CN111137868A - Preparation method of lithium phosphate - Google Patents
Preparation method of lithium phosphate Download PDFInfo
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- CN111137868A CN111137868A CN202010072597.6A CN202010072597A CN111137868A CN 111137868 A CN111137868 A CN 111137868A CN 202010072597 A CN202010072597 A CN 202010072597A CN 111137868 A CN111137868 A CN 111137868A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to the technical field of metallurgical ore separation and extraction, and particularly relates to a preparation method of lithium phosphate. The invention takes the lithium-phospho-aluminum as the raw material, solid matter with the main component of lithium phosphate is obtained by alkaline leaching and dissolution, and then the lithium phosphate is obtained by acid leaching, lithium precipitation and drying treatment. The preparation method of the lithium phosphate dissolves the lithium-phosphorus-aluminum alloy in a low-temperature alkaline leaching mode, can fully dissolve out phosphorus element and lithium element in the lithium-phosphorus-aluminum alloy, has the recovery rate of the lithium element of more than 98 percent, has the purity of the obtained lithium phosphate of more than 99 percent, can obviously reduce the production cost of the lithium phosphate, and has good application prospect.
Description
Technical Field
The invention belongs to the technical field of metallurgical ore separation and extraction, and particularly relates to a preparation method of lithium phosphate.
Background
With the development of society, new energy automobiles are continuously developed and applied due to the advantage of environmental protection, and the new energy automobiles can reduce the consumption of petroleum, prolong the service life of the petroleum and relieve the energy crisis on one hand; on the other hand, the new energy automobile is green, nontoxic and pollution-free, and the new energy automobile replaces part of fuel automobiles, so that the pollution of waste gas discharged by the fuel automobiles to the environment is greatly reduced. As a common lithium ion battery material, the lithium iron phosphate has the characteristics of long service life, large discharge capacity and the like, and the usage amount of the lithium iron phosphate in new energy automobiles is increased continuously. The lithium phosphate is used as a common raw material for preparing the lithium iron phosphate, so that the production cost is reduced, and the lithium iron phosphate can be better applied.
The existing preparation process of lithium phosphate is to prepare the lithium phosphate by taking a pure substance containing a lithium source and a phosphorus source as a raw material, so that the production cost is generally higher; although there is a process for preparing lithium phosphate by recycling waste batteries, the battery has complex components and low content of valuable elements which can be recycled in the battery, so that the problem of high difficulty in separation and purification is caused.
Disclosure of Invention
The invention aims to provide a preparation method of lithium phosphate, and aims to solve the requirement that the production cost of the existing lithium iron phosphate material needs to be reduced.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
a preparation method of lithium phosphate comprises the following steps:
crushing the lithium-phosphorus-aluminum to obtain lithium-phosphorus-aluminum powder;
mixing the lithium-phosphorus-aluminum powder with alkali for reaction, and performing solid-liquid separation to obtain a solid with a main component of lithium phosphate;
mixing and dissolving the solid with acid, and performing solid-liquid separation to obtain a lithium-containing solution;
and mixing the lithium-containing solution with alkali, and carrying out solid-liquid separation and drying to obtain the lithium phosphate.
As a preferable technical scheme of the invention, in the step of mixing and reacting the lithium-phosphorus-aluminum powder and the alkali, the mass ratio of the lithium-phosphorus-aluminum powder to the alkali is 1 (5-16).
In a preferred embodiment of the present invention, in the step of mixing and reacting the lithium-phosphorus-aluminum powder with an alkali, the alkali is at least one selected from sodium hydroxide and potassium hydroxide.
As a preferable technical scheme of the invention, in the step of mixing and reacting the lithium-phosphorus-aluminum powder and the alkali, the mass concentration of the alkali is 10-30%.
As a preferred technical scheme of the invention, in the step of mixing and reacting the lithium-phosphorus-aluminum powder and the alkali, the reaction temperature of the mixing reaction is 80-130 ℃.
As a preferable technical scheme of the invention, in the step of mixing and reacting the lithium-phosphorus-aluminum powder and the alkali, the reaction time of the mixing reaction is 1h-3 h.
In a preferred embodiment of the present invention, in the step of mixing and dissolving the solid material and the acid, the mass ratio of the solid material to the acid is 1 (2-10).
