CN106241838B - Lithium phosphate produces lithium carbonate technique - Google Patents
Lithium phosphate produces lithium carbonate technique Download PDFInfo
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- CN106241838B CN106241838B CN201610666095.XA CN201610666095A CN106241838B CN 106241838 B CN106241838 B CN 106241838B CN 201610666095 A CN201610666095 A CN 201610666095A CN 106241838 B CN106241838 B CN 106241838B
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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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Abstract
A kind of lithium phosphate produces lithium carbonate technique, comprises the following steps, and the preparation of supplementary material, lithium phosphate conversion, lithium sulfate feed liquid are produced, the producing of lithium carbonate, filter residue and filtrate recycle.Lithium phosphate of the invention produces lithium carbonate technique, principle is extracted by sulfate substitution using the heat energy of phosphorus, sulfuric acid crystalline lithium and phosphoric acid and partial solubility lithium sulfate is produced by separation of solid and liquid to reach the decomposition and separation purpose of lithium phosphate, during finally produce lithium sulfate solution and part lithium phosphate to precipitate come the conversion of regulation system by NaOH, lithium sulfate solution is directly precipitated with sodium carbonate without concentration and obtains industry and lithium carbonate product, and lithium phosphate and sodium radio-phosphate,P-32 solution circulating and recovering.The technique has that the rate of recovery is high, energy consumption is low, without waste residue the features such as.
Description
Technical field
Lithium carbonate technique is produced the present invention relates to a kind of lithium phosphate.
Background technology
, all there is the synthetical recovery of lithium in many industries in rise and the wide popularization and application of lithium due to new energy,
And lithium phosphate can be work perfectly well as reclaiming the intermediate of lithium and then convert purification as a kind of sediment under low consistency conditions
It is lithium carbonate product.Lithium phosphate be converted into that lithium carbonate technique uses substantially at present it is sour molten after again with the compound and phosphate radical of calcium
Form calcium phosphate and remove phosphate radical, then solution is concentrated obtains lithium carbonate product with sodium carbonate precipitation, and current technique is deposited
Low in the lithium rate of recovery, energy consumption is big, the big shortcoming of the quantity of slag.
The content of the invention
It is an object of the invention to provide a kind of rate of recovery it is high, energy consumption is low, the lithium phosphate without waste residue produces lithium carbonate technique.
Lithium phosphate of the invention produces lithium carbonate technique, comprises the following steps：
1st, the preparation of supplementary material：Lithium phosphate：10-16% containing lithium, it is powdered；Sulfuric acid：98% content, technical grade；NaOH：
99% content, technical grade；Sodium carbonate：99% content, technical grade；Dilute sulfuric acid is prepared：98% concentrated sulfuric acid is made into 60-70% concentration standby
With；Naoh concentration is prepared：By solid（99%）It is standby that NaOH is configured to 40% concentration；
2nd, lithium phosphate conversion：One ton of phosphoric acid lithium powder is added to and fills 1.5m3The pp of the dilute sulfuric acid that above-mentioned steps are prepared
Conversion 30 minutes is stirred in material stirring bucket, is then filtered by vacuum suction filter disk, filter residue and filtrate split standby；
3rd, lithium sulfate feed liquid is produced：By the filter residue that step 2 is produced put into stirring pp material stirrings bucket in, add
1.5 m3Clear water dissolves, and 40% sodium hydroxide solution then prepared with step 1 adjusts pH >=7, stirs 30 minutes, then passes through
Plate and frame filter press is filtered, and filter residue is lithium phosphate, and dry for standby, filtrate stores for future use；
4th, lithium carbonate is produced：The filtrate that step 3 is produced is added in the stainless steel cask with stirring, >=70 are heated to
DEG C, then the solid sodium carbonate insulated and stirred of 8~10 times of weight of input lithium content quality 30-60 minutes uses vacuum suction filter disk
Filtering, filter residue use >=70 DEG C hot water is washed twice on suction strainer disk, and drying and packaging is product lithium carbonate, and precipitation filtrates storage is standby
With cleaning solution discharge；
5th, filter residue and filtrate recycle：The filtrate that step 3 is produced merges with the filtrate that step 4 is produced and is put into band and stirs
Mix in pp materials bucket, pH >=7 are adjusted with NaOH, stir 30 minutes, then filtered by plate and frame filter press, after filter residue drying
The filter residue produced with step 3 is incorporated as feedstock circulation and uses, and filtrate returns to precipitate phosphoric acid for sodium phosphate can be concentrated as product
Lithium is used.
Lithium phosphate of the invention produces lithium carbonate technique, principle is extracted by sulfate substitution using the heat energy of phosphorus, by solid-liquid
Separate and produce sulfuric acid crystalline lithium and phosphoric acid and partial solubility lithium sulfate and reach the decomposition and separation purpose of lithium phosphate, during
Lithium sulfate solution and part lithium phosphate is finally produced to precipitate come the conversion of regulation system by NaOH, lithium sulfate solution is not
Directly precipitated with sodium carbonate with concentration and obtain industry and lithium carbonate product, and lithium phosphate and sodium radio-phosphate,P-32 solution circulating and recovering.The work
Skill has that the rate of recovery is high, energy consumption is low, without waste residue the features such as.
