CN109264748A - A method of lithium carbonate is prepared with crude lithium phosphate - Google Patents
A method of lithium carbonate is prepared with crude lithium phosphate Download PDFInfo
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- CN109264748A CN109264748A CN201811147713.5A CN201811147713A CN109264748A CN 109264748 A CN109264748 A CN 109264748A CN 201811147713 A CN201811147713 A CN 201811147713A CN 109264748 A CN109264748 A CN 109264748A
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- lithium
- phosphate
- crude
- roasting
- carbonate
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C01B25/325—Preparation by double decomposition
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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
- C01B25/34—Magnesium phosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B13/00—Fertilisers produced by pyrogenic processes from phosphatic materials
- C05B13/02—Fertilisers produced by pyrogenic processes from phosphatic materials from rock phosphates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of methods for preparing lithium carbonate with crude lithium phosphate; method includes the following steps: transforming agent is added in crude lithium phosphate; it is roasted at 200-1000 DEG C; protective gas is passed through before roasting and always in roasting process; by roasting after, material conversion at phosphate solid and soluble lithium salt mixture；Material after roasting carries out wet ball grinding, and phosphate solid and lithium-containing solution are obtained after filtering；It is 9.0-11.0 that lithium-containing solution, which adjusts pH value, is filtered to remove the precipitating of generation, adds sodium carbonate liquor reaction, obtains lithium carbonate.Lithium in crude lithium phosphate slag is recycled using method of the invention, the lithium rate of recovery is up to 98% or more.Present invention process is simple, and energy consumption cost is cheap, and that realizes crude lithium phosphate slag efficiently mentions lithium, and by-product calcium and magnesium phosphate can be used as calcium magnesium phosphate raw material, has considerable economic benefit.
Description
Technical field
The invention belongs to the regeneration recycling fields of waste and old lithium-containing materials, and in particular to a kind of with the preparation of crude lithium phosphate
The method of lithium carbonate.
Background technique
Lithium ion battery with advantages such as high specific energy, long circulation life, memory-less effects due to being widely used in moving
Telecommunications market and Prospect of EVS Powered with Batteries market.Along with the rapid development of lithium ion battery industry, to mutually powered-down
The demand sustainable growth of pond 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.In order to meet the booming needs of lithium ion battery industry, both at home and abroad around from
The technology that spodumene, lepidolite and salt lake bittern extract lithium has carried out a large amount of research work and has carried out industrialized production.?
In these production processes when handling before the waste water generated after to sinker discharges, soluble phosphate is usually added into remove
Heavy metal, alkaline-earth metal and lithium in water, form the waste residue of a large amount of phosphoric acid lithiums.At present in high efficiente callback lithium phosphate waste residue
The technical research report of lithium is less.
108285156 A of Chinese patent application CN, which is disclosed, a kind of extracts pure Lithium Carbonate from the phosphoric acid lithium waste residue
Method first handles lithium phosphate waste residue with acid solution, obtains pickle liquor after filtering；Add Dephosphorising agent, the cation and phosphorus of Dephosphorising agent
Acid group reaction generates compound M, and the anion of Dephosphorising agent is reacted with lithium ion generates compound Q, utilizes compound M, Q solubility
Difference be filtered to remove phosphate radical, obtain the filtrate containing lithium ion；Cleanser is added into filtrate, removes foreign ion, it is used
Cleanser be dissolvable sulfide, hydroxide, acetate, oxalates, carbonate etc.；Finally, soluble carbonate salt is added,
It reacts and lithium carbonate is made.The patent converts lithium solution and insoluble phosphate for lithium phosphate using wet processing, long flow path, instead
Should be slow, the separation of solid and liquid of gained insoluble slag is difficult.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the purpose of the present invention is to provide one kind with crude lithium phosphate
The method for preparing lithium carbonate.
