CN106241838A - Lithium carbonate technique produced by lithium phosphate - Google Patents
Lithium carbonate technique produced by lithium phosphate Download PDFInfo
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- CN106241838A CN106241838A CN201610666095.XA CN201610666095A CN106241838A CN 106241838 A CN106241838 A CN 106241838A CN 201610666095 A CN201610666095 A CN 201610666095A CN 106241838 A CN106241838 A CN 106241838A
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- Prior art keywords
- lithium
- phosphate
- produced
- filtrate
- 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
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Lithium carbonate technique produced by a kind of lithium phosphate, comprises the following steps, the preparation of supplementary material, lithium phosphate convert, lithium sulfate feed liquid is produced, the producing of lithium carbonate, the recycling of filtering residue and filtrate.Lithium carbonate technique produced by the lithium phosphate of the present invention, the heat energy utilizing phosphorus is extracted principle by sulfate substitution, produced lithium sulfate crystal and phosphoric acid by solid-liquid separation and partial solubility lithium sulfate reaches the decomposition and separation purpose of lithium phosphate, during carry out the conversion of regulation system by sodium hydroxide and finally produce lithium sulfate solution and part lithium phosphate and precipitate, lithium sulfate solution need not concentrate directly to precipitate with sodium carbonate and obtain industry and lithium carbonate product, and lithium phosphate and sodium radio-phosphate,P-32 solution circulating and recovering.This technique has that the response rate is high, energy consumption is low, without features such as waste residues.
Description
Technical field
The present invention relates to a kind of lithium phosphate and produce lithium carbonate technique.
Background technology
Due to rise and the wide popularization and application of lithium of new forms of energy, all there is the synthetical recovery problem of lithium in many industries,
And lithium phosphate can be work perfectly well as reclaiming the intermediate of lithium and then converting purification as a kind of precipitate under low consistency conditions
For lithium carbonate product.Lithium phosphate be converted into acid that lithium carbonate technique uses the most substantially molten after again with compound and the phosphate radical of calcium
Forming calcium phosphate and remove phosphate radical, then the concentrated sodium carbonate of solution precipitates and obtains lithium carbonate product, and current technique is deposited
Low in the lithium response rate, energy consumption is big, the shortcoming that the quantity of slag is big.
Summary of the invention
It is an object of the invention to provide a kind of response rate height, lithium carbonate technique produced by energy consumption lithium phosphate low, without waste residue.
Lithium carbonate technique produced by the lithium phosphate of the present invention, comprises the following steps:
1, the preparation of supplementary material: lithium phosphate: containing lithium 10-16%, powder；Sulphuric acid: 98% content, technical grade；Sodium hydroxide: 99%
Content, technical grade；Sodium carbonate: 99% content, technical grade；Dilute sulfuric acid is prepared: 98% concentrated sulphuric acid is made into 60-70% concentration standby；Hydrogen
Sodium oxide concentration is prepared: solid (99%) sodium hydroxide is configured to 40% concentration standby；
2, lithium phosphate converts: is joined by one ton of lithium phosphate powder and fills 1.5m3The pp material of the dilute sulfuric acid of above-mentioned steps preparation
In agitator, stirring converts 30 minutes, is then filtered by vacuum suction filter dish, and filtering residue and filtrate split standby；
3, lithium sulfate feed liquid is produced: filtering residue step 2 produced is put in the pp material stirring bucket of band stirring, adds 1.5 m3
Clear water dissolves, and then adjusts pH >=7 with 40% sodium hydroxide solution of step 1 preparation, stirs 30 minutes, then by sheet frame pressure
Filter filters, and filtering residue is lithium phosphate, and dry for standby, filtrate stores for future use；
4, the producing of lithium carbonate: filtrate step 3 produced joins in the stainless steel cask of band stirring, is heated to >=70 DEG C, throws
Enter solid sodium carbonate insulated and stirred 30-60 minute of 8～10 times of weight of lithium content quality, then filter with vacuum suction filter dish,
Filtering residue washs twice on suction strainer dish with >=70 DEG C of hot water, and drying and packaging is product lithium carbonate, and precipitation filtrates stores for future use, washing
Liquid discharges；
5, the recycling of filtering residue and filtrate: the filtrate that filtrate step 3 produced produces with step 4 merges puts into band stirring pp
In material bucket, regulate pH >=7 with sodium hydroxide, stir 30 minutes, then filtered by filter press, with step after filtering residue drying
Rapid 3 produce filtering residues be incorporated as feedstock circulation use, filtrate be sodium phosphate can concentrate as product return precipitate phosphoric acid lithium make
With.
