KR101873933B1 - Manufacturing method of lithium hydroxide using lithium carbonate - Google Patents
Manufacturing method of lithium hydroxide using lithium carbonate Download PDFInfo
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- KR101873933B1 KR101873933B1 KR1020170167493A KR20170167493A KR101873933B1 KR 101873933 B1 KR101873933 B1 KR 101873933B1 KR 1020170167493 A KR1020170167493 A KR 1020170167493A KR 20170167493 A KR20170167493 A KR 20170167493A KR 101873933 B1 KR101873933 B1 KR 101873933B1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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Abstract
Description
The present invention relates to a process for producing lithium hydroxide using lithium carbonate, and more particularly, to a process for producing lithium hydroxide by recycling calcium carbonate, which is a by-product produced in the process of producing lithium hydroxide, The present invention also relates to a process for producing lithium hydroxide using lithium carbonate which exhibits an effect.
Lithium hydroxide is used in the form of monohydrate or anhydride and is used in gas and air purification, heat transfer media, polymerization catalysts, improved grease production that can perform well at extreme temperatures, carbon dioxide absorbents in submarines and spacecrafts, And is used as a raw material of a lithium compound.
In addition, recently, as the market for electric vehicles has grown as a raw material for the cathode material of lithium secondary batteries used in electric vehicles, the market for lithium hydroxide has also been rapidly growing.
A conventional method for producing lithium hydroxide is a method for producing lithium hydroxide by reacting calcium hydroxide with lithium hydroxide.
[Reaction Scheme 1]
Li 2 CO 3 (S) + Ca (OH) 2 (S) + H 2 O (L)? 2LiOH.H 2 O (aq) + CaCO 3 (S)
The conventional method of producing lithium hydroxide generates about 1.2 ton of calcium carbonate as a by-product in order to produce 1 ton of lithium hydroxide, and calcium carbonate is inevitably discharged in the form of a calcium carbonate cake having a water content of 35 to 45 wt% . In the case of calcium carbonate cake having a water content of 40 wt%, about 2 tons is generated to produce 1 ton of lithium hydroxide. Calcium carbonate generated in the conventional process is a strong alkali cake containing lithium hydroxide as impurities. It is classified as municipal designated waste, resulting in high costs for disposal.
In addition, depending on the concentration of the aqueous solution of lithium hydroxide generated in terms of the yield of lithium, lithium loss may be generated up to 10 wt% compared to the amount of lithium supplied.
Korean Patent No. 10-0725589 discloses a method for producing lithium hydroxide using lithium carbonate waste and calcium hydroxide. However, as in the conventional commercialized processes, there is a problem that calcium carbonate is a byproduct, The concentration of the lithium hydroxide aqueous solution produced by converting lithium hydroxide into a solution phase by the solubility of lithium is low and the amount of lithium lost by the calcium carbonate cake can be reduced but there is a problem in that much evaporation cost is incurred in crystallizing lithium hydroxide there was.
Korean Patent No. 10-1179505 discloses a method for producing lithium hydroxide by using lithium carbonate waste and hydrogen peroxide. Although the prior art has the advantage that no byproduct is generated, the hydrogen peroxide is highly oxidative It is very dangerous when exposed to a human body and has explosive reactivity. In order to prevent this, it is necessary to react at a very low concentration to prepare a low concentration aqueous solution of lithium hydroxide, thereby causing a lot of evaporation cost to crystallize lithium hydroxide .
An object of the present invention is to provide a process for producing lithium hydroxide by using lithium carbonate which is environmentally friendly by recycling calcium carbonate, which is a by-product generated in the process of producing lithium hydroxide, and which exhibits an effect of reducing the processing cost and by- will be.
