CN110316747A - A method of synthetical recovery lithium and phosphorus from lithium phosphate - Google Patents
A method of synthetical recovery lithium and phosphorus from lithium phosphate Download PDFInfo
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- CN110316747A CN110316747A CN201910676709.6A CN201910676709A CN110316747A CN 110316747 A CN110316747 A CN 110316747A CN 201910676709 A CN201910676709 A CN 201910676709A CN 110316747 A CN110316747 A CN 110316747A
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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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- C—CHEMISTRY; METALLURGY
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- 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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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/08—Carbonates; Bicarbonates
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Abstract
The method of the invention discloses a kind of from lithium phosphate synthetical recovery lithium and phosphorus.The method of the invention realizes the targets of the efficient synthetical recovery to phosphorus and lithium in phosphoric acid lithium material, 98.5% or more is up to for the rate of recovery of lithium, the purity of lithium carbonate is up to 99% or more, while to the rate of recovery of phosphorus up to 96% or more, the purity of dibasic alkaliine is up to 95% or more.Method of the invention is lower to the purity requirement of lithium phosphate, it may be implemented in the efficient synthetical recovery in the range of lithium phosphate purity is 30%~95% to phosphorus therein and lithium, and limitation is small, recovery method mild condition of the invention simultaneously, it is generated in reaction process without gas, big calorimetric will not be released, it thus pollutes small, it is low for equipment requirements, entirely react easily controllable, and obtained by-product is hydrophosphate, utility value is high, entire cost recovery is low, is conducive to carry out large-scale practical application.
Description
Technical field
The present invention relates to recovery technology field more particularly to a kind of methods of synthetical recovery lithium and phosphorus from lithium phosphate.
Background technique
In recent years, lithium ion battery was widely used in mobile electronic communication market and Prospect of EVS Powered with Batteries city
?.Demand sustainable growth along with the rapid development of lithium ion battery industry, to associated batteries material.
When preparing electrode material used in lithium ion battery, because being influenced by reactivity etc., lithium phosphate is seldom direct
For producing anode material for lithium-ion batteries.And in anode material for lithium-ion batteries production process to sinker after the waste water that generates
When carrying out discharge pre-treatment, heavy metal, alkaline-earth metal and the lithium for being usually added into soluble phosphate to go in water removal, thus formed
The waste residue of a large amount of phosphoric acid lithiums, but the lithium phosphate obtained in this way can not be used directly as raw material or product, can not be passed through
Simple method is purified, and along with the use scope of lithium phosphate is extremely narrow, therefore research converts it to the work of other products
Skill (such as: lithium carbonate etc.), the recycling and reusing of lithium phosphate is had a very important significance.
CN109264748A discloses a kind of method for preparing lithium carbonate with crude lithium phosphate, by lithium phosphate and transforming agent
Starvation high temperature calcining be converted to phosphate solid and soluble lithium salt mixture, after by mixture carry out wet process ball
Mill, obtains phosphate solid and lithium-containing solution, by adjusting the pH of lithium-containing solution, removes precipitating and adds sodium carbonate, obtain carbon
Sour lithium, although this method reaches 98.0% and 95.0% for the rate of recovery of lithium and phosphorus, this method needs to be continually fed into high
Expensive protective gas, and this method is to the more demanding of equipment, equipment seriously corroded, thus causes production cost excessively high,
And will cause certain environmental pollution, it is not suitable for being mass produced.
CN108928839A discloses the method for lithium phosphate production lithium chloride solution, and this method uses lithium phosphate to add for raw material
Enter transforming agent to be converted in acid condition, after with alkali neutralization lithium chloride is obtained by filtration, but this method only simply illustrates
The production method of lithium chloride solution, to lithium chloride subsequent processing without reference to while the method for producing lithium chloride solution use
Single, limitation is strong, and CN108928839A is converted in the case where pH is 0.5~2.0 acid condition, in fact phosphorus under this condition
Acid group, which is first reacted with acid, generates dihydrogen phosphate, and dihydrogen phosphate continuation is reacted with phosphate radical generates one hydrogen radical of phosphoric acid, although its
Calcium monohydrogenphosphate precipitating is finally also created, but passes through two-step reaction, actually to the conversion of phosphorus and is not thorough, that is to say, that drop
The low recovery utilization rate of phosphorus, while a large amount of acid of this method consumption, corrosive equipment, the high requirements on the equipment are also unfavorable
In later maintenance.
Therefore, it there is no the method for high efficiente callback phosphorus and lithium from lithium phosphate at present.
Summary of the invention
The method of the purpose of the present invention is to provide a kind of from lithium phosphate synthetical recovery lithium and phosphorus.
