CN109292798B - Process for producing anhydrous lithium chloride by crystallization method - Google Patents
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Abstract
A process for producing anhydrous lithium chloride by a crystallization method is characterized by comprising the following steps: sequentially comprises the following steps: roasting, fine-turning, acidifying, mixing and squeezing lithium-containing minerals to obtain a lithium sulfate-containing leaching solution; adding calcium chloride for conversion, squeezing and filtering to obtain a squeezed filtrate; evaporating and concentrating the squeezed filtrate, cooling and filtering to obtain impurity-separated filter residue and impurity-separated filtrate; evaporating and concentrating the impurity-separated filtrate until solid is separated out, and performing heat preservation and centrifugal separation to obtain primary centrifugal mother liquor and primary centrifugal wet material; returning the primary centrifugal mother liquor to a cooling section; dissolving the primary centrifugal wet material, filtering, heating, evaporating and concentrating the filtrate until solid is separated out, and performing heat preservation and centrifugal separation to obtain secondary centrifugal mother liquor and a secondary centrifugal wet material; heating, evaporating and concentrating the secondary centrifugal mother liquor until solid is separated out, and drying the secondary centrifugal wet material to obtain the anhydrous lithium chloride product. The invention does not need to add barium chloride and carbonate in the whole process, has simple impurity removal process, low production cost and high purity of anhydrous lithium chloride.
Description
Technical Field
The invention relates to the field of preparation of anhydrous lithium chloride, and particularly relates to a process for producing anhydrous lithium chloride by a crystallization method.
Background
The anhydrous lithium chloride is mainly used for producing electrolytic lithium metal, and the existing anhydrous lithium chloride production method mainly comprises two main types: in either spray drying or crystallization method, a suitable lithium chloride solution is prepared in the early stage. In order to prepare a proper lithium chloride solution, the lithium chloride solution needs to be subjected to impurity removal, so that the impurity content of the lithium chloride solution meets the requirements of a spray drying method and a crystallization method.
In the existing process for preparing anhydrous lithium chloride by a crystallization method, for example, in Chinese patents CN 100469696C, CN 101172624A, CN 105731503B, CN 105836767B and CN 101172624A, in order to prepare a proper lithium chloride solution, the calcium and sulfate radicals in the lithium chloride solution are all or partially subjected to impurity removal; wherein CN 100469696C, CN 101172624A, CN 105836767B, CN 101172624A is prepared by removing sulfate radical with barium chloride, removing calcium and barium with carbonate, and adjusting pH with hydrochloric acid to remove carbonate radical; patent CN 105731503B uses lithium sulfate and sodium chloride to prepare lithium chloride solution by freeze crystallization, but also needs to use carbonate to remove calcium. That is, the traditional crystallization process requires the operation of removing sulfate radical and calcium from the lithium chloride solution at the front end, usually barium chloride is added to remove sulfate radical, then calcium or excess barium is removed by carbonate, excess carbonate is removed by hydrochloric acid, the pH value is reversely adjusted to be neutral by alkali, and the neutralization solution is heated, evaporated, concentrated and crystallized once or twice, so that the qualified anhydrous lithium chloride product is obtained, and the production process is long.
Disclosure of Invention
The invention provides a process for producing anhydrous lithium chloride by a crystallization method, which solves the problems that the impurity removal process at the front end of the existing lithium chloride crystallization production process is long, the production cost is high, and the production is unsafe because barium chloride, a highly toxic chemical, is usually introduced for removing sulfate radicals.
In order to achieve the purpose, the invention adopts the technical scheme that: a process for producing anhydrous lithium chloride by a crystallization method sequentially comprises the following steps:
step (1), sequentially roasting, fine-turning, acidifying, mixing and squeezing lithium-containing minerals to obtain a leaching solution containing lithium sulfate;
step (2), adding calcium chloride into the leaching solution containing lithium sulfate for conversion, and then squeezing and filtering to obtain a squeezed filtrate;
heating the squeezed filtrate for evaporation and concentration, then cooling and filtering to obtain impurity separation filter residues and impurity separation filtrate, and washing the impurity separation filter residues;
heating, evaporating and concentrating the impurity-separated filtrate obtained in the step (3) until solid is separated out, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet material;
step (5), returning the primary centrifugal mother liquor obtained in the step (4) to the cooling section of the step (3), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (3); dissolving the primary centrifugal wet material obtained in the step (4) with water, filtering, heating, evaporating and concentrating the filtrate until solid is separated out, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and a secondary centrifugal wet material;
and (6) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (4) until solids are separated out, and drying the secondary centrifugal wet material obtained in the step (5) to obtain an anhydrous lithium chloride product.