It is an object of the present invention to provide a process for producing a lithium carbonate slurry, which comprises preparing a lithium carbonate slurry to produce a lithium carbonate slurry, a calcium hydroxide reaction step in which a slurry of calcium carbonate is mixed with a lithium carbonate slurry prepared through the lithium carbonate slurry preparation step, A solid-liquid separation step of separating the reactant into calcium carbonate and an aqueous lithium hydroxide solution, and a lithium hydroxide recovery step of recovering lithium hydroxide in the aqueous solution of lithium hydroxide recovered through the solid-liquid separation step. After the solid-liquid separation step, The calcium carbonate recovered in the calcium hydroxide reaction step after the calcination of the calcium carbonate separated from the calcium carbonate slurry is converted into a calcium hydroxide slurry by mixing with water and then the calcium carbonate slurry is further recycled. .
According to a preferred aspect of the present invention, the lithium carbonate slurry is prepared by mixing 50 to 2500 parts by weight of water with 100 parts by weight of lithium carbonate.
According to a more preferred feature of the present invention, in the calcium hydroxide reaction step, the calcium hydroxide contained in the calcium hydroxide slurry is mixed with 98 to 130 parts by weight based on 100 parts by weight of lithium carbonate contained in the lithium carbonate slurry produced through the lithium carbonate slurry preparation step .
According to a further preferred feature of the present invention, the calcium hydroxide slurry is prepared by mixing 30 to 2500 parts by weight of water with 100 parts by weight of calcium oxide.
According to a further preferred feature of the present invention, the calcium hydroxide reaction step is carried out at a temperature of 20 to 90 DEG C for 10 to 300 minutes.
According to a further preferred feature of the present invention, the firing is performed at a temperature of 650 to 1300 캜 for 1 to 10 hours.
The process for producing lithium hydroxide using lithium carbonate according to the present invention is not only environmentally friendly by recycling calcium carbonate, which is a by-product produced in the process of producing lithium hydroxide, but also exhibits an excellent effect of reducing the processing cost and raw material cost of by-products.
1 is a flowchart showing a method for producing lithium hydroxide using lithium carbonate according to the present invention.
FIG. 2 shows the results of XRD analysis of lithium hydroxide recovered through Example 1 of the present invention.
3 is a result of XRD analysis of calcium carbonate calcined 5 times through Example 1 of the present invention.
Hereinafter, preferred embodiments of the present invention and physical properties of the respective components will be described in detail with reference to the accompanying drawings. However, the present invention is not limited thereto, And this does not mean that the technical idea and scope of the present invention are limited.
The method for producing lithium hydroxide using lithium carbonate according to the present invention comprises the steps of preparing a lithium carbonate slurry (S101) for producing a lithium carbonate slurry, mixing the slurry of calcium hydroxide with the lithium carbonate slurry produced through the step (S101) (S103), a solid-liquid separation step (S105) of separating the reactant prepared through the calcium hydroxide reaction step (S103) into a calcium carbonate and an aqueous lithium hydroxide solution, and a solid-liquid separation step (S105) And a lithium hydroxide recovery step (S107) for recovering lithium hydroxide in an aqueous solution of lithium hydroxide. After the solid-liquid separation step (S105), the calcium carbonate separated in the solid-liquid separation step is calcined and mixed with water to convert it into a calcium hydroxide slurry Thereafter, the calcium carbonate recycle step (S106) to be reused in the calcium hydroxide reaction step (S103) is further performed.
The lithium carbonate slurry preparation step (S101) is a step of preparing a lithium carbonate slurry, wherein 50 to 2500 parts by weight of water is mixed with 100 parts by weight of lithium carbonate. The water used in the lithium carbonate slurry preparation step (S101) Although not particularly limited, various kinds of water may be used depending on the purity of the finally produced lithium hydroxide and the intended use. For example, when producing lithium hydroxide for use in electric vehicles, high purity is required, and therefore it is preferable to use water having a RO number or more.
