CN110316747B - Method for comprehensively recovering lithium and phosphorus from lithium phosphate - Google Patents
Method for comprehensively recovering lithium and phosphorus from lithium phosphate Download PDFInfo
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- CN110316747B CN110316747B CN201910676709.6A CN201910676709A CN110316747B CN 110316747 B CN110316747 B CN 110316747B CN 201910676709 A CN201910676709 A CN 201910676709A CN 110316747 B CN110316747 B CN 110316747B
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- 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
- C01B25/265—General methods for obtaining phosphates
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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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/34—Magnesium phosphates
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- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a method for comprehensively recovering lithium and phosphorus from lithium phosphate. The method provided by the invention realizes the aim of high-efficiency comprehensive recovery of phosphorus and lithium in the lithium phosphate material, the recovery rate of lithium is up to more than 98.5%, the purity of lithium carbonate is up to more than 99%, the recovery rate of phosphorus is up to more than 96%, and the purity of monohydrogen phosphate is up to more than 95%. The method has low requirement on the purity of the lithium phosphate, can realize the high-efficiency comprehensive recovery of the phosphorus and the lithium in the lithium phosphate within the range of 30-95 percent of the purity, has small limitation, has mild recovery method conditions, generates no gas in the reaction process, does not emit large amount of heat, has small pollution, low requirement on equipment, is easy to control the whole reaction, obtains the byproduct of the hydrogen phosphate, has high utilization value and low whole recovery cost, and is favorable for large-scale practical application.
Description
Technical Field
The invention relates to the technical field of recovery, in particular to a method for comprehensively recovering lithium and phosphorus from lithium phosphate.
Background
In recent years, lithium ion batteries have been widely used in the mobile electronic communication market and the power battery market for electric vehicles. With the rapid development of the lithium ion battery industry, the demand for relevant battery materials continues to increase.
When preparing electrode materials for lithium ion batteries, lithium phosphate is rarely directly used for producing positive electrode materials for lithium ion batteries due to the influence of reactivity and the like. When the wastewater generated after lithium deposition is subjected to discharge pretreatment in the production process of the lithium ion battery cathode material, soluble phosphate is usually added to remove heavy metals, alkaline earth metals and lithium in the water, so that a large amount of lithium phosphate-containing waste residues are formed, but the lithium phosphate obtained in the way cannot be directly used as a raw material or a product, cannot be purified by a simple method, and the application range of the lithium phosphate is extremely narrow, so that the research on a process for converting the lithium phosphate into other products (such as lithium carbonate and the like) has a very important significance for recycling the lithium phosphate.
CN109264748A discloses a method for preparing lithium carbonate from crude lithium phosphate, which comprises calcining lithium phosphate and a conversion agent in oxygen-isolated environment at high temperature to convert into a mixture of phosphate solid and soluble lithium salt, performing wet ball milling on the mixture to obtain phosphate solid and lithium-containing solution, removing the precipitate by adjusting the pH of the lithium-containing solution, and adding sodium carbonate to obtain lithium carbonate.
CN108928839A discloses a method for producing lithium chloride solution from lithium phosphate, which comprises adding a converting agent into the lithium phosphate as a raw material, converting the lithium phosphate under an acidic condition, neutralizing the lithium chloride with alkali, and filtering to obtain lithium chloride, but the method only describes the method for producing lithium chloride solution simply, and has no relation to the subsequent treatment of lithium chloride, and the method for producing lithium chloride solution is single and has strong limitation, and CN108928839A converts under an acidic condition with a pH of 0.5-2.0, in fact, under the condition, phosphate radicals react with acid to generate dihydrogen phosphate, dihydrogen phosphate radicals continue to react with phosphate radicals to generate monohydrogen phosphate, and though calcium monohydrogen phosphate precipitation is generated at last, the conversion of phosphorus is not complete in practice through two-step reaction, namely, the recovery utilization rate of phosphorus is reduced, and meanwhile, the method consumes a large amount of acid, is easy to corrode equipment, and has high requirements on equipment, and later maintenance is not facilitated.
