from the α phase to the β phase.
As described above, the lithium element can be more easily extracted by the phase transition from the α phase to the β phase. Specifically, the phase transformation was a β -phase, and the volume of the spodumene ore increased by about 30%. Therefore, the porosity is also increased, and the reactivity is further improved.
Accordingly, the amount of lithium element contained in 100 wt% of spodumene ore may be 1.0 wt% or less.
The average particle diameter of the coke in the chlorination reaction step may be about 100 to 400 μm.
Specifically, if the particle diameter of the coke is too small, the aggregation phenomenon may result in failure to perform the chlorination reaction.
The flow rate of the chlorine gas mixed in the chlorination reaction step can be 300sccm/min to 1500sccm/min.
Specifically, if the flow rate of chlorine gas is within the range, the chlorination reaction can be sufficiently performed. More specifically, if the flow rate of chlorine gas is small, the flow is not smooth, and the chlorination reaction may be difficult to proceed.
The chlorination reaction step may be performed at a pressure of 0.1 to 1atm.
The fluidization reaction proceeds only if the pressure range falls within the range.
In addition, the chlorination reaction step may be performed for 5 minutes to 2 hours.
When the chlorination reaction is carried out for the aforementioned time, the lithium element remaining in the spodumene ore can be efficiently extracted.
In the chlorination reaction step, lithium element remaining in the spodumene ore can be generated as lithium chloride gas as shown in the above reaction formulae 1 and 2. Therefore, the amount of lithium element remaining in the spodumene ore is reduced.
By the chlorination reaction step, metal oxides other than lithium can also be produced. The metal oxide may comprise SiO 2 .Al 2 O 3 An oxide.
The oxide may be discharged as a dry byproduct by a byproduct trap in an apparatus described below. The discharged by-product can be used as raw materials of cement, heat insulating materials and the like.
Then, a step of generating lithium chloride gas by the chlorination reaction and desublimating the gas may be performed.
Specifically, for the lithium chloride gas generated by the chlorination reaction step, solid lithium chloride may be prepared by the desublimation step. Therefore, lithium chloride can be finally extracted by the desublimation step.
Specifically, the desublimation step may cool the generated lithium chloride gas to 10 to 700 ℃. Still further specifically, it may be cooled to 20 ℃ to 550 ℃.
More specifically, the lithium chloride gas can be converted to a solid form and collected only upon cooling to the temperature.
An apparatus for preparing lithium chloride according to another embodiment of the present invention may comprise: a hopper for supplying spodumene ore, coke, or a combination thereof; a selective chlorinator connected to a lower portion of the hopper for causing a chlorination reaction; and a desublimation device connected to an upper portion of the selective chlorination device, for desublimating lithium chloride gas generated by the chlorination reaction.
Specifically, the spodumene ore, coke, or a combination thereof may be supplied to a selective chlorinator connected to a lower portion of a Hopper (Hopper).
A Selective chlorinator (Selective chlorinator) receiving spodumene ore, coke or a combination thereof from the hopper, and supplying chlorine gas (Cl) at a lower portion 2 ) To cause chlorination.
The conditions of the chlorination reaction at this time are as described in the above-mentioned method for producing lithium chloride.
Then, the lithium chloride gas generated by the chlorination reaction may move to a desublimation device connected to an upper portion of the selective chlorinator.
More specifically, in the desublimation device, cooling is performed as described in the foregoing lithium chloride production method, so that solid lithium chloride can be extracted.
Specifically, the selective chlorinator can further comprise a byproduct collector connected to the upper part of the selective chlorinator and used for collecting byproducts generated by the chlorination reaction. In this case, the byproduct collector may use a Cyclone collector (Cyclone), but is not limited thereto.
More specifically, after the aforementioned lithium chloride gas is discharged to the desublimation device connected to the upper portion of the selective chlorinator, the byproducts remaining in the chlorinator may be collected by a byproduct collector.
This is also shown in fig. 1.
Fig. 1 is a schematic view of an apparatus for preparing lithium chloride according to an embodiment of the present invention.
The following is a detailed description by way of example. However, the following examples are merely illustrative of the present invention, and the present invention is not limited to the following examples.
Examples
After the spodumene ore and coke charging hopper (hopper) were supplied to the flow chlorinator, chlorine gas was further added to the flow chlorinator to perform chlorination reaction. At this time, the particle size of the ore and coke is maintained in the range of about 100 μm to 400 μm.