The mixing ratio of lithium carbonate and water in the lithium carbonate slurry preparation step (S101) is variable depending on the lithium concentration of the slurry after the reaction and the amount of water used in the preparation of the calcium hydroxide slurry. After the reaction, the lithium concentration of the slurry is lithium hydroxide Lt; RTI ID = 0.0 > saturation < / RTI >
For example, at 20 ° C and a lithium concentration of 37 g / L or more, lithium hydroxide may be supersaturated and precipitated as crystals. In such a case, calcium carbonate and lithium hydroxide precipitate are present together, resulting in a lower recovery rate of lithium hydroxide. If the amount of water exceeds 2500 parts by weight, the concentration of lithium in the slurry after the reaction becomes too low to concentrate and concentrate lithium to crystallize lithium, so that the mixing ratio of lithium carbonate to water is 100 parts by weight of water Preferably 50 to 2000 parts by weight.
The calcium hydroxide reaction step (S103) is a step of mixing and reacting the calcium carbonate slurry with the lithium carbonate slurry prepared in the step (S101) of preparing the lithium carbonate slurry, And the calcium hydroxide contained in the calcium hydroxide slurry is mixed in a proportion of 98 to 130 parts by weight based on 100 parts by weight of the lithium carbonate and the mixture is reacted at a temperature of 20 to 90 DEG C for 10 to 300 minutes.
In the calcium hydroxide reaction step (S103), the calcium hydroxide contained in the slurry of calcium hydroxide is mixed with 98 to 130 parts by weight based on 100 parts by weight of the lithium carbonate contained in the lithium carbonate slurry so as to be reacted. If the amount of calcium hydroxide contained in the calcium hydroxide slurry is less than 98 parts by weight based on 100 parts by weight of lithium carbonate contained in the lithium carbonate slurry in step S103, the content of unreacted lithium carbonate in the aqueous lithium hydroxide solution is increased, When the content of the calcium hydroxide exceeds 130 parts by weight, calcium impurities increase in the aqueous solution of lithium hydroxide.
It is preferable that the lithium concentration of the total slurry obtained by mixing the lithium carbonate slurry and the calcium hydroxide slurry is maintained below the lithium hydroxide saturation concentration by the correlation with the lithium hydroxide recovery rate in the lithium carbonate slurry preparation step (S101) , The total slurry obtained by mixing the lithium carbonate slurry and the calcium hydroxide slurry is preferably prepared by mixing 50 to 2500 parts by weight of water with 100 parts by weight of lithium carbonate.
If the reaction temperature is lower than 20 ° C or the reaction time is less than 10 minutes, the reaction rate and conversion rate are largely lowered, and when the reaction temperature is lower than 20 ° C or the reaction time is less than 10 minutes, If the temperature exceeds 90 ° C or the reaction time exceeds 300 minutes, the evaporation rate of water during the reaction may be excessively increased, so that the lithium concentration of the reaction slurry may be concentrated above the saturation concentration of lithium hydroxide.
It is preferable that the calcium hydroxide slurry is prepared by mixing 30 to 2500 parts by weight of water with 100 parts by weight of calcium oxide.
The solid-liquid separation step (S105) is a step of separating the reactant produced through the calcium hydroxide reaction step (S103) into calcium carbonate and lithium hydroxide aqueous solution. The reactant produced through the calcium hydroxide reaction step (S103) A step of separating the solid calcium carbonate into a liquid aqueous solution of lithium hydroxide using a conventional method such as a press and a centrifugal separator.
The solid-liquid separation method used in the solid-liquid separation step (S105) is not particularly limited as long as it is a separation method in which calcium carbonate fine particles are not present in the lithium hydroxide aqueous solution in addition to the methods listed above.
In addition, it is preferable that the moisture content of the calcium carbonate recovered through the solid-liquid separation step (S105) is kept as low as possible.
After the solid-liquid separation step (S105), the calcium carbonate recycled in the solid-liquid separation step (S105) is recycled in the calcium hydroxide reaction step after the calcined calcium carbonate is calcined and mixed with water to form a calcium hydroxide slurry It proceeds.