The technical solution used in the present invention is:
The method of one of the objects of the present invention is to provide a kind of from lithium phosphate synthetical recovery lithium and phosphorus, including walk as follows
It is rapid:
1) add water slurrying in phosphoric acid lithium material, transforming agent is added and simultaneously adjusts pH=2.5~5；
2) heating reaction, filtering obtain lithium solution and dibasic alkaliine precipitating；
3) pH for adjusting lithium solution is that alkalinity cleans, and must clean lithium solution；
4) carbonate reaction is added, obtains lithium carbonate.
Preferably, above-mentioned steps 1) in adjust pH=3.0.
PH in step 1) is limited to above range by the present invention, generates one hydrogen radical of phosphoric acid, Ke Yiti by single step reaction
High transforming agent improves the effective rate of utilization of phosphorus to the conversion ratio of phosphorus, while can also reduce the consumption of acid, and reduction is produced into
This, and equipment will not be corroded substantially under the acid condition.
Preferably, above-mentioned steps 1) in the mass ratio of water and phosphoric acid lithium material be 5~10:1；More preferably 6:1.
Preferably, the molar ratio of phosphoric acid lithium material and transforming agent is 1:1.5~1.6 in step 1).
Preferably, the transforming agent in step 1) be selected from calcium sulfate, magnesium sulfate, calcium chloride, magnesium chloride, barium chloride, calcium nitrate,
At least one of magnesium nitrate, barium nitrate.
Preferably, the temperature of heating reaction is 70~90 DEG C in step 2).
Preferably, the time of heating reaction is 3~5h in step 2).
It is highly preferred that the temperature of heating reaction is 80 DEG C in step 2).
It is highly preferred that the time of heating reaction is 4h in step 2).
Preferably, phosphoric acid lithium material is selected from phosphoric acid lithium waste material in step 1).
Preferably, the content of lithium phosphate is 30%~95% in phosphoric acid lithium waste material in step 1)；More preferably 90%.
Preferably, the pH in step 3) is 9.0~11.0；More preferably 10~11.0.
The pH of step 3) is adjusted within the above range, is more advantageous to and removes impurity such as Ni, Ca, Mg, Co therein, make
The lithium solution that must be obtained is purer.
Preferably, the molar ratio of carbonate and the lithium in removal of impurities lithium solution is 0.55~0.75:1 in step 4)；More preferably
For 0.6:1.
The beneficial effects of the present invention are:
1, the method for the invention realizes the targets to phosphorus and the efficient synthetical recovery of lithium in phosphoric acid lithium material, for lithium
The rate of recovery is up to 98.5% or more, and the purity of lithium carbonate is up to 99% or more, while to the rate of recovery of phosphorus up to 96% or more, phosphoric acid
The purity of monohydric salt is up to 95% or more.
2, method of the invention is lower to the purity requirement of lithium phosphate, it can be achieved that being 30%~95% in lithium phosphate purity
To the efficient synthetical recovery of phosphorus therein and lithium in range, and limitation is small, while recovery method mild condition of the invention,
It is generated in reaction process without gas, big calorimetric will not be released, thus pollution is small, low for equipment requirements, entire reaction is easy to control
System, obtained by-product are dibasic alkaliine, and utility value is high, and entire cost recovery is low, is conducive to carry out large-scale reality
Using.
Specific embodiment
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art are according to the present invention
Some nonessential modifications and adaptations that the principle of elaboration is made all belong to the scope of protection of the present invention.Following specific works of example
Skill parameter etc. is also only an example in OK range, i.e. those skilled in the art can do suitable model by the explanation of this paper
Interior selection is enclosed, and does not really want to be defined in hereafter exemplary specific data.
Embodiment 1
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 10L pure water is added into beaker, the phosphoric acid lithium waste material that phosphoric acid lithium content is 30% is added while stirring
1841.3g (folding lithium metal 100g), it is rear that 800g calcium chloride transforming agent is added, utilize hydrochloric acid conditioning solution pH=3.5；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains the lithium solution and 625.2g calcium monohydrogenphosphate of 10.5L；
3) pH=10.0 that sodium carbonate liquor adjusts solution is added in lithium solution, remove Ni, Co therein, Mn, Ca,
10.0L removal of impurities lithium solution is obtained by filtration in the impurity such as Mg, Ba；
4) sodium carbonate liquor that 9.5L mass percent is 30%, after reacting 2h, mistake is added in 10.0L removal of impurities lithium solution
Lithium carbonate is obtained after filter washing is dry.
