CN102351160A - Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution - Google Patents
Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution Download PDFInfo
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Abstract
The invention relates to a method for preparing battery grade lithium dihydrogen phosphate with a high-purity lithium carbonate lithium depositing mother solution. The method comprises the steps of: conducting preliminary lithium extraction and deep lithium extraction to a lithium carbonate lithium depositing mother solution with phosphoric acid and phosphate so as to obtain a mixture of lithium phosphate and dilithium hydrogen phosphate, reacting the mixture with phosphoric acid to generate a lithium dihydrogen phosphate solution, then carrying out concentration and evaporation, cooling and crystallization, centrifugation, saturation washing, drying, air-stream crushing and packaging, thus obtaining the battery grade lithium dihydrogen phosphate. The method of preparing battery grade lithium dihydrogen phosphate in the invention fully makes use of the mother solution generated during high-purity lithium carbonate production, and has the advantages of simple process, easy operation, low production cost, over 90% of lithium recovery rate, and stable quality of the obtained battery grade lithium dihydrogen phosphate product, and is also suitable for preparing the lithium ion battery positive material lithium iron phosphate. Therefore, the method provided in the invention boasts broad market prospects, as well as good economic and social benefits.
Description
Technical field
The invention belongs to field of inorganic materials, relate to a kind of method of utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate.
Background technology
In recent years, the compound of lithium and lithium obtains application more and more widely in national life, has widespread use such as lithium-ion secondary cell at aspects such as laptop computer, mobile communication, power tools.At present, the positive electrode material that lithium cell is commonly used has the sour lithium of cobalt, lithium nickel cobalt dioxide, nickle cobalt lithium manganate, lithium manganate etc., but their total shortcomings are that safety performance is relatively poor, and production cost is high, and because cobalt resource is limited, its price has the trend that continues raising.As the iron lithium phosphate of novel anode material for lithium-ion batteries, more and more receive people's concern and attention.LiFePO 4 (LiFePO
4) as the positive electrode material of battery, not only have advantages such as good security, the feature of environmental protection, and cost is lower, has good market outlook.
One of main raw material of producing iron lithium phosphate is a monometallic.And the raw materials for production of the battery-grade lithium dihydrogen phosphate on the market are Quilonum Retard, lithium hydroxide and Trilithium phosphate, and these several cost of material are more expensive.
Lithium is a scarce resource, and the compound of lithium and lithium but is widely used by growing field, how to utilize lithium resource fully, and also taking into account energy-saving and cost-reducing simultaneously is enterprise and social questions of common interest.
In the traditional mode of production Quilonum Retard process, contain lithium in the mother liquor, and work as sewage disposal, cause the lithium loss more like this.So produce in the Quilonum Retard process, solving sinker mother liquor problem is one of key of Technology.
And mother liquor to handle traditional method be with hydrogen fluoride the sinker mother liquor to be carried lithium to prepare lithium fluoride, putting forward the lithium rate has only about 70%, carries also containing a large amount of fluorions in the mother liquor behind the lithium, poses a big pressure to environmental treatment.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate, preparing method's cost of this monometallic is low, features simple and practical process, facility investment is few and more environmental protection.
The present invention utilizes pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate; Through tentatively carry lithium, the degree of depth is carried lithium; Add phosphoric acid again and generate monometallic solution, process concentration and evaporation, crystallisation by cooling, centrifugation, saturated washing and oven dry; The product particle that obtains is thin and even; Color is bright in vain, is suitable for preparing the monometallic product of lithium ion anode material.
The technical scheme that technical solution problem of the present invention is adopted is:
Utilize pure Lithium Carbonate sinker mother liquor to prepare the method for battery-grade lithium dihydrogen phosphate, mainly comprise following processing step:
(a) tentatively carry lithium: in reactive tank, add the pure Lithium Carbonate mother liquor, drip an amount of phosphoric acid solution they are fully reacted, the pH value that control drips phosphoric acid afterreaction liquid is 5～7; The concentration of said pure Lithium Carbonate mother liquor is at least 99.9%;
(b) degree of depth is carried lithium: after the reaction solution in the step (a) is fully stirred, slowly drip Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution again, controlling its reacted pH value is 7～10, fully stirs, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries;
(c) separate: separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries;
(d) washing: Trilithium phosphate after will separating and the two lithium mixture water washings of phosphoric acid hydrogen;
(e) Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that utilize (d) to obtain prepare battery-grade lithium dihydrogen phosphate.