Lithium carbonate technique produced by the lithium phosphate of the present invention, utilizes the heat energy of phosphorus to be extracted principle by sulfate substitution, passes through solid-liquid
Separate and produce lithium sulfate crystal and phosphoric acid and partial solubility lithium sulfate to reach the decomposition and separation purpose of lithium phosphate, during
Carrying out the conversion of regulation system by sodium hydroxide and finally produce lithium sulfate solution and part lithium phosphate precipitation, lithium sulfate solution is not
Industry and lithium carbonate product is obtained with concentrating directly to precipitate with sodium carbonate, and lithium phosphate and sodium radio-phosphate,P-32 solution circulating and recovering.This work
Skill has that the response rate is high, energy consumption is low, without features such as waste residues.
Detailed description of the invention
Lithium carbonate technique produced by a kind of lithium phosphate, comprises the following steps:
1, the preparation of supplementary material: lithium phosphate: containing lithium 10-16%, powder；Sulphuric acid: 98% content, technical grade；Sodium hydroxide: 99%
Content, technical grade；Sodium carbonate: 99% content, technical grade；Dilute sulfuric acid is prepared: 98% concentrated sulphuric acid is made into 60-70% concentration standby；Hydrogen
Sodium oxide concentration is prepared: solid (99%) sodium hydroxide is configured to 40% concentration standby；
2, lithium phosphate converts: is joined by one ton of lithium phosphate powder and fills 1.5m3The 4 of the dilute sulfuric acid of above-mentioned steps 1 preparation
m3In pp material stirring bucket, stirring converts half an hour, is then filtered by vacuum suction filter dish, and filtering residue and filtrate split standby；
3, lithium sulfate feed liquid is produced: filtering residue step 2 produced puts into the 3m of band stirring3In the agitator of pp material, add
1.5m3Clear water dissolves, and then adjusts pH >=7 with 40% sodium hydroxide solution of step 1 preparation, stirs half an hour, then pass through plate
Frame Filter Press, filtering residue is lithium phosphate, and dry for standby, filtrate stores for future use；
4, the producing of lithium carbonate: filtrate step 3 produced joins a 2m3In the stainless steel cask of band stirring, be heated to >=
70 DEG C, put into solid sodium carbonate insulated and stirred half an hour of 8～10 times of weight of lithium content quality to 1 hour, then use vacuum
Suction strainer dish filters, and filtering residue washs twice on suction strainer dish with >=70 DEG C of hot water, and drying and packaging is product lithium carbonate, and precipitation filtrates stores up
Depositing standby, cleaning mixture discharges；
5, the recycling of filtering residue and filtrate: the filtrate that filtrate step 3 produced produces with step 4 merges puts into 4m3Band stirs
Mix in pp material bucket, regulate pH >=7 with sodium hydroxide (liquid, solid), stir half an hour, then pass through filter press
Filtering, the filtering residue produced with step 3 after filtering residue drying is incorporated as feedstock circulation and uses, and filtrate is that sodium phosphate can concentrate as product
Product return precipitate phosphoric acid lithium and use.
Claims (2)
1. lithium carbonate technique produced by a lithium phosphate, it is characterised in that: it comprises the following steps:
(1), the preparation of supplementary material: lithium phosphate: containing lithium 10-16%, powder；Sulphuric acid: 98% content, technical grade；Sodium hydroxide:
99% content, technical grade；Sodium carbonate: 99% content, technical grade；Dilute sulfuric acid is prepared: 98% concentrated sulphuric acid is made into 60-70% concentration standby
With；Naoh concentration is prepared: solid sodium hydroxide is configured to 40% concentration standby；
(2), lithium phosphate converts: is joined by one ton of lithium phosphate powder and fills 1.5m3The pp material of the dilute sulfuric acid of above-mentioned steps preparation
In matter agitator, stirring converts 30 minutes, is then filtered by vacuum suction filter dish, and filtering residue and filtrate split standby；
(3), lithium sulfate feed liquid is produced: is put into by the filtering residue that step (2) produces in the pp material stirring bucket of band stirring, adds
1.5 m3Clear water dissolves, and 40% sodium hydroxide solution then prepared by step (1) adjusts pH >=7, stirs 30 minutes, then leads to
Crossing filter press to filter, filtering residue is lithium phosphate, and dry for standby, filtrate stores for future use；
(4), the producing of lithium carbonate: the filtrate that step (3) produces is joined in the stainless steel cask of band stirring, be heated to >=70
DEG C, put into solid sodium carbonate insulated and stirred 30-60 minute of 8～10 times of weight of lithium content quality, then use vacuum suction filter dish
Filtering, filtering residue washs twice on suction strainer dish with >=70 DEG C of hot water, and drying and packaging is product lithium carbonate, and precipitation filtrates stores standby
With, cleaning mixture discharges.