In a preferred embodiment of the present invention, in the step of mixing and dissolving the solid material and an acid, the acid is at least one selected from the group consisting of nitric acid, hydrochloric acid, sulfuric acid, and oxalic acid.
In a preferable embodiment of the present invention, in the step of mixing and dissolving the solid material and the acid, the mass concentration of the acid is 10% to 30%.
In a preferred embodiment of the present invention, in the step of mixing the lithium-containing solution with a base, the mass ratio of the lithium-containing solution to the base is (1-2): 1.
In a preferred embodiment of the present invention, in the step of mixing the lithium-containing solution with a base, the base is at least one selected from sodium hydroxide and potassium hydroxide.
As a preferable technical solution of the present invention, in the step of mixing the lithium-containing solution with the alkali, the mass concentration of the alkali is 20% to 50%.
As a preferable technical scheme of the invention, the particle size of the lithium-phosphorus-aluminum powder is 10-100 μm.
As a preferred technical scheme of the invention, the drying temperature is 100-180 ℃.
As a preferable technical scheme of the invention, the drying time is 1h-3 h.
The preparation method of the lithium phosphate dissolves the lithium-phosphorus-aluminum alloy in a low-temperature alkaline leaching mode, can fully dissolve out phosphorus element and lithium element in the lithium-phosphorus-aluminum alloy with low cost, has the recovery rate of the lithium element of more than 98 percent, ensures that the purity of the obtained lithium phosphate is more than 99 percent, can obviously reduce the production cost of the lithium phosphate, and has good application prospect. In addition, the preparation method of the lithium phosphate has the advantages of simplicity, practicability and convenience in implementation, and is suitable for large-scale industrial production.
Detailed Description
In order to make the objects, technical solutions and technical effects of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and the embodiments described below are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments obtained by a person of ordinary skill in the art without any inventive step in connection with the embodiments of the present invention shall fall within the scope of protection of the present invention. Those whose specific conditions are not specified in the examples are carried out according to conventional conditions or conditions recommended by the manufacturer; the reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be understood that the weight of the related components mentioned in the embodiments of the present invention may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, it is within the scope of the disclosure that the content of the related components is scaled up or down according to the embodiments of the present invention. Specifically, the weight described in the embodiments of the present invention may be a unit of mass known in the chemical field such as μ g, mg, g, kg, etc.
In addition, unless the context clearly uses otherwise, an expression of a word in the singular is to be understood as encompassing the plural of the word. The terms "comprises" or "comprising" are intended to specify the presence of stated features, quantities, steps, operations, elements, portions, or combinations thereof, but are not intended to preclude the presence or addition of one or more other features, quantities, steps, operations, elements, portions, or combinations thereof.
The embodiment of the invention provides a preparation method of lithium phosphate, which comprises the following steps:
s1, crushing the lithium-phosphorus-aluminum to obtain lithium-phosphorus-aluminum powder;
s2, mixing lithium-phosphorus-aluminum powder with alkali for reaction, and performing solid-liquid separation to obtain a solid with a main component of lithium phosphate;
s3, mixing the solid with acid for reaction, and carrying out solid-liquid separation to obtain a lithium-containing solution;
and S4, mixing the lithium-containing solution and alkali for reaction, and carrying out solid-liquid separation and drying to obtain the lithium phosphate.
The invention reacts with the crushed lithium-phosphorus-aluminum by low-temperature alkaline leaching to generate a mixture of lithium phosphate, phosphate and aluminate, and solid matters with the main components of lithium phosphate can be separated by solid-liquid separation by utilizing the characteristic that the lithium phosphate is difficult to dissolve in alkali liquor, so that the invention has the advantage of full dissolution of lithium element; and then, performing acid leaching, lithium precipitation and drying treatment on a solid substance with the main component of lithium phosphate, wherein the recovery rate of lithium element is more than 98%, the purity of the obtained lithium phosphate is more than 99%, and the lithium phosphate can be used as a high-quality raw material for preparing lithium iron phosphate for subsequent treatment. The raw material of the invention is the low-cost lithium phosphoaluminate, which can obviously reduce the production cost of the lithium phosphate, and the preparation method of the lithium phosphate is simple and easy to implement and convenient to implement, thereby having good application prospect.
