CN106745099A - A kind of method that utilization lithium phosphate prepares lithium carbonate - Google Patents
A kind of method that utilization lithium phosphate prepares lithium carbonate Download PDFInfo
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- CN106745099A CN106745099A CN201611099570.6A CN201611099570A CN106745099A CN 106745099 A CN106745099 A CN 106745099A CN 201611099570 A CN201611099570 A CN 201611099570A CN 106745099 A CN106745099 A CN 106745099A
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- lithium
- solution
- phosphate
- lithium phosphate
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a kind of method that utilization lithium phosphate prepares lithium carbonate.The technical scheme that the method is used is：Cleaning-dissolving-removal of impurities-sinker-propose phosphorus-recovery.In process of production, elemental lithium is recycled, loss less, high income, the lithium carbonate purity of output is high, quality better, can reach LITHIUM BATTERY.The present invention largely using the chemical spent material lithium phosphate for having harm can either can produce the lithium carbonate of market in urgent need again.
Description
Technical field
The present invention relates to a kind of method that utilization lithium phosphate prepares lithium carbonate.
Background technology
With the development of lithium battery new-energy automobile, the value of lithium is redefined, and the price of lithium carbonate also skyrockets all the way.
The chemical spent material that this allows for that a part of amount containing lithium is low, be difficult extraction is taken seriously, among these just comprising lithium phosphate.Lithium phosphate
With certain toxicity, if not being utilized and consuming, its long-time storage also has certain danger.In addition, lithium phosphate is difficult
Water is dissolved in, cause makes it difficult to be used directly.At present, only there is a small amount of application in industries such as medicine, catalyst and test reagents,
It can be seen that, industrialized utilization lithium phosphate is very necessary.
The content of the invention
The invention provides a kind of method that utilization lithium phosphate prepares lithium carbonate, can either largely using the chemical industry for having harm
Waste material lithium phosphate, can produce the lithium carbonate of market in urgent need again.
In order to reach the effect above, the method that a kind of utilization lithium phosphate that the present invention is provided prepares lithium carbonate, methods described
Comprise the following steps:
Cleaning：Lithium phosphate is added to the water, cleaning removal Na, K, Cl etc. are dissolved in the impurity of water；
Dissolving：In to addition watery hydrochloric acid in the lithium phosphate after cleaning, and being stirred continuously dissolves the lithium phosphate, Gu
Liquid is separated, and obtains saturation lithium-containing solution；
Removal of impurities：The lithium-containing solution is heated to 80 DEG C, and adds appropriate saturation NaOH solution, in the removal solution
Mg, Fe, Cu impurity, separation of solid and liquid obtain mother liquor containing lithium；
Sinker：The mother liquor containing lithium is heated to 80-100 DEG C, and adds 80-100 DEG C of Na2CO4Solution, obtains carbonic acid
Lithium is precipitated, and is separated by filtration and is obtained lithium carbonate and sinker filtrate；
Carry phosphorus：The filtrate heating of heating sinker, adds CaCl2Solution, then use Na2CO3Solution tone pitch, generation calcium monohydrogen phosphate sinks
Form sediment, by precipitate and separate and wash with water, obtain calcium monohydrogen phosphate finished product；
And
Reclaim：Phosphoric acid is added to the solution carried after phosphorus, remaining lithium in solution is precipitated in the form of lithium phosphate, solid-liquid point
From obtaining lithium phosphate.
Preferably, 50-100 DEG C of the water temperature, wash number is 1-3 times.
Preferably, the percentage of the watery hydrochloric acid is 5%-20%.
Preferably, the heating-up temperature of the sinker filtrate is 40-60 DEG C.
The invention has the advantages that：
1. in production process of the present invention, elemental lithium is recycled, loss less, high income.
2. byproduct phosphoric acid hydrogen calcium purity is high, is not required to purify processing again, may be directly applied to other industry.
3. lithium carbonate purity is high, quality better, can reach LITHIUM BATTERY.
4. technical process uses reactive liquid solution, and course of reaction is easily controllable, and product is easily isolated.
5. production equipment does not use pressure apparatus, safe and stable.
Specific embodiment
With reference to production instance, the invention will be further elaborated.
Practical application technical scheme of the invention is：Cleaning-dissolving-removal of impurities-sinker-propose phosphorus-recovery
Step one：Cleaning：120Kg lithium phosphates are added into 1m3In water, 60 DEG C of water temperature is gradually heated to, heated while stirring,
Then upper liquid is separated, removes the impurity such as Na, K, Cl soluble in water.Add 1m3Water carries out second cleaning, will be big
It is partially soluble in the Impurity removal of water.
Step 2：Dissolving：To being slowly added to 1m in the lithium phosphate after cleaning310% watery hydrochloric acid, and be stirred continuously, until
Lithium phosphate all dissolves, and obtains lithium-containing solution.
Step 3：Removal of impurities：Lithium-containing solution is heated to 80 DEG C, and adds appropriate saturation NaOH solution, make Mg in solution,
The impurity such as Fe, Cu react generation sediment.Removal sediment, obtains mother liquor containing lithium.
Step 4：Sinker：Lithium mother liquor will be contained and be heated to 90 DEG C, be slowly added to 0.8m3Na2CO3Solution (Na2CO4Solution by
220Kg sodium carbonate and 1m3Water normal-temperature dissolution is formed), stir while adding, obtain lithium carbonate precipitation.It is separated by filtration and obtains about
220Kg lithium carbonates, lithium carbonate product is turned into through drying, crushing, packaging.