Therefore, there is no method for efficiently recovering phosphorus and lithium from lithium phosphate.
Disclosure of Invention
The invention aims to provide a method for comprehensively recovering lithium and phosphorus from lithium phosphate.
The technical scheme adopted by the invention is as follows:
one of the purposes of the invention is to provide a method for comprehensively recovering lithium and phosphorus from lithium phosphate, which comprises the following steps:
1) adding water into a lithium phosphate material for pulping, adding a conversion agent, and adjusting the pH value to 2.5-5;
2) heating for reaction, and filtering to obtain a lithium solution and a monohydrogen phosphate precipitate;
3) adjusting the pH of the lithium solution to be alkaline, and removing impurities to obtain an impurity-removed lithium solution;
4) and adding carbonate to react to obtain lithium carbonate.
Preferably, the pH is adjusted to 3.0 in step 1) above.
The invention limits the pH value in the step 1) to the range, and the monobasic phosphate is generated by one-step reaction, so that the conversion rate of the conversion agent to phosphorus can be improved, namely the effective utilization rate of phosphorus is improved, the consumption of acid can be reduced, the production cost is reduced, and the equipment is basically not corroded under the acidic condition.
Preferably, the mass ratio of the water to the lithium phosphate material in the step 1) is 5-10: 1; more preferably 6: 1.
preferably, the molar ratio of the lithium phosphate material to the converting agent in step 1) is 1: 1.5 to 1.6.
Preferably, the transforming agent in step 1) is selected from at least one of calcium sulfate, magnesium sulfate, calcium chloride, magnesium chloride, barium chloride, calcium nitrate, magnesium nitrate, barium nitrate.
Preferably, the heating reaction temperature in the step 2) is 70-90 ℃.
Preferably, the heating reaction time in the step 2) is 3-5 h.
More preferably, the temperature of the heating reaction in step 2) is 80 ℃.
More preferably, the heating reaction time in step 2) is 4 h.
Preferably, the lithium phosphate material in step 1) is selected from lithium phosphate waste.
Preferably, the content of lithium phosphate in the lithium phosphate-containing waste material in the step 1) is 30-95%; more preferably 90%.
Preferably, the pH value in the step 3) is 9.0-11.0; more preferably 10 to 11.0.
Adjusting the pH value of step 3) within the above range is more favorable for removing impurities such as Ni, Ca, Mg and Co therein, so that the obtained lithium solution is purer.
Preferably, the molar ratio of the carbonate to the lithium in the lithium impurity removal solution in the step 4) is 0.55-0.75: 1; more preferably 0.6: 1.
the invention has the beneficial effects that:
1. the method provided by the invention realizes the aim of efficiently and comprehensively recovering phosphorus and lithium in the lithium phosphate material, the recovery rate of lithium is up to more than 98.5%, the purity of lithium carbonate is up to more than 99%, the recovery rate of phosphorus is up to more than 96%, and the purity of monohydrogen phosphate is up to more than 95%.
2. The method has low requirement on the purity of the lithium phosphate, can realize the high-efficiency comprehensive recovery of the phosphorus and the lithium in the lithium phosphate within the range of 30-95 percent of the purity, has small limitation, has mild recovery method conditions, generates no gas in the reaction process, does not emit large amount of heat, has small pollution, has low requirement on equipment, is easy to control the whole reaction, obtains the byproduct of the monohydrogen phosphate, has high utilization value and low whole recovery cost, and is favorable for large-scale practical application.
Detailed Description
The present invention will be described in further detail with reference to examples. It will also be understood that the following examples are included merely for purposes of further illustrating the invention and are not to be construed as limiting the scope of the invention, as the invention extends to insubstantial modifications and adaptations of the invention following in the light of the principles set forth herein. The specific process parameters and the like of the following examples are also only one example of suitable ranges, and the skilled person can make a selection within the suitable ranges through the description herein, and are not limited to the specific data of the following examples.