It should be noted that, although the steps S1-S4 describe the preparation process of lithium phosphate in a specific order, it is not required that the steps be performed in the specific order, and the steps may be performed simultaneously or sequentially according to actual situations.
In S1, the reaction contact area between the lithium-phosphorus-aluminum and the alkali can be increased by pulverizing the lithium-phosphorus-aluminum, thereby increasing the mixing reaction time of the lithium-phosphorus-aluminum and the alkali and improving the dissolution rate and recovery rate of lithium. In some embodiments, the lithium phosphoaluminum powder is crushed to a particle size of 10 μm to 100 μm. Specifically, typical, but not limiting, particle sizes of the lithium-phosphorus-aluminum powder are 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm.
In S2, the lithium-phosphorus-aluminum powder is mixed with alkali to react to generate a mixture of lithium phosphate, phosphate and aluminate (shown as formula (I)). Wherein, because the lithium phosphate is difficult to dissolve in the alkali liquor, the lithium phosphate is separated from the aluminate mixed solution in a solid-liquid separation mode to obtain a solid substance with the main component of the lithium phosphate. Wherein, the alkali is mainly mixed with the lithium phosphorus aluminum powder in the form of alkali solution for reaction.
Formula (I): LiAl (F, OH) PO4+OH-→Li3PO4↓+AlO2 -+PO4 3-+AlF3↓。
In the mixing reaction of the lithium phosphorus aluminum powder and the alkali, the ratio of the lithium phosphorus aluminum powder to the alkali is optimized, so that the alkali leaching reaction rate can be accelerated, and the cost increase caused by adding excessive alkali can be avoided. In some embodiments, the mass ratio of the lithium-phosphorus-aluminum powder to the alkali is controlled to be 1 (5-16), so that the lithium-phosphorus-aluminum powder and the alkali can be quickly and completely reacted. Specifically, typical, but not limiting, mass ratios between the lithium phosphorous aluminum powder and the base are 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, 1: 16.
In the mixed reaction of the lithium-phosphorus-aluminum powder and the alkali, the alkali leaching reaction rate can be accelerated by selecting the proper alkali and the proper alkali concentration, and meanwhile, the influence of introducing redundant impurities on the subsequent treatment process is avoided. In some embodiments, sodium hydroxide and/or potassium hydroxide is selected to be mixed and reacted with the lithium-phosphorus-aluminum powder, and the mass concentration of the sodium hydroxide and/or potassium hydroxide is 10% -30%. In particular, typical, but not limiting, mass concentrations of sodium hydroxide and/or potassium hydroxide are 10%, 15%, 20%, 25%, 30%.
In the mixing reaction of the lithium-phosphorus-aluminum powder and the alkali, the alkali leaching reaction rate can be further accelerated by optimizing the mixing reaction conditions, so that the lithium element is fully dissolved out, and the recovery rate of the lithium phosphate is improved. In some embodiments, the reaction temperature of the mixing reaction is 80 ℃ to 130 ℃ and the reaction time of the mixing reaction is 1h to 3 h. Specifically, typical but not limiting reaction temperatures are 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃; typical but not limiting reaction times are 1h, 1.5h, 2h, 2.5h, 3 h.
In S3, since lithium phosphate is soluble in acid, the solid material whose main component is lithium phosphate is mixed and dissolved with acid, lithium phosphate can be dissolved in acid, and then other impurities in the solid material are removed by solid-liquid separation, and the resulting solution is a lithium-containing solution whose main component is lithium phosphate.
In the mixed dissolution of the solid with lithium phosphate as the main component and acid, the dissolution rate of lithium phosphate can be accelerated by optimizing the proportion of the solid and the acid, and the problems of pH environment deviation from the optimal reaction environment, cost increase and the like caused by adding excessive acid are avoided. In some embodiments, the mass ratio of the solid with lithium phosphate as the main component to the acid is controlled to be 1 (2-10), so that the lithium phosphate is rapidly and fully dissolved. Specifically, typical, but not limiting, mass ratios between the solid of lithium phosphate as the main ingredient and the acid are 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1: 10.