Said step (e) mainly comprises following processing step:
(e 1) adds a spot of pure water to Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that step (d) obtains, and after fully stirring, adds an amount of phosphoric acid, and the pH value of regulating mixed solution is 1.5～2;
(e2) settled solution that step (e1) is obtained concentrates, and is heated to about 130 ℃, and temperature error when having waited crystal to separate out, makes it be cooled to 30～40 ℃ at ± 10 ℃;
(e3) the monometallic de-watering of slurries that step (e2) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, saturated drip washing at least 2 times;
(e4) the monometallic oven dry that step (e3) is obtained, temperature is controlled at 80～120 ℃, obtains battery-grade lithium dihydrogen phosphate.
The method of utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate provided by the invention can also comprise following processing step:
(f) pulverize: the battery-grade lithium dihydrogen phosphate that obtains in (e) step is ground into D
50The product of＜10 μ m.
Preferably, the temperature of reaction of pure Lithium Carbonate mother liquor and an amount of phosphoric acid solution is controlled at 60～100 ℃ in the said step (a).
Phosphoric acid concentration in the said step (a) is 40～85%, and the phosphate dihydrogen sodium concentration in the said step (b) is 10～50%, and sodium phosphate concentration is 10～50%.Preferably, said phosphoric acid concentration is 85%, and said phosphate dihydrogen sodium concentration is 20%, and said sodium phosphate concentration is 20%.
Preferably, the temperature of bath water is 60～90 ℃ in the said step (d).
Preferably; The dewatering of monometallic is in the said step (e2): monometallic is put into the whizzer centrifuge dehydration, when water outlet place flowing water is not the streamline shape, add the washing of monometallic saturated solution again; The recentrifuge dehydration, saturated repeatedly drip washing 2～6 times.
Preferably, the dropping time of phosphoric acid solution was controlled at 30～120 minutes in the said step (a), and the dropping time that drips Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution in the said step (b) was controlled at 30～120 minutes.
Preferably, battery-grade lithium dihydrogen phosphate becomes D through comminution by gas stream in the said step (f)
50The product of＜10 μ m.
The present invention compared with prior art has following advantage:
The present invention utilizes preparation pure Lithium Carbonate mother liquor; And carry lithium with the Sodium phosphate dibasic degree of depth after adopting phosphoric acid tentatively to carry lithium; Obtain intermediates Trilithium phosphate and phosphoric acid hydrogen two lithium mixtures; Add an amount of phosphoric acid production again and go out battery-grade lithium dihydrogen phosphate; This method technology is simple; Processing ease; Production cost is low; The iron lithium phosphate that products obtained therefrom battery-grade lithium dihydrogen phosphate steady quality, purity be high, can be used to synthesis of anode material of lithium-ion battery; Has vast market prospect, better economic and social benefit.
This processing method is with phosphoric acid and the sinker mother liquor is tentatively carried lithium to phosphoric acid salt and the degree of depth is carried lithium; Putting forward the lithium rate can reach more than 90%; Obtain Trilithium phosphate and phosphoric acid hydrogen two lithium mixtures, utilize this mixture to prepare the high value added product monometallic again, also can solve mother liquor fluoride pollution problem.
Description of drawings
Fig. 1 is according to the process flow sheet that utilizes pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate of the present invention.
Embodiment
Utilize pure Lithium Carbonate sinker mother liquor to prepare the method for battery-grade lithium dihydrogen phosphate, mainly comprise following processing step:
(a) tentatively carry lithium: in reactive tank, add the pure Lithium Carbonate mother liquor, drip an amount of phosphoric acid they are fully reacted, the pH value that control drips phosphoric acid afterreaction liquid is 5～7; The concentration of said pure Lithium Carbonate mother liquor is at least 99.9%.