Example 1
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 10L of pure water into a beaker, adding 1841.3g (100 g of lithium metal phosphate) of lithium phosphate waste containing 30% of lithium phosphate while stirring, adding 800g of calcium chloride conversion agent, and adjusting the pH value of the solution to 3.5 by using hydrochloric acid;
2) heating to 80 ℃, reacting for 4h at constant temperature, and filtering to obtain 10.5L of lithium solution and 625.2g of calcium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to 10.0, removing impurities such as Ni, Co, Mn, Ca, Mg, Ba and the like, and filtering to obtain 10.0L of impurity-removed lithium solution;
4) adding 9.5L of sodium carbonate solution with the mass percent of 30% into 10.0L of the lithium removal solution, reacting for 2h, filtering, washing and drying to obtain the lithium carbonate.
Wherein, the lithium concentration of the 10.5L lithium solution obtained in the step 2) is 9.43g/L, the lithium conversion rate in the lithium phosphate is 99.01 percent, the phosphorus conversion rate is 96.54 percent, the purity of the calcium monohydrogen phosphate is 95.16 percent, and the purity of the lithium carbonate obtained in the step 4) is 99.32 percent.
Example 2
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 15L of pure water into a beaker, adding 920.6g (100 g of lithium metal phosphate) of lithium phosphate waste with the lithium phosphate content of 60% while stirring, adding 1000g of a calcium sulfate conversion agent, and adjusting the pH value of the solution to 3.0 by using sulfuric acid;
2) heating to 80 ℃, reacting for 4h at constant temperature, and filtering to obtain 16.2L of lithium solution and 636.0g of calcium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to be 10.2, removing impurities in the solution, and filtering to obtain 17.3L of impurity-removed lithium solution;
4) adding 16.5L of sodium carbonate solution with the mass percent of 30% into 17.3L of the lithium removal solution, reacting for 2h, filtering, washing and drying to obtain the lithium carbonate.
Wherein, the lithium concentration of the 17.3L lithium solution obtained in the step 2) is 5.75g/L, the lithium conversion rate in the lithium phosphate is calculated to be 99.47%, the phosphorus conversion rate is 98.22%, the purity of the calcium monohydrogen phosphate is 96.41%, and the purity of the lithium carbonate obtained in the step 4) is 99.15%.
Example 3
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 5L of pure water into a beaker, adding 690.5g (100 g) of lithium phosphate waste with the lithium phosphate content of 80 percent while stirring, then adding 1400g of calcium nitrate conversion agent, and adjusting the pH value of the solution to 2.5 by using nitric acid;
2) heating to 80 ℃, reacting for 4h at constant temperature, and filtering to obtain 5.6L of lithium solution and 622.0g of calcium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to be 10.5, removing impurities in the solution, and filtering to obtain 5.4L of impurity-removed lithium solution;
4) and adding 5.2L of 30 mass percent sodium carbonate solution into 5.4L of the lithium removal solution, reacting for 2 hours, filtering, washing and drying to obtain the lithium carbonate.
Wherein, the lithium concentration of the 5.4L lithium solution obtained in the step 2) is 18.29g/L, the lithium conversion rate in the lithium phosphate is calculated to be 98.77%, the phosphorus conversion rate is 96.13%, the purity of the calcium monohydrogen phosphate is 96.31%, and the purity of the lithium carbonate obtained in the step 4) is 99.63%.
Example 4
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 5L of pure water into a beaker, adding 690.5g (100 g) of lithium phosphate waste with the lithium phosphate content of 80 percent while stirring, adding 1750g of barium chloride conversion agent, and adjusting the pH value of the solution to 2.5 by using hydrochloric acid;
2) heating to 85 ℃, reacting for 4 hours at constant temperature, and filtering to obtain 5.5L of lithium solution and 717.8g of barium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to be 10.8, removing impurities in the solution, and filtering to obtain 5.8L of impurity-removed lithium solution;
4) and adding 5.4L of sodium carbonate solution with the mass percent of 30% into the 5.8 impurity-removed lithium solution, reacting for 2 hours, filtering, washing and drying to obtain the lithium carbonate.