The relevant content in the above technical solution is explained as follows:
1. in the scheme, in the step (2), the ratio of the sulfate radical to the calcium is 1.05-1.1: 1, adding calcium chloride into the leaching solution containing the lithium sulfate for conversion.
2. In the above scheme, in the step (3), the squeezed filtrate is heated, evaporated and concentrated to Li2The concentration of O is 180-220 g/L, and then the mixture is cooled to 20-40 ℃. Washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution. And (3) returning washing water obtained by washing the impurity-separated filter residue to the size mixing working section in the step (1).
3. In the scheme, in the step (4), the impurity-separated filtrate obtained in the step (3) is heated, evaporated and concentrated until 40% -50% of solids are separated out at 160-170 ℃.
4. In the scheme, in the step (5), 1.5-2 mL of the primary centrifugal wet material obtained in the step (4): dissolving 1g of water with a liquid-solid ratio, filtering, heating, evaporating and concentrating the filtrate until 40-50% of solids are separated out at 160-170 ℃.
5. In the scheme, in the step (6), the heating, evaporation and concentration are carried out until 40-50% of solids are separated out at 160-170 ℃, and the drying temperature is 150-200 ℃.
6. In the above scheme, in the step (1), Li is contained in the leaching solution containing lithium sulfate2The concentration of O is about 15-30 g/L lithium sulfate solution.
The design concept of the invention is as follows: the invention relates to a new process for producing anhydrous lithium chloride by a crystallization method, which needs to control the contents of four main impurity elements of sulfate radical, calcium, sodium and potassium when preparing an anhydrous lithium chloride product by the crystallization method, and avoids influencing the product quality. The new process by the invention is no longer requiredThe procedure of removing sulfate radical and calcium in the traditional crystallization method process comprises the steps of obtaining a squeezed filtrate after squeezing through proper conversion and proportioning of a front-end lithium sulfate solution and calcium chloride, heating, evaporating and concentrating the squeezed filtrate to Li2And (3) the concentration of O is 180-220 g/L, cooling to 20-40 ℃ for impurity separation, filtering to obtain impurity separation filtrate, and evaporating, concentrating and crystallizing the impurity separation filtrate twice to obtain a qualified anhydrous lithium chloride product. The specific process is as follows:
in the steps (2) and (3), after the leaching solution containing the lithium sulfate is converted with calcium chloride and is pressed and filtered, Li in the pressed filtrate2The O concentration is 15-30 g/L, SO4 2-The concentration is 3-4 g/L, Ca2+Concentration is 0.5-1.5 g/L, and the solution is heated, evaporated and concentrated to Li2The concentration of O reaches 180-220 g/L, the heating, evaporation and concentration at the moment are to improve the concentration of lithium sulfate in the solution and simultaneously separate out impurities, most of the impurities can be separated out after cooling, and the main components of impurity separation filter residues are sodium chloride, calcium sulfate and sodium sulfate. Li in impurity-separated filtrate2The concentration of O is 180-220 g/L, SO4 2-The concentration is 0.5 to 1 g/L, Ca2+The concentration is 0.5-1 g/L, which shows that the concentration of lithium sulfate is greatly improved, and the concentrations of sulfate radical and calcium ion are obviously reduced.
In the step (4), lithium chloride is a fixed main component precipitated after heating, evaporation and concentration. The potassium ions can be removed by heat preservation and centrifugal separation at the temperature of 150-160 ℃.
In the step (5), the primary centrifugal mother liquor obtained in the step (4) is returned to the cooling section of the step (3), so that a circulation is formed, lithium chloride is collected to the maximum extent, and calcium ions, sulfate ions and sodium ions can be further removed. And performing secondary centrifugal separation to further remove potassium ions.
In the step (6), the secondary centrifugal mother liquor is returned to the heating evaporation concentration section in the step (4), so that a circulation is formed in the novel process, lithium chloride is collected to the maximum extent, and potassium ions can be further removed.