The method of receiving from the hopper is to mix the spodumene ore and the coke and then inject the mixture into the hopper from the upper part.
The flow rate of the chlorine gas is 1000sccm/min. The pressure inside the flow chlorinator is 1atm.
At this time, the chlorination reaction temperature and the amount of coke added were varied as shown in table 1 below to conduct the test.
After performing the chlorination reaction at the temperature disclosed in the following table 1 for 1 hour, the generated lithium chloride (LiCl) gas was cooled to 25 ℃ in a condenser (condenser) to prepare LiCl in a solid state.
Further, siO is a product of the preparation 2 ·Al 2 O 3 And discharged as a by-product through a Cyclone collector (Cyclone).
As a result, in order to compare the chlorination reaction degree based on the reaction temperature and the coke addition amount, the amount of lithium remaining in the spodumene ore was measured after extracting lithium chloride according to the examples and comparative examples. The amount of residual lithium in the spodumene ore was determined by inductively coupled plasma emission spectrometry (ICP-AES). The average values of the measurement values obtained after two or more measurements are shown in table 1.
[ Table 1]
In particular, it can be seen that, for the examples satisfying the temperature range and the coke addition amount according to one embodiment of the present invention, the effect of extracting lithium from spodumene ore is more superior than the comparative examples that do not satisfy the temperature range and the coke addition amount.
More specifically, it can be seen that the amount of residual lithium in the spodumene ore is reduced more as the chlorination reaction temperature is higher also in the examples.
As can be seen from the results of the chlorination reaction performed at 1100 deg.c or more according to the example of the present invention, the amount of residual lithium in the spodumene ore was reduced to at least 2.73% (example 1). It can be seen that the examples of the present application extracted residual lithium in the spodumene ore as lithium chloride.
Furthermore, in the case of adding coke in example 1 (examples 2 to 5), the amount of lithium remaining in the spodumene ore was further reduced.
In addition, it can be seen that the amount of residual lithium in the spodumene ore is more reduced in the temperature range of more than 1100 ℃. Further specifically, even in examples in which the chlorination reaction was carried out at 1150 ℃, the lithium extraction effects of examples 7-9 in which coke was added at a ratio of 0.01% to 0.2% were the most excellent.
At a temperature range of 1200 c or higher, the lithium extraction effect is more superior than in the foregoing examples 1 to 9. Specifically, it can be seen that in examples in which the chlorination reaction was carried out at 1200 ℃ or more, the amount of residual lithium in the spodumene ores of examples 12 to 17 to which coke was added in a proportion of 0.04% to 0.28% was very small. That is, it can be concluded that the most lithium chloride was produced.
On the other hand, it can be seen that the amount of residual lithium in the spodumene ore of comparative example 2 in which the chlorination reaction was performed at 900 ℃ was 3.09 wt%, and the lithium chloride production effect was better than that of comparative example 1 in which the amount of residual lithium in the spodumene ore was 3.27 wt%, but was very poor with respect to the examples.
This is because, when the chlorination reaction is carried out at 900 ℃ as in comparative example 2, a phase transition from the α phase to the β phase is difficult to occur. In the case of comparative example 2, the chlorination reaction in the alpha phase state would occur because the reaction efficiency would theoretically decrease without increasing the rate of porosity in the ore.
The correlation result can also be confirmed by fig. 2.
Fig. 2 is a graph showing the amount of change in residual lithium in the spodumene ore based on the chlorination reaction temperature and the coke addition amount of examples and comparative examples.
The embodiments of the present invention have been described above with reference to the drawings, but it is understood that those skilled in the art to which the present invention pertains can implement the present invention in other specific ways without changing the technical idea or essential features.
It is therefore to be understood that the above-described embodiments are illustrative in all respects, and not restrictive. The scope of the present invention should be determined by the appended claims, rather than by the description herein, and all changes and modifications that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
Claims (13)
1. A method for preparing lithium chloride, comprising:
mixing spodumene and chlorine gas and then carrying out chlorination reaction; and
a step of generating lithium chloride gas by the chlorination reaction and desublimating the gas,
the step of chlorination is carried out at a temperature ranging from above 1100 ℃ to below 1200 ℃,
in the step of the chlorination reaction, the reaction mixture,
the spodumene ore and chlorine gas also contain coke,
the coke is blended to 0.04 wt% to 0.28 wt% relative to the total weight of the spodumene ore.