The purpose of the invention is achieved by the following technical solution:
A method of lithium carbonate is prepared with crude lithium phosphate, comprising the following steps:
(1) crude lithium phosphate is dry, transforming agent is added, grinding mixes, and 1-6h is roasted at 200-1000 DEG C, roasts
Before be passed through protective gas always in roasting process, with take away reaction generate vapor and other side reaction gases, keep away
Exempt from Carbon Dioxide in Air and side reaction occurs for transforming agent, while reducing impurity phase and oxygen generation side reaction；After roasting,
Material conversion at phosphate solid and soluble lithium salt mixture；
The crude lithium phosphate, be during extracting lithium the waste water that generates be added before discharge soluble phosphate with
Remove heavy metal, alkaline-earth metal and the lithium in water removal, the waste residue of the phosphoric acid lithium of formation；
The drying is preferably dried to moisture content < 1.0%wt；
The transforming agent is one or more of calcium chloride, calcium sulfate, magnesium chloride, magnesium sulfate, calcium nitrate or magnesium nitrate；
Used transforming agent is the sulfate, villaumite or nitrate of alkaline-earth metal, and effect is to grab lithium phosphate under the high temperature conditions
In phosphate radical, form new calcium phosphate phase/magnesium, anion and lithium ion combine, and form soluble lithium salt；
The addition mole of the transforming agent is 0.5-0.8 times of lithium mole in crude lithium phosphate；
The grinding is preferably ground to 74 μm of granularity <；
The preferred nitrogen of the protective gas, argon gas or helium；
The preferred 2-4h of the calcining time；
(2) will the material that obtained after roasting be added ball mill in carry out wet ball grinding, obtained after filtering phosphate solid and
Lithium-containing solution；Material caking phenomenon is serious after roasting, caking materials need to be crushed to certain fineness by ball milling, increased in material
The leaching rate of soluble lithium salt；
The wet ball grinding, slurry liquid-solid ratio are preferred (2-3): 1；It is milled to fineness of materials >=100 mesh；
(3) it is 9.0-11.0 that the lithium-containing solution obtained, which is added alkaline matter and adjusts pH value, is filtered to remove the precipitating of generation, obtains
To pure lithium solution；Sodium carbonate liquor is added, after reaction, filtering will obtain lithium carbonate after washing of precipitate, drying；
The alkaline matter is one or more of sodium carbonate, potassium carbonate or lithium carbonate；
The sodium carbonate liquor preferred mass volumetric concentration is 30%；
The time of the reaction preferred 2h.
Reaction mechanism of the invention is under the high temperature conditions, to realize lithium phosphate and alkali earth metal sulfate, villaumite, nitrate
Conversion:
2Li3PO4+3MeCl2=6LiCl+Me3(PO4)2Me=Ca, Mg
2Li3PO4+3Me(NO3)2=6LiNO3+Me3(PO4)2Me=Ca, Mg
2Li3PO4+3MeSO4=3Li2SO4+Me3(PO4)2Me=Ca, Mg
Li++CO3 2-=Li2CO3↓
The present invention has the following advantages and effects with respect to the prior art:
Lithium in crude lithium phosphate slag is recycled using method of the invention, the lithium rate of recovery is up to 98% or more.Work of the present invention
Skill is simple, and energy consumption cost is cheap, and that realizes crude lithium phosphate slag efficiently mentions lithium, and by-product calcium and magnesium phosphate can be used as calcium magnesium phosphate
Raw material has considerable economic benefit.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
A method of lithium carbonate is prepared with crude lithium phosphate, comprising the following steps:
(1) dry mixed
It takes the crude lithium phosphate of 100g (Li content 17.45%wt) dry to moisture 0.74%, 150g anhydrous calcium chloride is added
Mixed grinding is to 74 μm of designated size <；
(2) roasting conversion
The material that step (1) is uniformly mixed is put into heating furnace, nitrogen is passed through, under the conditions of 300 DEG C, roasts 3h, it will
Material conversion at phosphate solid and soluble lithium salt mixture；
(3) ball milling water logging
By the material 250g after roasting conversion, water 600ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Calcium phosphate solid and lithium-containing solution 600ml, lithium content 28.71g/L calculate to obtain lithium leaching rate 98.72%.
(4) lithium liquid cleans
The lithium-containing solution 600ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH value to 10.2, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 350ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
Embodiment 2
A method of lithium carbonate is prepared with crude lithium phosphate, comprising the following steps:
(1) dry mixed
Take the crude lithium phosphate of 100g (Li content 17.45%wt) dry to moisture 0.41%, be added 50g anhydrous calcium chloride and
70g anhydrous magnesium chloride mixed grinding is to 74 μm of designated size <；
(2) roasting conversion
The material that step (1) is uniformly mixed is put into heating furnace, nitrogen is passed through, under the conditions of 500 DEG C, roasts 4h, it will
Material conversion at phosphate solid and soluble lithium salt mixture；
(3) ball milling water logging
By the material 220g after roasting conversion, water 600ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Calcium phosphate solid and lithium-containing solution 600ml, lithium content 28.52g/L calculate to obtain lithium leaching rate 98.06%.
(4) lithium liquid cleans
The lithium-containing solution 600ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH value to 10.6, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 350ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
Embodiment 3
A method of lithium carbonate is prepared with crude lithium phosphate, comprising the following steps:
(1) dry mixed
It takes the crude lithium phosphate of 100g (Li content 17.45%wt) dry to moisture 0.39%, 180g dead plaster is added
Mixed grinding is to 74 μm of designated size <；
(2) roasting conversion
The material that step (1) is uniformly mixed is put into heating furnace, argon gas is passed through, under the conditions of 600 DEG C, roasts 5h, it will
Material conversion at phosphate solid and soluble lithium salt mixture；
(3) ball milling water logging
By the material 280g after roasting conversion, water 800ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Calcium phosphate solid and lithium-containing solution 800ml, lithium content 21.59g/L calculate to obtain lithium leaching rate 99.00%.