Step 5：Carry phosphorus：Filtrate after sinker is heated to 55 DEG C, CaCl is added2Solution, then use Na2CO3Solution tone pitch,
Generation calcium monohydrogen phosphate precipitation.By precipitate and separate and wash with water, obtain about 170Kg calcium monohydrogen phosphate finished products.
Step 6：Reclaim：Phosphoric acid is added to the solution carried after phosphorus, by remaining lithium in solution with precipitation in the form of lithium phosphate
Come, separation of solid and liquid obtains lithium phosphate, participate in production process next time.
The above is specific produce reality of the invention, it is noted that the invention is not restricted to disclosed embodiment,
Conversely, it is contemplated that covering the various modifications and equivalents included in Claims scope.Therefore, the embodiment above
It is exemplary, the present invention is limited never in any form.
Claims (4)
1. a kind of method that utilization lithium phosphate prepares lithium carbonate, it is characterised in that：The described method comprises the following steps:
Cleaning：Lithium phosphate is added to the water, cleaning removal Na, K, Cl etc. are dissolved in the impurity of water；
Dissolving：In to addition watery hydrochloric acid in the lithium phosphate after cleaning, and being stirred continuously dissolves the lithium phosphate, solid-liquid point
From obtaining saturation lithium-containing solution；
Removal of impurities：The lithium-containing solution is heated to 80 DEG C, and adds appropriate saturation NaOH solution, remove Mg in the solution, Fe,
Cu impurity, separation of solid and liquid obtains mother liquor containing lithium；
Sinker：The mother liquor containing lithium is heated to 80-100 DEG C, and adds 80-100 DEG C of Na2CO3Solution, obtains lithium carbonate and sinks
Form sediment, be separated by filtration and obtain lithium carbonate；
Carry phosphorus：Heating sinker filtrate, adds CaCl2Solution, then use Na2CO3Solution tone pitch, generation calcium monohydrogen phosphate precipitation, will precipitate
Separate and wash with water, obtain calcium monohydrogen phosphate finished product；
And
Reclaim：Phosphoric acid is added to the solution carried after phosphorus, remaining lithium in solution is precipitated in the form of lithium phosphate, separation of solid and liquid is obtained
To lithium phosphate.
2. the method for claim 1, it is characterised in that 50-100 DEG C of the water temperature, wash number is 1-3 times.
3. the method for claim 1, it is characterised in that the percentage of the watery hydrochloric acid is 5%-20%.
4. the method for claim 1, it is characterised in that the heating-up temperature of the sinker filtrate is 40-60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611099570.6A CN106745099A (en) | 2016-12-05 | 2016-12-05 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611099570.6A CN106745099A (en) | 2016-12-05 | 2016-12-05 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
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| Publication Number | Publication Date |
|---|---|
| CN106745099A true CN106745099A (en) | 2017-05-31 |
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| CN201611099570.6A Withdrawn CN106745099A (en) | 2016-12-05 | 2016-12-05 | A kind of method that utilization lithium phosphate prepares lithium carbonate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108155434A (en) * | 2017-12-25 | 2018-06-12 | 中南大学 | A kind of method that lithium is recycled in the waste electrolyte from lithium ion battery |
| 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 |
| CN110759364A (en) * | 2019-11-13 | 2020-02-07 | 江西金辉锂业有限公司 | Method for preparing high-purity lithium carbonate by using crude lithium phosphate |
| CN111153419A (en) * | 2018-11-07 | 2020-05-15 | 全雄 | Method for extracting lithium |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
| US11821056B2 (en) | 2020-01-29 | 2023-11-21 | Uong CHON | Lithium extraction method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445730A (en) * | 2014-11-21 | 2015-03-25 | 贵阳中化开磷化肥有限公司 | Comprehensive utilization method of wastewater containing phosphorus and fluorine |
| CN104745823A (en) * | 2015-03-12 | 2015-07-01 | 湖南邦普循环科技有限公司 | Method for recycling lithium from waste lithium ion battery |
-
2016
- 2016-12-05 CN CN201611099570.6A patent/CN106745099A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445730A (en) * | 2014-11-21 | 2015-03-25 | 贵阳中化开磷化肥有限公司 | Comprehensive utilization method of wastewater containing phosphorus and fluorine |
| CN104745823A (en) * | 2015-03-12 | 2015-07-01 | 湖南邦普循环科技有限公司 | Method for recycling lithium from waste lithium ion battery |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108155434A (en) * | 2017-12-25 | 2018-06-12 | 中南大学 | A kind of method that lithium is recycled in the waste electrolyte from lithium ion battery |
| CN111153419A (en) * | 2018-11-07 | 2020-05-15 | 全雄 | Method for extracting lithium |
| CN111153419B (en) * | 2018-11-07 | 2022-08-09 | 全雄 | Method for extracting lithium |
| 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 |
| CN110316747B (en) * | 2019-07-25 | 2022-03-11 | 湖南邦普循环科技有限公司 | Method for comprehensively recovering lithium and phosphorus from lithium phosphate |
| CN110759364A (en) * | 2019-11-13 | 2020-02-07 | 江西金辉锂业有限公司 | Method for preparing high-purity lithium carbonate by using crude lithium phosphate |
| US11821056B2 (en) | 2020-01-29 | 2023-11-21 | Uong CHON | Lithium extraction method |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
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Application publication date: 20170531 |