Preferably, in reactive tank, add the pure Lithium Carbonate mother liquor, be heated 60～100 ℃, begin to drip phosphoric acid, the dropping time was controlled at 30～120 minutes, and control drips pH=6～7 of phosphoric acid, reaches and tentatively puies forward the lithium purpose.
The temperature of reaction of pure Lithium Carbonate mother liquor and an amount of phosphoric acid solution is controlled at 60～100 ℃, is in order to obtain the high lithium rate of putting forward.
(b) degree of depth is carried lithium: after the reaction solution in the step (a) is fully stirred, slowly drip Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution again, controlling its reacted pH value is 7～10, fully stirs, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries.
Preferably, after reaction solution in the step (a) fully stirred, slowly drip Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution again; Control its reacted pH=7～9, fully stir, and insulation 2h; Obtain Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries, can reach the degree of depth like this and carry lithium more than 90%.The concentration of SODIUM PHOSPHATE, MONOBASIC is preferably 20%, and the concentration of sodium phosphate is preferably 20%.
(c) separate: separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries while hot.
(d) washing: Trilithium phosphate after will separating and the two lithium mixture water washings of phosphoric acid hydrogen.
The temperature of bath water is preferably 60～90 ℃.
(e) Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that utilize (d) to obtain prepare battery-grade lithium dihydrogen phosphate.
Step (e) can be utilized prior art for preparing, preferably adopts following processing step:
(e1) Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that obtain to step (d) add a spot of water (being preferably pure water), after fully stirring, add an amount of phosphoric acid, and the pH value of regulating mixed solution is 1.5～2.
(e2) settled solution that step (e1) is obtained concentrates, and is heated to about 130 ℃, and temperature error when having waited crystal to separate out, makes it be cooled to 30～40 ℃ at ± 10 ℃.
(e3) the monometallic de-watering of slurries that step (e2) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, saturated drip washing at least 2 times.
The dewatering of monometallic: monometallic is put into the whizzer centrifuge dehydration, when water outlet place flowing water is not the streamline shape, add the washing of monometallic saturated solution again, recentrifuge dehydration, saturated repeatedly drip washing 2～6 times.
(e4) the monometallic oven dry that step (e3) is obtained, temperature is controlled at 80～120 ℃, and the time is 1～2h, obtains battery-grade lithium dihydrogen phosphate.
(f) pulverize: the battery-grade lithium dihydrogen phosphate that obtains in the step (e) is ground into D
50The product of＜10 μ m.
Step (f) is follow-up pulverising step, and for example battery-grade lithium dihydrogen phosphate becomes D through comminution by gas stream
50The product of＜10 μ m.
Embodiment 1:
(a) the pure Lithium Carbonate mother liquor 500L of adding 99.9% puts into reaction kettle in reactive tank, is heated 90 ± 5 ℃, begins to drip 85% phosphoric acid solution, controls its reacted pH=5, is tentatively carried the lithium product;
(b) with after reaction solution fully stirs in (a) step, slowly drip disodium phosphate soln again, temperature is controlled at 80～85 ℃, fully stirs, and endpoint pH is controlled to be pH=7, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries after being incubated 1 hour;
(c) separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries while hot, put forward lithium rate 90%;
(d) Trilithium phosphate and the two lithium mixture hot washes of phosphoric acid hydrogen after will separating;
(e) after Trilithium phosphate that (d) obtained and phosphoric acid hydrogen two lithium mixtures add a spot of pure water and fully stir, add the pH to 1.5 that phosphoric acid is regulated mixed solution;
(f) settled solution in (e) step is concentrated, be heated to 130 ℃, when having waited crystal to separate out, feed water coolant and make it be cooled to 30 ℃;
(g) the monometallic de-watering of slurries that step (f) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, saturated repeatedly drip washing 3 times.
(h) the monometallic oven dry that obtains in (g) step is handled, temperature is controlled at 120 ℃, and the time is 2h, obtains battery-grade lithium dihydrogen phosphate.
(i) battery-grade lithium dihydrogen phosphate that obtains in (h) step is passed through comminution by gas stream to D
50The product of＜10 μ m, and the product that obtains packed.