In the above step, when Li2When the concentration of O reaches 180-220 g/L, salting out is carried out by using high-concentration chloride ionsEffect and Co-ion Effect of lithium ions SO4 2-Reduced to 0.5-1 g/L, Ca2+Reducing the concentration to 0.5-1 g/L, and crystallizing the impurity-separated filtrate twice to obtain an anhydrous lithium chloride product with qualified sulfate radicals and calcium, so that barium chloride is not added to remove sulfate radicals and carbonate is not used to remove calcium in the whole process.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention does not need to add barium chloride to remove sulfate radical and carbonate to remove calcium in the whole process, thereby having safer production.
(2) The impurity removal process is simple and low in production cost.
(3) The anhydrous lithium chloride prepared by the method has high purity, and the content of main impurities of the anhydrous lithium chloride is lower than the national standard of products.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further described below with reference to the following examples:
example 1: process for producing anhydrous lithium chloride by crystallization method
Sequentially comprises the following steps: (1) roasting, fine-turning, acidifying, leaching, size mixing and squeezing spodumene to obtain Li2100L of lithium sulfate-containing leaching solution with the O concentration of 15 g/L;
(2) adding 5.82kg of calcium chloride solid into the leachate, carrying out conversion reaction for half an hour, and then squeezing and filtering;
(3) heating the squeezed filtrate obtained in the previous step, evaporating and concentrating to 130 ℃ until Li is obtained2The concentration of O is 198 g/L, and the hot solution is filtered;
(4) cooling the filtrate obtained in the previous step to 30 ℃, then filtering to obtain impurity-separated filter residue and impurity-separated filtrate, and washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution; washing water obtained by washing impurity-separated filter residues returns to the size mixing working section in the step (1);
(5) heating, evaporating and concentrating the impurity-separated filtrate obtained in the previous step until 40% -50% of solids are separated out at 160 ℃, wherein the fact that 40% -50% of solids are separated out means that the volume of the separated solids accounts for 40% -50% of the volume of the mixed solution after evaporation and concentration; performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet materials;
(6) returning the obtained primary centrifugal mother liquor to the cooling working section in the step (4), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (4) to 20-40 ℃; the wet material obtained in the previous step is treated by a centrifugal separation method by using 1.5 mL: dissolving 1g of pure water with a liquid-solid ratio, heating, evaporating and concentrating until 41% of solids are separated out at 160 ℃, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and secondary centrifugal wet materials;
(7) and (3) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (5) until 40-50% of solids are separated out at 160-170 ℃, and drying the obtained secondary centrifugal wet material at 150-200 ℃ to obtain 0.426kg of anhydrous lithium chloride product.
Example 2: process for producing anhydrous lithium chloride by crystallization method
Sequentially comprises the following steps: (1) roasting, fine-turning, acidifying, leaching, size mixing and squeezing spodumene to obtain Li2100L of lithium sulfate-containing leaching solution with the O concentration of 20 g/L;
(2) adding 8.14kg of calcium chloride solid into the leachate, carrying out conversion reaction for half an hour, and then squeezing and filtering;
(3) heating the squeezed filtrate obtained in the previous step, evaporating and concentrating to 139 ℃ until Li is obtained2The O concentration is 218 g/L, and the hot solution is filtered;
(4) cooling the filtrate obtained in the previous step to 40 ℃, then filtering to obtain impurity-separated filter residue and impurity-separated filtrate, and washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution; washing water obtained by washing impurity-separated filter residues returns to the size mixing working section in the step (1);
(5) heating, evaporating and concentrating the impurity-separated filtrate obtained in the previous step until 40% of solids are separated out at 170 ℃; performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet materials;
(6) returning the obtained primary centrifugal mother liquor to the cooling working section in the step (4), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (4) to 20-40 ℃; 2mL of the primary centrifugal wet material obtained in the previous step: dissolving 1g of pure water with a liquid-solid ratio, heating, evaporating and concentrating until 43% of solids are separated out at 170 ℃, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and secondary centrifugal wet materials;
(7) and (3) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (5) until 40-50% of solids are separated out at 160-170 ℃, and drying the obtained secondary centrifugal wet material at 150-200 ℃ to obtain 0.513kg of anhydrous lithium chloride product.