During the mixed dissolution of the solid with lithium phosphate as the main component and acid, the dissolution rate can be accelerated by selecting proper acid and proper acid concentration, and the influence of introducing redundant impurities on the subsequent treatment process is avoided. In some embodiments, the acid is selected from at least one of nitric acid, hydrochloric acid, sulfuric acid, and oxalic acid, and the mass concentration of the acid is 10% -30%. In particular, typical, but not limiting, acid concentrations are 10%, 15%, 20%, 25%, 30% by mass.
Since the main component of the lithium-containing solution is lithium phosphate, and the lithium phosphate has the characteristic of being insoluble in alkali, in S4, the lithium-containing solution is mixed with alkali and then subjected to solid-liquid separation, so that the lithium phosphate can be separated in the form of precipitate, and then subjected to drying treatment to obtain the lithium phosphate product.
In the mixing of the lithium-containing solution and the alkali, the dissolution rate of lithium phosphate can be accelerated by optimizing the proportion of the lithium-containing solution and the alkali, and the problems of cost increase, deviation from the optimal pH value of the reaction and the like caused by adding excessive alkali are avoided. In some embodiments, the mass ratio of the lithium-containing solution to the base is controlled to be (1-2): 1. In particular, typical, but not limiting, mass ratios between the lithium-containing solution and the base are 1:1, 1.2:1, 1.4:1, 1.5:1, 1.6:1, 1.8:1, 2: 1.
In the mixing of the lithium-containing solution and the alkali, the precipitation rate of the lithium phosphate can be accelerated by selecting the proper alkali and the proper alkali concentration, and meanwhile, the influence of introducing redundant impurities on the subsequent treatment process is avoided. In some embodiments, sodium hydroxide and/or potassium hydroxide is selected to be mixed with the lithium-containing solution, and the mass concentration of the sodium hydroxide and/or potassium hydroxide is 20-50%. In particular, typical, but not limiting, mass concentrations of sodium hydroxide and/or potassium hydroxide are 20%, 25%, 30%, 35%, 40%, 45%, 50%.
In the mixing of the lithium-containing solution and the alkali, the precipitation rate of the lithium phosphate can be further accelerated by optimizing the mixing conditions, so that the lithium element is fully precipitated, and the recovery rate of the lithium phosphate is improved. In some embodiments, the temperature of mixing is 60 ℃ to 90 ℃ and the time of mixing is 2h to 5 h. Specifically, typical but non-limiting mixing temperatures are 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃; typical, but not limiting, mixing times are 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5 h.
In the process of drying the precipitated lithium phosphate, the drying efficiency can be accelerated and the production time and cost can be saved by optimizing the drying temperature and the drying time. In some embodiments, the temperature of drying is from 100 ℃ to 180 ℃; the drying time is 1h-3 h. Specifically, typical but not limiting drying temperature is 100 ℃, 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃; typical but not limiting drying times are 1h, 1.5h, 2h, 2.5h, 3 h.
In the embodiment of the present invention, solid-liquid separation may be performed by at least one of filtration, centrifugation, evaporation, sedimentation, and the like, and the corresponding operation method is a method commonly used in the art and will not be described herein again.
In order to make the above implementation details and operations of the present invention clearly understood by those skilled in the art and to make the progress of the preparation method of lithium phosphate according to the embodiment of the present invention obvious, the above technical solution is illustrated by a plurality of examples below. The results of measuring the dawsonite component used in each example are shown in table 1.