The calcium carbonate recovered in the solid-liquid separation step (S105) is converted into calcium oxide through calcination, and then 30 to 2500 parts by weight of water is mixed with 100 parts by weight of the converted calcium oxide to prepare a calcium hydroxide slurry, When the calcium carbonate as a by-product, which is a by-product, is recycled in the calcium hydroxide reaction step after the calcium carbonate slurry is recovered through the above process, the calcium carbonate which is disposed of is recycled to be eco-friendly and the calcium carbonate as a by- And a raw material cost for purchasing a calcium hydroxide slurry can be saved.
At this time, it is preferable that the firing is performed at a temperature of 650 to 1300 ° C for 1 to 10 hours. If the firing temperature is less than 650 ° C or the firing time is less than 1 hour, the thermal decomposition of the calcium carbonate does not proceed properly, Exceeds 1300 DEG C or the firing time exceeds 10 hours, the lithium remaining in the calcium carbonate reacts with calcium to generate a poorly soluble LixCaxOx and the like, so that the conversion of the calcium hydroxide slurry is lowered and the unreacted lithium .
The step of recovering lithium hydroxide (S107) is a step of recovering lithium hydroxide in the recovered lithium hydroxide aqueous solution through the solid-liquid separation step (S105). The recovered lithium hydroxide solution is recovered by vacuum evaporation It is the step of recovering lithium hydroxide by applying the painting method.
Hereinafter, the process for producing lithium hydroxide using lithium carbonate according to the present invention and the physical properties of lithium hydroxide prepared through the process will be described with reference to examples.
PREPARATION EXAMPLE 1 Preparation of Lithium Carbonate Slurry
200 g of a lithium carbonate slurry was prepared by mixing 180 g of water with 20 g of lithium carbonate (purity: 99.8 wt%).
PREPARATION EXAMPLE 2 Preparation of calcium hydroxide slurry
16.6 g of calcium hydroxide and 210.4 g of water were mixed to prepare 227 g of a calcium hydroxide slurry.
≪ Example 1 >
227 g of the calcium hydroxide slurry prepared in Preparation Example 2 was introduced into 200 g of the lithium carbonate slurry prepared in Preparation Example 1, and the mixture was reacted at a temperature of 70 ° C for 2 hours. The solid calcium carbonate separated and separated by solid-liquid separation by a centrifugal separator was calcined at a temperature of 650 ° C for 3 hours to convert it to calcium oxide, and 210.4 g of water was mixed with 16.6 g of the converted calcium oxide to prepare a calcium hydroxide slurry. Was repeated five times. The aqueous lithium hydroxide solution separated from the centrifugal separator was recovered and then crystallized by vacuum evaporation crystallization method to recover lithium hydroxide.
The recovered lithium recovered through Example 1 was measured and shown in Table 1 below.
<Table 1>
As shown in Table 1, calcium carbonate generated during the reaction of lithium carbonate and calcium hydroxide was calcined / hydrated and reused as calcium hydroxide. As a result, it was confirmed that about 94% of lithium was uniformly recovered in the aqueous lithium hydroxide solution .
In addition, as a result of crystallizing lithium hydroxide from the aqueous solution of lithium hydroxide recovered in the fifth repetition, it was confirmed that pure lithium hydroxide monohydrate was produced as shown in FIG. 2 below.
3, it can be confirmed that pure calcined calcium oxide is produced upon calcination of calcium carbonate even after 5 repetitions.
≪ Comparative Example 1 &
The procedure of Example 1 was followed except that the calcination temperature of calcium carbonate was changed from 1300 占 폚 to 3 hours to recover lithium hydroxide.
The recovery rate of lithium recovered through Comparative Example 1 was measured and shown in Table 2 below.
<Table 2>
As shown in Table 2 above, it can be seen that the recovery of lithium recovered in the lithium hydroxide aqueous solution becomes lower as the number of repetition increases as a result of calcination / hydration of calcium carbonate occurring during the reaction of lithium carbonate and calcium hydroxide and as calcium hydroxide.