Embodiment 2:
(a) in reactive tank, add 99.9% pure Lithium Carbonate mother liquor 500L and put into reaction kettle, be heated 90 ± 5 ℃, begin to drip 60% phosphoric acid solution, control its reacted pH=6, tentatively carried the lithium product;
(b) with after reaction solution fully stirs in (a) step, slowly drip disodium phosphate soln again, temperature is controlled at 80～85 ℃, fully stirs, and endpoint pH is controlled to be pH=9, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries behind the insulation 1h;
(c) separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries while hot, put forward lithium rate 92%;
(d) Trilithium phosphate and the two lithium mixture hot washes of phosphoric acid hydrogen after will separating;
(e) after Trilithium phosphate that (d) obtained and phosphoric acid hydrogen two lithium mixtures add a spot of pure water and fully stir, add the pH to 1.6 that phosphoric acid is regulated mixed solution;
(f) settled solution in (e) step is concentrated, be heated to 130 ℃, when having waited crystal to separate out, feed water coolant and make it be cooled to 40 ℃;
(g) the monometallic de-watering of slurries that step (f) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, saturated repeatedly drip washing 5 times.
(h) the monometallic oven dry that obtains in (g) step is handled, temperature is controlled at 100 ℃, and the time is 2h, obtains battery-grade lithium dihydrogen phosphate.
(i) battery-grade lithium dihydrogen phosphate that obtains in (h) step is passed through comminution by gas stream to D
50The product of＜10 μ m, and the product that obtains packed.
Embodiment 3:
(a) the pure Lithium Carbonate mother liquor 500L of adding 99.9% puts into reaction kettle in reactive tank, is heated 90 ± 5 ℃, begins to drip 40% phosphoric acid solution, controls its reacted pH=7, is tentatively carried the lithium product;
(b) with after reaction solution fully stirs in (a) step, slowly drip disodium phosphate soln again, temperature is controlled at 80～85 ℃, fully stirs, and endpoint pH is controlled to be pH=10, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries behind the insulation 1h;
(c) separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries while hot, put forward lithium rate 91%;
(d) Trilithium phosphate and the two lithium mixture hot washes of phosphoric acid hydrogen after will separating;
(e) after Trilithium phosphate that (d) obtained and phosphoric acid hydrogen two lithium mixtures add a spot of pure water and fully stir, add the pH to 1.8 that phosphoric acid is regulated mixed solution;
(f) settled solution in (e) step is concentrated, be heated to 130 ℃, when having waited crystal to separate out, feed water coolant and make it be cooled to 40 ℃;
(g) the monometallic de-watering of slurries that step (f) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, drip washing is 6 times repeatedly.
(h) the monometallic oven dry that obtains in (g) step is handled, temperature is controlled at 90 ℃, and the time is 2h, obtains battery-grade lithium dihydrogen phosphate.
(i) battery-grade lithium dihydrogen phosphate that obtains in (h) step is passed through comminution by gas stream to D
50The product of＜10 μ m, and the product that obtains packed.
The monometallic technical target of the product is following in the foregoing description:
Table 1 monometallic technical target of the product
By the foregoing description and product composition analytical results can find out that the method for preparing battery-grade lithium dihydrogen phosphate of the present invention is simple, processing ease, production cost be low; Products obtained therefrom battery-grade lithium dihydrogen phosphate steady quality can be used for preparing lithium cell anode material of lithium iron phosphate.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction, every foundation technical spirit of the present invention all still belongs to the protection domain of technical scheme of the present invention to any simple modification, equivalent variations and modification that above embodiment did.