2. The method for producing lithium chloride according to claim 1, wherein,
after the step of the chlorination reaction is carried out,
the amount of residual lithium element in the spodumene ore is 2.8 wt% or less relative to the total weight of the spodumene ore.
3. A method for preparing lithium chloride, which comprises the steps of,
mixing the spodumene ore and chlorine gas and then carrying out chlorination reaction; and
a step of generating lithium chloride gas by the chlorination reaction and desublimating the gas,
the step of chlorination is carried out at a temperature ranging from above 1100 ℃ to below 1200 ℃,
and the spodumene ore and chlorine gas, in addition, also contain coke,
the coke is mixed to 0.01 to 0.2 wt% with respect to the total weight of the spodumene ore.
4. The method for producing lithium chloride according to claim 3, wherein,
after the step of the chlorination reaction is carried out,
the amount of residual lithium element in the spodumene ore is 1.5 wt% or less with respect to the total weight of the spodumene ore.
5. A method for preparing lithium chloride, which comprises the steps of,
mixing spodumene and chlorine gas and then carrying out chlorination reaction; and
a step of generating lithium chloride gas by the chlorination reaction and desublimating the gas,
the step of chlorination is carried out at a temperature in the range of 1200 ℃ to 1400 ℃,
in the step of the chlorination reaction, the reaction mixture,
the spodumene ore and chlorine gas also contain coke,
the coke is blended to 0.04 wt% to 0.28 wt% relative to the total weight of the spodumene ore.
6. The method for producing lithium chloride according to claim 5, wherein,
after the step of the chlorination reaction is carried out,
the amount of residual lithium element in the spodumene ore is 1.0 wt% or less relative to the total weight of the spodumene ore.
7. The method for producing lithium chloride according to any one of claims 1 to 6, wherein,
the step of the chlorination reaction is carried out under a pressure of 0.1 to 1atm.
8. The method for producing lithium chloride according to any one of claims 1 to 6, wherein,
in the step of the chlorination reaction, the reaction mixture,
the flow rate of chlorine gas is 300sccm to 1500sccm.
9. The method for producing lithium chloride according to any one of claims 1 to 6, wherein,
the step of chlorination is carried out for 5 minutes to 2 hours.
10. The method for producing lithium chloride according to any one of claims 1 to 6, wherein,
the desublimation step is to cool the generated lithium chloride gas to 10 ℃ to 770 ℃.
11. The method for producing lithium chloride according to any one of claims 1 to 6, wherein,
the average particle diameter of the coke is 100 to 400 μm.
12. An apparatus for preparing lithium chloride, comprising:
a hopper for supplying spodumene ore, coke, or a combination thereof;
a selective chlorinator connected to a lower portion of the hopper for causing a chlorination reaction; and
a desublimation device connected to an upper portion of the selective chlorination device for desublimating lithium chloride gas generated by a chlorination reaction,
the coke is mixed to 0.01 to 0.28 wt% with respect to the total weight of the spodumene ore.
13. The apparatus for producing lithium chloride as claimed in claim 12, wherein,
the selective chlorinator also comprises a byproduct collector which is connected with the upper part of the selective chlorinator and is used for collecting byproducts generated by chlorination reaction.
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| KR1020180065556A KR102063810B1 (en) | 2018-06-07 | 2018-06-07 | Method for manufacturing lithiumchlorid and device of the same |
| KR10-2018-0065556 | 2018-06-07 | ||
| PCT/KR2018/009871 WO2019235687A1 (en) | 2018-06-07 | 2018-08-27 | Method and apparatus for producing lithium chloride |
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| KR102400897B1 (en) * | 2019-12-20 | 2022-05-20 | 주식회사 포스코 | Method of extracting lithium from lithium-containing ore |
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| WO2019235687A1 (en) | 2019-12-12 |
| AU2018427068A1 (en) | 2021-01-21 |
| KR102063810B1 (en) | 2020-01-08 |
| KR20190139048A (en) | 2019-12-17 |
| CN112351953A (en) | 2021-02-09 |
| AU2018427068B2 (en) | 2022-03-10 |
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