≪ Comparative Example 2 &
Lithium hydroxide was recovered by mixing 100 g of the calcium hydroxide slurry prepared in Preparation Example 2 with 200 g of the lithium carbonate slurry prepared in Preparation Example 1, by proceeding in the same manner as in Example 1 above.
≪ Comparative Example 3 &
Lithium hydroxide was recovered by mixing 160 g of the calcium hydroxide slurry prepared in Preparation Example 2 with 200 g of the lithium carbonate slurry prepared in Preparation Example 1, in the same manner as in Example 1.
Recovery rates of lithium recovered through Comparative Examples 2 to 3 were measured and are shown in Table 3 below.
<Table 3>
As shown in Table 3 above, when the amount of calcium hydroxide aqueous solution is insufficient as in Comparative Examples 2 and 3, the lithium concentration of the generated lithium aqueous solution is low and the recovery rate of lithium is low.
S101; Lithium carbonate slurry preparation step
S103; Calcium hydroxide reaction step
S105; Solid-liquid separation step
S106; Calcium carbonate recycling step
S107; Lithium hydroxide recovery step
Claims (6)
A calcium hydroxide reaction step of mixing and reacting a slurry of calcium hydroxide with the lithium carbonate slurry prepared through the step of preparing the lithium carbonate slurry;
A solid-liquid separation step of separating the reactant prepared through the calcium hydroxide reaction step into calcium carbonate and aqueous lithium hydroxide solution; And
And a lithium hydroxide recovery step of recovering lithium hydroxide in the recovered aqueous solution of lithium hydroxide through the solid-liquid separation step,
After the solid-liquid separation step, the calcium carbonate separated in the solid-liquid separation step is calcined and further mixed with water to convert it into a calcium hydroxide slurry and then reused in the calcium hydroxide reaction step,
The calcium hydroxide reaction step is carried out at a temperature of 70 DEG C for 2 hours,
Wherein the calcination is carried out at 650 DEG C for 3 hours to convert to calcium oxide.
Wherein the lithium carbonate slurry is prepared by mixing 50 to 2500 parts by weight of water with 100 parts by weight of lithium carbonate.
Wherein the calcium hydroxide reaction step is carried out such that the calcium hydroxide contained in the calcium hydroxide slurry is mixed in a proportion of 98 to 130 parts by weight based on 100 parts by weight of the lithium carbonate contained in the lithium carbonate slurry produced through the lithium carbonate slurry preparation step. (Process for producing lithium hydroxide using lithium).
Wherein the calcium hydroxide slurry is prepared by mixing 30 to 2500 parts by weight of water with 100 parts by weight of calcium oxide.
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Cited By (11)
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CN110395748A (en) * | 2019-08-27 | 2019-11-01 | 福建常青新能源科技有限公司 | The method that lithium carbonate causticizing process prepares lithium hydroxide |
KR102122156B1 (en) * | 2019-07-19 | 2020-06-11 | 전웅 | Method of preparing lithium hydroxide |
KR20200069054A (en) | 2018-12-06 | 2020-06-16 | 주식회사 에코프로이노베이션 | Preparation method of lithium hydroxide from lithium concentration by calcination with sodium sulfate |
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KR102122156B1 (en) * | 2019-07-19 | 2020-06-11 | 전웅 | Method of preparing lithium hydroxide |
CN110395748A (en) * | 2019-08-27 | 2019-11-01 | 福建常青新能源科技有限公司 | The method that lithium carbonate causticizing process prepares lithium hydroxide |
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KR102382209B1 (en) * | 2021-10-28 | 2022-04-05 | 주식회사 리켐텍 | High-purity lithium hydroxide manufacturing method |
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KR20230065608A (en) | 2021-11-05 | 2023-05-12 | 전남대학교산학협력단 | Method for producing Lithium hydroxide using Lithium carbonate and Barium compounds |
KR102544969B1 (en) | 2021-11-05 | 2023-06-20 | 전남대학교산학협력단 | Method for producing Lithium hydroxide using Lithium carbonate and Barium compounds |
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