(4) lithium liquid cleans
The lithium-containing solution 800ml that step (3) is obtained is added sodium carbonate liquor and adjusts pH value to 10.1, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 300ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
Embodiment 4
A method of lithium carbonate is prepared with crude lithium phosphate, comprising the following steps:
(1) dry mixed
It takes the crude lithium phosphate of 100g (Li content 17.45%wt) dry to moisture 0.32%, mono- water calcium nitrate of 220g is added
With 60g magnesium nitrate hexahydrate mixed grinding to 74 μm of designated size <；
(2) roasting conversion
The material that step (1) is uniformly mixed is put into heating furnace, argon gas is passed through, under the conditions of 300 DEG C, roasts 5h, it will
Material conversion at phosphate solid and soluble lithium salt mixture；
(3) ball milling water logging
By the material 320g after roasting conversion, water 1000ml is added in ball mill and carries out wet ball grinding, obtains after filtering
Calcium phosphate solid and lithium-containing solution 1000ml, lithium content 17.28g/L calculate to obtain lithium leaching rate 99.03%.
(4) lithium liquid cleans
The lithium-containing solution 1000ml that step (3) is obtained is added solution of potassium carbonate and adjusts pH value to 10.4, removes therein
Pure lithium solution is obtained by filtration in impurity；
(5) prepared by lithium carbonate
30% sodium carbonate liquor of 300ml is added into the lithium solution 400ml that step (4) obtains, after reacting 2h, crosses diafiltration
It washs, obtains lithium carbonate product after dry.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of method for preparing lithium carbonate with crude lithium phosphate, it is characterised in that the following steps are included:
(1) crude lithium phosphate is dry, transforming agent is added, grinding mixes, and 1-6h is roasted at 200-1000 DEG C, before roasting
With protective gas is passed through in roasting process always, after roasting, material conversion is at phosphate solid and soluble lithium salt
Mixture；
The transforming agent is one or more of calcium chloride, calcium sulfate, magnesium chloride, magnesium sulfate, calcium nitrate or magnesium nitrate；
(2) material obtained after roasting is added in ball mill and carries out wet ball grinding, phosphate solid is obtained after filtering and containing lithium
Solution；
(3) it is 9.0-11.0 that the lithium-containing solution obtained, which is added alkaline matter and adjusts pH value, is filtered to remove the precipitating of generation, obtains pure
Net lithium solution；Sodium carbonate liquor is added, after reaction, filtering will obtain lithium carbonate after washing of precipitate, drying.
2. according to the method described in claim 1, it is characterized by: the addition mole of step (1) described transforming agent is crude
0.5-0.8 times of lithium mole in lithium phosphate.
3. according to the method described in claim 1, it is characterized by: protective gas described in step (1) be nitrogen, argon gas or
Helium.
4. according to the method described in claim 1, it is characterized by: alkaline matter described in step (3) is sodium carbonate, potassium carbonate
Or one or more of lithium carbonate.
5. according to the method described in claim 1, it is characterized by: drying described in step (1) is dry to moisture content <
1.0%wt.
6. according to the method described in claim 1, it is characterized by: grinding described in step (1) is to be ground to 74 μm of granularity <.
7. according to the method described in claim 1, it is characterized by: calcining time described in step (1) is 2-4h.
8. according to the method described in claim 1, it is characterized by: wet ball grinding described in step (2), slurry liquid-solid ratio are
(2-3): 1, it is milled to fineness of materials >=100 mesh.
9. according to the method described in claim 1, it is characterized by: its quality volume of sodium carbonate liquor described in step (3) is dense
Degree is 30%.
10. according to the method described in claim 1, it is characterized by: the time of step (3) described reaction is 2h.
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| CN201811147713.5A CN109264748B (en) | 2018-09-29 | 2018-09-29 | Method for preparing lithium carbonate from crude lithium phosphate |
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| CN201811147713.5A CN109264748B (en) | 2018-09-29 | 2018-09-29 | Method for preparing lithium carbonate from crude lithium phosphate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110316747A (en) * | 2019-07-25 | 2019-10-11 | 湖南邦普循环科技有限公司 | A method of synthetical recovery lithium and phosphorus from lithium phosphate |
| CN112357938A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by using lithium phosphate |
| 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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| CN112357938A (en) * | 2020-11-12 | 2021-02-12 | 萍乡市拓源实业有限公司 | Method for preparing battery-grade lithium carbonate by using lithium phosphate |
| 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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