TABLE 1 measurement results of the components of the Lifoenite
| Burn out reduction (1025 ℃ C.) | 7.11(％) | PbO | 58.05(mg/kg) |
| Al2O3 | 32.49(％) | ZnO | 311.18(mg/kg) |
| SiO2 | 9.20(％) | CdO | 6.33(mg/kg) |
| Fe2O3 | 0.12(％) | SrO | 331.36(mg/kg) |
| P2O5 | 41.51(％) | MnO | 229.73(mg/kg) |
| S | 0.78(％) | Cr2O3 | 3.05(mg/kg) |
| F | ＜0.01(％) | NiO | 5.04mg/kg) |
| Li2O | 7.66(％) | CoO | 2.05(mg/kg) |
| Na2O | 0.30(％) | CuO | 49.20(mg/kg) |
| CaO | 0.38(％) | MgO | 292.25(mg/kg) |
| K2O | 0.37(％) | Rb2O | 17.27(mg/kg) |
| TiO2 | 639.51(mg/kg) | Cs2O | 389.44(mg/kg) |
| BaO | 138.46(mg/kg) | BeO | 76.39(mg/kg) |
Example 1
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to obtain lithium-phosphorus-aluminum powder with the particle size of 60 mu m;
(2) taking 100g of lithium-phosphorus-aluminum powder, adding 550mL of 23% sodium hydroxide solution at 90 ℃, heating and reacting for 1.2h, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid substance with a main component of lithium phosphate;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 140mL of 15% sulfuric acid into the filter residue B, stirring and dissolving for 40min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 50mL of sodium hydroxide solution with the mass concentration of 40% into the lithium-containing solution, precipitating lithium at 60 ℃ for 2h, filtering, washing, and drying at 150 ℃ for 2h to obtain a lithium phosphate product.
Example 2
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to obtain lithium-phosphorus-aluminum powder with the particle size of 50 mu m;
(2) taking 120g of lithium-phosphorus-aluminum powder, adding 800mL of 15% sodium hydroxide solution at 100 ℃, heating for reaction for 3h, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid containing lithium phosphate as a main component;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 160mL of sulfuric acid with the mass concentration of 20% into the filter residue B, stirring and dissolving for 35min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 60mL of 30% sodium hydroxide solution into the lithium-containing solution, precipitating lithium at 80 ℃ for reaction for 5h, filtering, washing, and drying at 120 ℃ for 3h to obtain a lithium phosphate product.
Example 3
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to obtain lithium-phosphorus-aluminum powder with the particle size of 30 mu m;
(2) taking 70g of lithium-phosphorus-aluminum powder, adding 500mL of 20% sodium hydroxide solution at 130 ℃, heating and reacting for 1h, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid substance with the main component of lithium phosphate;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 120mL of sulfuric acid with the mass concentration of 30% into the filter residue B, stirring and dissolving for 30min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 70mL of 35% sodium hydroxide solution into the lithium-containing solution, precipitating lithium at 65 ℃ for reaction for 3h, filtering, washing, and drying at 100 ℃ for 2.5h to obtain a lithium phosphate product.
Example 4
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to obtain lithium-phosphorus-aluminum powder with the particle size of 10 mu m;
(2) taking 50g of lithium-phosphorus-aluminum powder, adding 750mL of 10% sodium hydroxide solution at the mass concentration, heating and reacting for 1.8h at 110 ℃, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid substance with the main component of lithium phosphate;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 200mL of sulfuric acid with the mass concentration of 15% into the filter residue B, stirring and dissolving for 50min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 90mL of 25% sodium hydroxide solution into the lithium-containing solution, precipitating lithium at 70 ℃ for reaction for 4h, filtering, washing, and drying at 160 ℃ for 1.5h to obtain a lithium phosphate product.
Example 5
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to obtain lithium-phosphorus-aluminum powder with the particle size of 100 mu m;
(2) taking 150g of lithium-phosphorus-aluminum powder, adding 650mL of 30% sodium hydroxide solution at 80 ℃, heating and reacting for 2.2h, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid substance with a main component of lithium phosphate;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 180mL of sulfuric acid with the mass concentration of 10% into the filter residue B, stirring and dissolving for 60min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 80mL of sodium hydroxide solution with the mass concentration of 20% into the lithium-containing solution, precipitating lithium at 90 ℃ for reaction for 2.5h, filtering, washing, and drying at 180 ℃ for 1h to obtain a lithium phosphate product.
Example 6
A preparation method of lithium phosphate comprises the following steps:
(1) crushing the lithium-phosphorus-aluminum powder to 70 mu m;
(2) taking 140g of lithium-phosphorus-aluminum powder, adding 600mL of 28% sodium hydroxide solution at 120 ℃, heating and reacting for 1.8h, and filtering to obtain filter residue A and filtrate A, wherein the obtained filter residue A is a solid containing lithium phosphate as a main component;
(3) washing the filter residue A with water for 3 times, and filtering to obtain filter residue B and filtrate B. Adding 100mL of 25% sulfuric acid into the filter residue B, stirring and dissolving for 45min at room temperature, and filtering to obtain a lithium-containing solution;
(4) adding 100mL of 50% sodium hydroxide solution into the lithium-containing solution, precipitating lithium at 80 ℃ for reaction for 3.5h, filtering, washing, and drying at 170 ℃ for 2h to obtain a lithium phosphate product.