Example 3: process for producing anhydrous lithium chloride by crystallization method
Sequentially comprises the following steps: (1) roasting, fine-turning, acidifying, leaching, size mixing and squeezing spodumene to obtain Li2100L of lithium sulfate-containing leaching solution with the O concentration of 20 g/L;
(2) adding 7.99kg of calcium chloride solid into the leachate, carrying out conversion reaction for half an hour, and then squeezing and filtering;
(3) heating the squeezed filtrate obtained in the previous step, evaporating and concentrating to 133 ℃ until Li is obtained2The O concentration is 203 g/L, and the hot solution is filtered;
(4) cooling the filtrate obtained in the previous step to 35 ℃, then filtering to obtain impurity-separated filter residue and impurity-separated filtrate, and washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution; washing water obtained by washing impurity-separated filter residues returns to the size mixing working section in the step (1);
(5) heating, evaporating and concentrating the impurity-separated filtrate obtained in the previous step until 40% of solids are separated out at 165 ℃; performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet materials;
(6) returning the obtained primary centrifugal mother liquor to the cooling working section in the step (4), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (4) to 20-40 ℃; the wet material obtained in the previous step is treated by a centrifugal separator with the following weight ratio of 1.7 mL: dissolving 1g of pure water with a liquid-solid ratio, heating, evaporating and concentrating until 46% of solids are separated out at 165 ℃, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and secondary centrifugal wet materials;
(7) and (3) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (5) until 40-50% of solids are separated out at 160-170 ℃, and drying the obtained secondary centrifugal wet material at 150-200 ℃ to obtain 0.573kg of anhydrous lithium chloride product.
Example 4: process for producing anhydrous lithium chloride by crystallization method
Sequentially comprises the following steps: (1) roasting, fine-turning, acidifying, leaching, size mixing and squeezing spodumene to obtain Li2100L of lithium sulfate-containing leaching solution with the O concentration of 30 g/L;
(2) adding 11.65kg of calcium chloride solid into the leachate, carrying out conversion reaction for half an hour, and then squeezing and filtering;
(3) heating the squeezed filtrate obtained in the previous step, evaporating and concentrating to 136 ℃ until Li is obtained2The O concentration is 213 g/L, and the hot solution is filtered;
(4) cooling the filtrate obtained in the previous step to 35 ℃, then filtering to obtain impurity-separated filter residue and impurity-separated filtrate, and washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution; washing water obtained by washing impurity-separated filter residues returns to the size mixing working section in the step (1);
(5) heating, evaporating and concentrating the impurity-separated filtrate obtained in the previous step until 43% of solids are separated out at 160 ℃; performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet materials;
(6) returning the obtained primary centrifugal mother liquor to the cooling working section in the step (4), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (4) to 20-40 ℃; the wet material obtained in the previous step is treated by a centrifugal separator with the volume of 1.8 mL: dissolving 1g of pure water with a liquid-solid ratio, heating, evaporating and concentrating until 48% of solids are separated out at 170 ℃, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and secondary centrifugal wet materials;
(7) and (3) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (5) until 40-50% of solids are separated out at 160-170 ℃, and drying the obtained secondary centrifugal wet material at 150-200 ℃ to obtain 0.867kg of anhydrous lithium chloride product.
Example 5: process for producing anhydrous lithium chloride by crystallization method
Sequentially comprises the following steps: (1) roasting, fine-turning, acidifying, leaching, size mixing and squeezing spodumene to obtain Li2150L of lithium sulfate-containing leaching solution with the O concentration of 24 g/L;
(2) adding 14.65kg of calcium chloride solid into the leachate, carrying out conversion reaction for half an hour, and then squeezing and filtering;
(3) heating the squeezed filtrate obtained in the previous step, evaporating and concentrating to 132 ℃ until Li is obtained2The O concentration is 203 g/L, and the hot solution is filtered;
(4) cooling the filtrate obtained in the previous step to 31 ℃, then filtering to obtain impurity-separated filter residue and impurity-separated filtrate, and washing the impurity-separated filter residue by using normal-temperature saturated sodium chloride solution; washing water obtained by washing impurity-separated filter residues returns to the size mixing working section in the step (1);
(5) heating, evaporating and concentrating the impurity-separated filtrate obtained in the previous step until the temperature is 167 ℃, and separating out 45% of solids; performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet materials;
(6) returning the obtained primary centrifugal mother liquor to the cooling working section in the step (4), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (4) to 20-40 ℃; the wet material obtained in the previous step is treated by a centrifugal separator with the volume of 1.6 mL: dissolving 1g of pure water with a liquid-solid ratio, heating, evaporating and concentrating until 49% of solids are separated out at 170 ℃, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and secondary centrifugal wet materials;
(7) and (3) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (5) until 40-50% of solids are separated out at 160-170 ℃, and drying the obtained secondary centrifugal wet material at 150-200 ℃ to obtain 1.087kg of anhydrous lithium chloride product.