Wherein, the lithium concentration of 10.5L lithium solution obtained in step 2) is 9.43g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 99.01%, the conversion ratio of phosphorus is 96.54%, and the purity of calcium monohydrogenphosphate is 95.16%, what step 4) obtained
The purity of lithium carbonate is 99.32%.
Embodiment 2
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 15L pure water is added into beaker, the lithium phosphate waste material 920.6g that phosphoric acid lithium content is 60% is added while stirring
(folding lithium metal 100g), it is rear that 1000g calcium sulfate transforming agent is added, utilize sulfuric acid regulation solution pH=3.0；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains 16.2L lithium solution and 636.0g calcium monohydrogenphosphate；
3) pH=10.2 that sodium carbonate liquor adjusts solution is added in lithium solution, removes impurity therein, is obtained by filtration
17.3L removal of impurities lithium solution；
4) sodium carbonate liquor that 16.5L mass percent is 30% is added in 17.3L removal of impurities lithium solution, after reacting 2h,
Lithium carbonate is obtained after filtration washing is dry.
Wherein, the lithium concentration of 17.3L lithium solution obtained in step 2) is 5.75g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 99.47%, the conversion ratio of phosphorus is 98.22%, and the purity of calcium monohydrogenphosphate is 96.41%, what step 4) obtained
The purity of lithium carbonate is 99.15%.
Embodiment 3
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 5L pure water is added into beaker, the lithium phosphate waste material 690.5g that phosphoric acid lithium content is 80% is added while stirring
(folding lithium metal 100g), it is rear that the agent of 1400g conversion of calcium nitrate is added, pH value of solution=2.5 are adjusted using nitric acid；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains 5.6L lithium solution and 622.0g calcium monohydrogenphosphate；
3) pH=10.5 that sodium carbonate liquor adjusts solution is added in lithium solution, removes impurity therein, is obtained by filtration
5.4L removal of impurities lithium solution；
4) sodium carbonate liquor that 5.2L mass percent is 30%, after reacting 2h, mistake is added in 5.4L removal of impurities lithium solution
Lithium carbonate is obtained after filter washing is dry.
Wherein, the lithium concentration of 5.4L lithium solution obtained in step 2) is 18.29g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 98.77%, the conversion ratio of phosphorus is 96.13%, and the purity of calcium monohydrogenphosphate is 96.31%, what step 4) obtained
The purity of lithium carbonate is 99.63%.
Embodiment 4
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 5L pure water is added into beaker, the lithium phosphate waste material 690.5g that phosphoric acid lithium content is 80% is added while stirring
(folding lithium metal 100g), it is rear that 1750g barium chloride transforming agent is added, utilize hydrochloric acid conditioning solution pH=2.5；
2) 85 DEG C, isothermal reaction 4h are heated to, filtering obtains one hydrogen barium of 5.5L lithium solution and 717.8g phosphoric acid；
3) pH=10.8 that sodium carbonate liquor adjusts solution is added in lithium solution, removes impurity therein, is obtained by filtration
5.8L removal of impurities lithium solution；
4) sodium carbonate liquor that 5.4L mass percent is 30%, after reacting 2h, filtering is added in 5.8 removal of impurities lithium solution
Lithium carbonate is obtained after washing is dry.
Wherein, the lithium concentration of 5.8L lithium solution obtained in step 2) is 17.05g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 98.89%, the conversion ratio of phosphorus is 96.47%, and the purity of one hydrogen barium of phosphoric acid is 96.0%, the carbon that step 4) obtains
The purity of sour lithium is 99.51%.
Embodiment 5
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 8L pure water is added into beaker, the lithium phosphate waste material 613.7g that phosphoric acid lithium content is 90% is added while stirring
(folding lithium metal 100g), it is rear that 730g magnesium chloride transforming agent is added, utilize hydrochloric acid conditioning solution pH=3.0；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains one hydrogen magnesium of 9.2L lithium solution and 554.28g phosphoric acid；
3) pH=10.8 that sodium carbonate liquor adjusts solution is added in lithium solution, remove Ni, Co therein, Mn, Ca,
9.8L removal of impurities lithium solution is obtained by filtration in the impurity such as Mg, Ba；
4) sodium carbonate liquor that 9.6L mass percent is 30%, after reacting 2h, mistake is added in 9.8L removal of impurities lithium solution
Lithium carbonate is obtained after filter washing is dry.
Wherein, the lithium concentration of 9.8L lithium solution obtained in step 2) is 10.12g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 99.18%, phosphorous recovery 97.02%, the purity of one hydrogen magnesium of phosphoric acid is 96.5%, the carbonic acid that step 4) obtains
The purity of lithium is 99.08%.