The recovery rates of lithium elements and the purity of lithium phosphate products obtained in examples 1 to 6 are shown in Table 2.
TABLE 2 recovery of lithium element and purity results for lithium phosphate product
| Examples | Recovery rate of lithium element | Purity of lithium phosphate |
| Example 1 | 98.86 | 99.17 |
| Example 2 | 98.74 | 99.31 |
| Example 3 | 98.13 | 99.26 |
| Example 4 | 98.36 | 99.56 |
| Example 5 | 98.54 | 99.41 |
| Example 6 | 98.92 | 99.64 |
As can be seen from Table 2, the lithium phosphate product prepared by using the lithium-phosphorus-aluminum as the raw material has the advantages of high recovery rate of lithium element and high purity of the obtained lithium phosphate, and can be used as the raw material for preparing lithium iron phosphate with excellent performance.
Claims (10)
1. A preparation method of lithium phosphate is characterized by comprising the following steps:
crushing the lithium-phosphorus-aluminum to obtain lithium-phosphorus-aluminum powder;
mixing the lithium-phosphorus-aluminum powder with alkali for reaction, and performing solid-liquid separation to obtain a solid with a main component of lithium phosphate;
mixing and dissolving the solid with acid, and performing solid-liquid separation to obtain a lithium-containing solution;
and mixing the lithium-containing solution with alkali, and carrying out solid-liquid separation and drying to obtain the lithium phosphate.
2. The method for preparing lithium phosphate according to claim 1, wherein in the step of mixing and reacting the lithium-phosphorus-aluminum powder with the alkali, the mass ratio of the lithium-phosphorus-aluminum powder to the alkali is 1 (5-16).
3. The method for preparing lithium phosphate according to claim 1, wherein in the step of mixing and reacting the lithium-phosphorus-aluminum powder with a base, the base is at least one selected from sodium hydroxide and potassium hydroxide; and/or
The mass concentration of the alkali is 10-30%.
4. The method for preparing lithium phosphate according to claim 1, wherein in the step of mixing lithium-phosphorus-aluminum powder with alkali for reaction, the reaction temperature of the mixing reaction is 80 ℃ to 130 ℃; and/or
The reaction time of the mixing reaction is 1h-3 h.
5. The method for producing lithium phosphate according to claim 1, wherein in the step of mixing and dissolving the solid material and the acid, the mass ratio of the solid material to the acid is 1 (2-10).
6. The method for producing lithium phosphate according to claim 1, wherein in the step of mixing and dissolving the solid with an acid, the acid is at least one selected from nitric acid, hydrochloric acid, sulfuric acid, and oxalic acid; and/or
The mass concentration of the acid is 10-30%.
7. The method for producing lithium phosphate according to claim 1, wherein in the step of mixing the lithium-containing solution with a base, the mass ratio of the lithium-containing solution to the base is (1-2): 1.
8. The method for preparing lithium phosphate according to claim 1, wherein in the step of mixing the lithium-containing solution with a base, the base is at least one selected from the group consisting of sodium hydroxide and potassium hydroxide; and/or
The mass concentration of the alkali is 20-50%.
9. The method for producing lithium phosphate according to any one of claims 1 to 8, wherein the particle size of the lithium-phosphorus-aluminum powder is 10 μm to 100 μm.
10. The method for preparing lithium phosphate according to any one of claims 1 to 8, wherein the drying temperature is 100 ℃ to 180 ℃; and/or
The drying time is 1h-3 h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2024026A (en) * | 1933-11-17 | 1935-12-10 | Warner Chemical Company | Recovering lithium compounds |
| CN108910851A (en) * | 2018-09-21 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of lithium-containing compound is prepared by amblygonite |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2024026A (en) * | 1933-11-17 | 1935-12-10 | Warner Chemical Company | Recovering lithium compounds |
| CN108910851A (en) * | 2018-09-21 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of lithium-containing compound is prepared by amblygonite |
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Application publication date: 20200512 |