Specific embodiment
A kind of lithium phosphate produces lithium carbonate technique, comprises the following steps：
1st, the preparation of supplementary material：Lithium phosphate：10-16% containing lithium, it is powdered；Sulfuric acid：98% content, technical grade；NaOH：
99% content, technical grade；Sodium carbonate：99% content, technical grade；Dilute sulfuric acid is prepared：98% concentrated sulfuric acid is made into 60-70% concentration standby
With；Naoh concentration is prepared：By solid（99%）It is standby that NaOH is configured to 40% concentration；
2nd, lithium phosphate conversion：One ton of phosphoric acid lithium powder is added to and fills 1.5m3The 4 of the dilute sulfuric acid that above-mentioned steps 1 are prepared
m3Conversion half an hour is stirred in pp material stirrings bucket, is then filtered by vacuum suction filter disk, filter residue and filtrate split standby；
3rd, lithium sulfate feed liquid is produced：The filter residue that step 2 is produced is put into the 3m with stirring3In the agitator of pp materials,
Add 1.5m3Clear water dissolves, and 40% sodium hydroxide solution then prepared with step 1 adjusts pH >=7, stirs half an hour, Ran Houtong
Plate and frame filter press filtering is crossed, filter residue is lithium phosphate, and dry for standby, filtrate stores for future use；
4th, lithium carbonate is produced：The filtrate that step 3 is produced is added to a 2m3In stainless steel cask with stirring, heating
To >=70 DEG C, the solid sodium carbonate insulated and stirred half an hour of 8~10 times of weight of lithium content quality is put into 1 hour, Ran Houyong
Vacuum suction filter disk is filtered, and filter residue use >=70 DEG C hot water is washed twice on suction strainer disk, and drying and packaging is product lithium carbonate, precipitation filter
Liquid is stored for future use, cleaning solution discharge；
5th, filter residue and filtrate recycle：The filtrate that step 3 is produced merges with the filtrate that step 4 is produced and is put into 4m3
In band stirring pp material buckets, NaOH is used（Liquid, solid）Regulation pH >=7, stir half an hour, then by sheet frame pressure
Filter is filtered, and the filter residue produced with step 3 after filter residue drying is incorporated as feedstock circulation and uses, and filtrate can concentrate work for sodium phosphate
Used for product returns to precipitate phosphoric acid lithium.
Claims (1)
1. a kind of lithium phosphate produces lithium carbonate technique, it is characterised in that：It is comprised the following steps：
（1）, supplementary material preparation：Lithium phosphate：10-16% containing lithium, it is powdered；Sulfuric acid：98% content, technical grade；NaOH：
99% content, technical grade；Sodium carbonate：99% content, technical grade；Dilute sulfuric acid is prepared：98% concentrated sulfuric 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 conversion：One ton of phosphoric acid lithium powder is added to and fills 1.5m3The pp materials of the dilute sulfuric acid that above-mentioned steps are prepared
Conversion 30 minutes is stirred in matter agitator, is then filtered by vacuum suction filter disk, filter residue and filtrate split standby；
（3）, lithium sulfate feed liquid produces：By step（2）The filter residue of generation is put into the pp material stirrings bucket with stirring, is added
1.5 m3Clear water dissolves, and then uses step（1）40% sodium hydroxide solution adjustment pH >=7 prepared, stir 30 minutes, Ran Houtong
Plate and frame filter press filtering is crossed, filter residue is lithium phosphate, and dry for standby, filtrate stores for future use；
（4）, lithium carbonate produces：By step（3）The filtrate of generation is added in the stainless steel cask with stirring, is heated to >=70
DEG C, then the solid sodium carbonate insulated and stirred of 8~10 times of weight of input lithium content quality 30-60 minutes uses vacuum suction filter disk
Filtering, filter residue use >=70 DEG C hot water is washed twice on suction strainer disk, and drying and packaging is product lithium carbonate, and precipitation filtrates storage is standby
With cleaning solution discharge.
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| CN106241838B true CN106241838B (en) | 2017-07-07 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019227157A1 (en) * | 2018-05-30 | 2019-12-05 | Lithium Australia Nl | Process for recovering lithium values |
| CN108862335B (en) * | 2018-07-20 | 2021-04-23 | 上海中锂实业有限公司 | Method for preparing lithium carbonate from 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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| CN100469697C (en) * | 2007-08-21 | 2009-03-18 | 四川天齐锂业股份有限公司 | Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution |
| KR101238890B1 (en) * | 2010-08-10 | 2013-03-04 | 재단법인 포항산업과학연구원 | Production method of lithium carbonate from brines |
| KR101126286B1 (en) * | 2010-08-12 | 2012-03-20 | 재단법인 포항산업과학연구원 | Manufacturing method of lithium carbonate with high purity |
| JP5406822B2 (en) * | 2010-11-30 | 2014-02-05 | 日鉄鉱業株式会社 | Method for producing lithium carbonate |
| CN103408041B (en) * | 2013-08-22 | 2015-08-05 | 四川国理锂材料有限公司 | The production technique of Quilonum Retard |
| CN103950956B (en) * | 2014-05-22 | 2015-10-14 | 甘孜州泸兴锂业有限公司 | A kind of triphane concentrate Production By Sulfuric Acid Process Quilonum Retard technique |
| CN105502441B (en) * | 2016-01-14 | 2017-05-24 | 天齐锂业股份有限公司 | Method for continuously producing cell-grade lithium carbonate |
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