Comparative example 1
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 10L pure water is added into beaker, the lithium phosphate waste material 920g (folding that phosphoric acid lithium content is 60% is added while stirring
Lithium metal 100g), it is rear that 850g calcium chloride transforming agent is added, utilize hydrochloric acid conditioning solution pH=1.5；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains the lithium solution and 613.7g calcium monohydrogenphosphate of 10.8L；
3) pH=10.0 that sodium carbonate liquor adjusts solution is added in lithium solution, remove Ni, Co therein, Mn, Ca,
10.5L removal of impurities lithium solution is obtained by filtration in the impurity such as Mg, Ba；
4) sodium carbonate liquor that 9.8L mass percent is 30%, after reacting 2h, mistake is added in 10.5L removal of impurities lithium solution
Lithium carbonate is obtained after filter washing is dry.
Wherein, the lithium concentration of 10.8L lithium solution obtained in step 2) is 9.08g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 98.06%, the conversion ratio of phosphorus is 94.75%, and the purity of calcium monohydrogenphosphate is 94.2%, the carbon that step 4) obtains
The purity of sour lithium is 99.0%.
Comparative example 2
A method of synthetical recovery lithium and phosphorus from lithium phosphate include the following steps:
1) 10L pure water is added into beaker, the lithium phosphate waste material 920g (folding that phosphoric acid lithium content is 60% is added while stirring
Lithium metal 100g), it is rear that 850g calcium chloride transforming agent is added, utilize hydrochloric acid conditioning solution pH=5.5；
2) 80 DEG C, isothermal reaction 4h are heated to, filtering obtains the lithium solution and 600.2g calcium monohydrogenphosphate of 11.2L；
3) pH=10.0 that sodium carbonate liquor adjusts solution is added in lithium solution, remove Ni, Co therein, Mn, Ca,
11.0L removal of impurities lithium solution is obtained by filtration in the impurity such as Mg, Ba；
4) sodium carbonate liquor that 10.5L mass percent is 30% is added in 11.0L removal of impurities lithium solution, after reacting 2h,
Lithium carbonate is obtained after filtration washing is dry.
Wherein, the lithium concentration of 11.2L lithium solution obtained in step 2) is 8.65g/L, and the lithium in lithium phosphate is calculated
Conversion ratio be 96.88%, the conversion ratio of phosphorus is 92.76%, and the purity of calcium monohydrogenphosphate is 91.16%, what step 4) obtained
The purity of lithium carbonate is 98.32%.
Claims (10)
1. a kind of method of synthetical recovery lithium and phosphorus from lithium phosphate, characterized by the following steps:
1) add water slurrying in phosphoric acid lithium material, transforming agent is added and simultaneously adjusts pH=2.5~5；
2) heating reaction, filtering obtain lithium solution and dibasic alkaliine precipitating；
3) pH for adjusting lithium solution is that alkalinity cleans, and must clean lithium solution；
4) carbonate reaction is added, obtains lithium carbonate.
2. according to the method described in claim 1, it is characterized by: adjusting pH=3.0 in step 1).
3. according to the method described in claim 1, it is characterized by: the mass ratio of water and the phosphoric acid lithium material is in step 1)
5~10:1.
4. according to the method described in claim 1, it is characterized by: phosphoric acid lithium material described in step 1) and the transforming agent
Molar ratio is 1:1.5~1.6.
5. according to the method described in claim 1, it is characterized by: transforming agent described in step 1) be selected from calcium sulfate, magnesium sulfate,
At least one of calcium chloride, magnesium chloride, barium chloride, calcium nitrate, magnesium nitrate, barium nitrate.
6. according to the method described in claim 1, it is characterized by: the temperature of heating reaction is 70~90 DEG C in step 2)；It is excellent
The time of selection of land, the middle heating reaction of step 2) is 3~5h.
7. according to the method described in claim 1, it is characterized by: step 1) the phosphoric acid lithium material is useless selected from phosphoric acid lithium
Material.
8. according to the method described in claim 7, it is characterized by: lithium phosphate contains in the waste material of phosphoric acid lithium described in step 1)
Amount is 30%~95%.
9. method described in any one according to claim 1~8, it is characterised in that: the pH in step 3) is 9.0~11.0.
10. method described in any one according to claim 1~8, it is characterised in that: carbonate and removal of impurities lithium are molten in step 4)
The molar ratio of lithium in liquid is 0.55~0.75:1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111498872A (en) * | 2020-04-14 | 2020-08-07 | 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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| 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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| CN110316747B (en) | 2022-03-11 |
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