Table 1: in the embodiments 1-5, the product indexes of main impurities and the national standard of anhydrous lithium chloride products, unit: is based on
As can be seen from Table 1, the anhydrous lithium chloride prepared in examples 1 to 5 has high purity, and the main impurity content of the anhydrous lithium chloride is lower than the national standard of the product and meets the national standard.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A process for producing anhydrous lithium chloride by a crystallization method is characterized by comprising the following steps: sequentially comprises the following steps:
step (1), sequentially roasting, fine-turning, acidifying, mixing and squeezing lithium-containing minerals to obtain a leaching solution containing lithium sulfate; li in the leaching solution containing lithium sulfate2The concentration of O is 15-30 g/L;
step (2), adding calcium chloride into the leaching solution containing lithium sulfate for conversion, and then squeezing and filtering to obtain a squeezed filtrate;
heating the squeezed filtrate for evaporation and concentration, then cooling and filtering to obtain impurity separation filter residues and impurity separation filtrate; heating the squeezed filtrate to evaporate and concentrate to Li2The concentration of O is 180-220 g/L, and then the mixture is cooled to 20-40 ℃;
heating, evaporating and concentrating the impurity-separated filtrate obtained in the step (3) until solid is separated out, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain primary centrifugal mother liquor and primary centrifugal wet material;
step (5), returning the primary centrifugal mother liquor obtained in the step (4) to the cooling section of the step (3), and cooling the primary centrifugal mother liquor and the concentrated squeezing filtrate in the step (3); dissolving the primary centrifugal wet material obtained in the step (4) with water, filtering, heating, evaporating and concentrating the filtrate until solid is separated out, and performing heat preservation and centrifugal separation at 150-160 ℃ to obtain secondary centrifugal mother liquor and a secondary centrifugal wet material;
and (6) returning the secondary centrifugal mother liquor to the heating evaporation concentration working section in the step (4) until solids are separated out, and drying the secondary centrifugal wet material obtained in the step (5) to obtain an anhydrous lithium chloride product.
2. The process for producing anhydrous lithium chloride by crystallization according to claim 1, wherein: in the step (2), the molar ratio of sulfate radicals to calcium is 1.05-1.1: 1, adding calcium chloride into the leaching solution containing the lithium sulfate for conversion.
3. The process for producing anhydrous lithium chloride by crystallization according to claim 1, wherein: and (3) washing the impurity-separated filter residue by using a normal-temperature saturated sodium chloride solution.
4. The process for producing anhydrous lithium chloride by crystallization according to claim 3, wherein: and (3) returning washing water obtained by washing the impurity-separated filter residue to the size mixing working section in the step (1).
5. The process for producing anhydrous lithium chloride by crystallization according to claim 1, wherein: in the step (4), the impurity-separated filtrate obtained in the step (3) is heated, evaporated and concentrated to 160-170 ℃, and solid is separated out.
6. The process for producing anhydrous lithium chloride by crystallization according to claim 1, wherein: in the step (5), the amount of the primary wet centrifugal material obtained in the step (4) is 1.5-2 mL: dissolving 1g of water with a liquid-solid ratio, filtering, heating, evaporating and concentrating the filtrate until the temperature is 160-170 ℃, and separating out solids.
7. The process for producing anhydrous lithium chloride by crystallization according to claim 1, wherein: in the step (6), heating, evaporating and concentrating until the temperature is 160-170 ℃, separating out solids, and drying at 150-200 ℃.
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| US4261960A (en) * | 1979-04-11 | 1981-04-14 | Foote Mineral Company | Removal of boron from lithium chloride brine |
| US4271131A (en) * | 1979-04-11 | 1981-06-02 | Foote Mineral Company | Production of highly pure lithium chloride from impure brines |
| CN1872688A (en) * | 2006-06-12 | 2006-12-06 | 南通大学 | Method for preparing lithium chloride free from water |
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