Wherein the lithium concentration of the 5.8L lithium solution obtained in the step 2) was 17.05g/L, the conversion rate of lithium in lithium phosphate was calculated to be 98.89%, the conversion rate of phosphorus was calculated to be 96.47%, the purity of barium monohydrogen phosphate was calculated to be 96.0%, and the purity of lithium carbonate obtained in the step 4) was calculated to be 99.51%.
Example 5
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 8L of pure water into a beaker, adding 613.7g (100 g) of lithium phosphate waste with the lithium phosphate content of 90 percent while stirring, adding 730g of magnesium chloride conversion agent, and adjusting the pH value of the solution to 3.0 by using hydrochloric acid;
2) heating to 80 ℃, reacting for 4 hours at constant temperature, and filtering to obtain 9.2L of lithium solution and 554.28g of magnesium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to 10.8, removing impurities such as Ni, Co, Mn, Ca, Mg, Ba and the like, and filtering to obtain 9.8L of impurity-removed lithium solution;
4) adding 9.6L of sodium carbonate solution with the mass percent of 30% into 9.8L of the lithium removal solution, reacting for 2h, filtering, washing and drying to obtain the lithium carbonate.
Wherein the lithium concentration of the 9.8L lithium solution obtained in the step 2) was 10.12g/L, the conversion rate of lithium in lithium phosphate was calculated to be 99.18%, the phosphorus recovery rate was 97.02%, the purity of magnesium monohydrogen phosphate was 96.5%, and the purity of lithium carbonate obtained in the step 4) was 99.08%.
Comparative example 1
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 10L of pure water into a beaker, adding 920g of lithium phosphate waste (100 g of lithium metal phosphate) with the lithium phosphate content of 60% while stirring, then adding 850g of calcium chloride conversion agent, and adjusting the pH value of the solution to 1.5 by using hydrochloric acid;
2) heating to 80 ℃, reacting for 4h at constant temperature, and filtering to obtain 10.8L of lithium solution and 613.7g of calcium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to 10.0, removing impurities such as Ni, Co, Mn, Ca, Mg, Ba and the like, and filtering to obtain 10.5L of impurity-removed lithium solution;
4) adding 9.8L of sodium carbonate solution with the mass percent of 30% into 10.5L of the lithium removal solution, reacting for 2h, filtering, washing and drying to obtain the lithium carbonate.
Wherein, the lithium concentration of the 10.8L lithium solution obtained in the step 2) is 9.08g/L, the lithium conversion rate in the lithium phosphate is calculated to be 98.06%, the phosphorus conversion rate is calculated to be 94.75%, the purity of the calcium monohydrogen phosphate is calculated to be 94.2%, and the purity of the lithium carbonate obtained in the step 4) is calculated to be 99.0%.
Comparative example 2
A method for comprehensively recovering lithium and phosphorus from lithium phosphate comprises the following steps:
1) adding 10L of pure water into a beaker, adding 920g of lithium phosphate waste (100 g of lithium metal phosphate) with the lithium phosphate content of 60% while stirring, then adding 850g of calcium chloride conversion agent, and adjusting the pH value of the solution to 5.5 by using hydrochloric acid;
2) heating to 80 ℃, reacting for 4h at constant temperature, and filtering to obtain 11.2L of lithium solution and 600.2g of calcium monohydrogen phosphate;
3) adding a sodium carbonate solution into the lithium solution to adjust the pH value of the solution to 10.0, removing impurities such as Ni, Co, Mn, Ca, Mg, Ba and the like, and filtering to obtain 11.0L of impurity-removed lithium solution;
4) and adding 10.5L of sodium carbonate solution with the mass percent of 30% into 11.0L of the lithium removal solution, reacting for 2 hours, filtering, washing and drying to obtain the lithium carbonate.