Claims (10)
1. utilize pure Lithium Carbonate sinker mother liquor to prepare the method for battery-grade lithium dihydrogen phosphate, it is characterized in that, mainly comprise following processing step:
(a) tentatively carry lithium: in reactive tank, add the pure Lithium Carbonate mother liquor, drip an amount of phosphoric acid solution they are fully reacted, the pH value that control drips phosphoric acid afterreaction liquid is 5～7; The concentration of said pure Lithium Carbonate mother liquor is at least 99.9%;
(b) degree of depth is carried lithium: after the reaction solution in the step (a) is fully stirred, slowly drip Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution again, controlling its reacted pH value is 7～10, fully stirs, and obtains Trilithium phosphate and phosphoric acid hydrogen two lithium mixed slurries;
(c) separate: separate lithium salts and mother liquor in Trilithium phosphate and the phosphoric acid hydrogen two lithium mixed slurries;
(d) washing: Trilithium phosphate after will separating and the two lithium mixture water washings of phosphoric acid hydrogen;
(e) Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that utilize (d) to obtain prepare battery-grade lithium dihydrogen phosphate.
2. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1 is characterized in that, said step (e) mainly comprises following processing step:
(e1) Trilithium phosphate and the phosphoric acid hydrogen two lithium mixtures that obtain to step (d) add a spot of pure water, after fully stirring, add an amount of phosphoric acid, and the pH value of regulating mixed solution is 1.5～2;
(e2) settled solution that step (e1) is obtained concentrates, and is heated to about 130 ℃, and temperature error when having waited crystal to separate out, makes it be cooled to 30～40 ℃ at ± 10 ℃;
(e3) the monometallic de-watering of slurries that step (e2) is obtained obtains the thick product of monometallic, again with the washing of monometallic saturated solution, and dehydration once more, saturated drip washing at least 2 times;
(e4) the monometallic oven dry that step (e3) is obtained, temperature is controlled at 80～120 ℃, obtains battery-grade lithium dihydrogen phosphate.
3. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1 is characterized in that, also comprises following processing step:
(f) pulverize: the battery-grade lithium dihydrogen phosphate that obtains in (e) step is ground into D
50The product of＜10 μ m.
4. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1 is characterized in that: the pure Lithium Carbonate mother liquor is controlled at 60～100 ℃ with the temperature of reaction of an amount of phosphoric acid solution in the said step (a).
5. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1; It is characterized in that: the phosphoric acid concentration in the said step (a) is 40～85%; Phosphate dihydrogen sodium concentration in the said step (b) is 10～50%, and sodium phosphate concentration is 10～50%.
6. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 5; It is characterized in that: the phosphoric acid concentration in the said step (a) is 85%; Phosphate dihydrogen sodium concentration in the said step (b) is 20%, and sodium phosphate concentration is 20%.
7. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1 is characterized in that: the temperature of bath water is 60～90 ℃ in the said step (d).
8. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 2; It is characterized in that; The dewatering of monometallic is in the said step (e2): monometallic is put into the whizzer centrifuge dehydration; When water outlet place flowing water is not the streamline shape; Add the washing of monometallic saturated solution again; The recentrifuge dehydration, saturated repeatedly drip washing 2～6 times.
9. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 1; It is characterized in that: the dropping time of phosphoric acid solution was controlled at 30～120 minutes in the said step (a), and the dropping time that drips Sodium phosphate dibasic or sodium radio-phosphate,P-32 solution in the said step (b) was controlled at 30～120 minutes.
10. the method for utilizing pure Lithium Carbonate sinker mother liquor to prepare battery-grade lithium dihydrogen phosphate according to claim 3 is characterized in that: battery-grade lithium dihydrogen phosphate becomes D through comminution by gas stream in the said step (f)
50The product of＜10 μ m.
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| CN104925837A (en) * | 2015-03-18 | 2015-09-23 | 江西赣锋锂业股份有限公司 | Method of preparing lithium salt by recovering lithium deposition mother liquor of battery grade lithium carbonate |
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| CN114132907A (en) * | 2021-11-05 | 2022-03-04 | 安徽大学绿色产业创新研究院 | Method for recovering lithium from lithium precipitation mother liquor of high-purity lithium carbonate |
| CN115744850A (en) * | 2022-12-15 | 2023-03-07 | 昆明川金诺化工股份有限公司 | Preparation method of high-quality lithium dihydrogen phosphate |
| CN115744850B (en) * | 2022-12-15 | 2024-02-02 | 昆明川金诺化工股份有限公司 | Preparation method of high-quality lithium dihydrogen phosphate |
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