Lithium carbonate technique produced by lithium phosphate the most according to claim 1, it is characterised in that: the filtrate that step (3) is produced
The filtrate produced with step (4) merges puts in band stirring pp material bucket, regulates pH >=7 with sodium hydroxide, stirs 30 minutes, so
Being filtered by filter press afterwards, the filtering residue produced with step (3) after filtering residue drying is incorporated as feedstock circulation and uses, and filtrate is
Sodium phosphate can concentrate and use as product return precipitate phosphoric acid lithium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610666095.XA CN106241838B (en) | 2016-08-15 | 2016-08-15 | Lithium phosphate produces lithium carbonate technique |
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| CN201610666095.XA CN106241838B (en) | 2016-08-15 | 2016-08-15 | Lithium phosphate produces lithium carbonate technique |
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| CN106241838A true CN106241838A (en) | 2016-12-21 |
| CN106241838B CN106241838B (en) | 2017-07-07 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110127731A (en) * | 2019-05-15 | 2019-08-16 | 上海中锂实业有限公司 | A method of battery-level lithium carbonate is directly prepared by lithium phosphate |
| CN112703260A (en) * | 2018-05-30 | 2021-04-23 | 澳大利亚锂公司 | Method for recovering lithium values |
| WO2024074162A1 (en) * | 2022-10-04 | 2024-04-11 | Geomet S.R.O. | Method and system for treatment of lithiferous ore |
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| CN101125668A (en) * | 2007-08-21 | 2008-02-20 | 四川省射洪锂业有限责任公司 | Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution |
| KR20120014828A (en) * | 2010-08-10 | 2012-02-20 | 재단법인 포항산업과학연구원 | Production method of lithium carbonate from brines |
| KR20120021675A (en) * | 2010-08-12 | 2012-03-09 | 재단법인 포항산업과학연구원 | Manufacturing method of lithium carbonate with high purity |
| JP2012116681A (en) * | 2010-11-30 | 2012-06-21 | Nittetsu Mining Co Ltd | Method for producing lithium carbonate |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| CN103950956A (en) * | 2014-05-22 | 2014-07-30 | 甘孜州泸兴锂业有限公司 | Process for producing lithium carbonate from spodumene concentrate by sulfuric acid method |
| CN105502441A (en) * | 2016-01-14 | 2016-04-20 | 四川天齐锂业股份有限公司 | Method for continuously producing cell-grade lithium carbonate |
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2016
- 2016-08-15 CN CN201610666095.XA patent/CN106241838B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101125668A (en) * | 2007-08-21 | 2008-02-20 | 四川省射洪锂业有限责任公司 | Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution |
| KR20120014828A (en) * | 2010-08-10 | 2012-02-20 | 재단법인 포항산업과학연구원 | Production method of lithium carbonate from brines |
| KR20120021675A (en) * | 2010-08-12 | 2012-03-09 | 재단법인 포항산업과학연구원 | Manufacturing method of lithium carbonate with high purity |
| JP2012116681A (en) * | 2010-11-30 | 2012-06-21 | Nittetsu Mining Co Ltd | Method for producing lithium carbonate |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| CN103950956A (en) * | 2014-05-22 | 2014-07-30 | 甘孜州泸兴锂业有限公司 | Process for producing lithium carbonate from spodumene concentrate by sulfuric acid method |
| CN105502441A (en) * | 2016-01-14 | 2016-04-20 | 四川天齐锂业股份有限公司 | Method for continuously producing cell-grade lithium carbonate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112703260A (en) * | 2018-05-30 | 2021-04-23 | 澳大利亚锂公司 | Method for recovering lithium values |
| 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 |
| CN110127731A (en) * | 2019-05-15 | 2019-08-16 | 上海中锂实业有限公司 | A method of battery-level lithium carbonate is directly prepared by lithium phosphate |
| WO2024074162A1 (en) * | 2022-10-04 | 2024-04-11 | Geomet S.R.O. | Method and system for treatment of lithiferous ore |
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| Publication number | Publication date |
|---|---|
| CN106241838B (en) | 2017-07-07 |
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