Wherein the lithium concentration of the 11.2L lithium solution obtained in the step 2) is 8.65g/L, the lithium conversion rate in the lithium phosphate is 96.88%, the phosphorus conversion rate is 92.76%, the purity of the calcium monohydrogen phosphate is 91.16%, and the purity of the lithium carbonate obtained in the step 4) is 98.32% by calculation.
Claims (7)
1. A method for comprehensively recovering lithium and phosphorus from lithium phosphate is characterized by comprising the following steps: the method comprises the following steps:
1) adding water into a lithium phosphate material for pulping, adding a conversion agent, and adjusting the pH to be 2.5-5;
2) heating for reaction, and filtering to obtain a lithium solution and a monohydrogen phosphate precipitate;
3) adjusting the pH of the lithium solution to be alkaline, and removing impurities to obtain an impurity-removed lithium solution;
4) adding carbonate to react to obtain lithium carbonate;
the transforming agent in the step 1) is at least one selected from calcium sulfate, magnesium sulfate, calcium chloride, magnesium chloride, barium chloride, calcium nitrate, magnesium nitrate and barium nitrate;
step 1) the lithium phosphate material is selected from lithium phosphate waste;
the content of the lithium phosphate in the lithium phosphate waste material in the step 1) is 30-95%.
2. The method of claim 1, wherein: step 1) pH = 3.0.
3. The method of claim 1, wherein: the mass ratio of the water to the lithium phosphate material in the step 1) is 5-10: 1.
4. the method of claim 1, wherein: the molar ratio of the lithium phosphate material to the conversion agent in the step 1) is 1: 1.5 to 1.6.
5. The method of claim 1, wherein: the heating reaction temperature in the step 2) is 70-90 ℃; the heating reaction time in the step 2) is 3-5 h.
6. The method according to any one of claims 1 to 5, wherein: the pH value in the step 3) is 9.0-11.0.
7. The method according to any one of claims 1 to 5, wherein: the mol ratio of the carbonate to the lithium in the lithium impurity removal solution in the step 4) is 0.55-0.75: 1.
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| CN111498872B (en) * | 2020-04-14 | 2022-12-13 | 赣州虔博新材料科技有限公司 | Lithium phosphate recycling process |
| CN113830799A (en) * | 2021-09-24 | 2021-12-24 | 安顺远景新材料有限公司 | Method for preparing battery-grade lithium carbonate by using lithium phosphate and waste gypsum |
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| JP2011168461A (en) * | 2010-02-22 | 2011-09-01 | Eco-System Recycling Co Ltd | Method for producing high-concentration lithium liquid from lithium-containing liquid and method for producing lithium carbonate |
| CN106745099A (en) * | 2016-12-05 | 2017-05-31 | 天津二八科技股份有限公司 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
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| CN108862335A (en) * | 2018-07-20 | 2018-11-23 | 上海中锂实业有限公司 | A method of lithium carbonate is prepared with lithium phosphate |
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| CN109264748A (en) * | 2018-09-29 | 2019-01-25 | 广东邦普循环科技有限公司 | A method of lithium carbonate is prepared with crude lithium phosphate |
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- 2019-07-25 CN CN201910676709.6A patent/CN110316747B/en active Active
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| GB1024361A (en) * | 1962-06-20 | 1966-03-30 | Mini Richesses Nature | Lithium carbonate and by-product extraction |
| JP2011168461A (en) * | 2010-02-22 | 2011-09-01 | Eco-System Recycling Co Ltd | Method for producing high-concentration lithium liquid from lithium-containing liquid and method for producing lithium carbonate |
| CN106745099A (en) * | 2016-12-05 | 2017-05-31 | 天津二八科技股份有限公司 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
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| CN108862335A (en) * | 2018-07-20 | 2018-11-23 | 上海中锂实业有限公司 | A method of lithium carbonate is prepared with lithium phosphate |
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