CN101481125A - Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate - Google Patents
Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate Download PDFInfo
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- CN101481125A CN101481125A CNA200910024433XA CN200910024433A CN101481125A CN 101481125 A CN101481125 A CN 101481125A CN A200910024433X A CNA200910024433X A CN A200910024433XA CN 200910024433 A CN200910024433 A CN 200910024433A CN 101481125 A CN101481125 A CN 101481125A
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- sodium carbonate
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Abstract
The invention discloses a method for producing lithium carbonate by circularly applying mother solution from which lithium is subsided to prepare a sodium carbonate solution, which comprises the sequential steps such as refrigerating the mother solution from which lithium is subsided, filtering the mother solution from which sodium is sought out, heating the purified liquid of the mother solution from which the sodium is sought out, sweating out the mother solution to prepare the sodium carbonate solution, and performing reaction of the sodium carbonate solution with the lithium sulfate solution so that lithium is subsided. The invention has the characteristics of high lithium sedimentation efficiency, simple technique, stable product, high production efficiency, high recovery rate, low consumption of sodium carbonate, low energy consumption and low cost.
Description
Technical field:
The present invention relates to a kind of method that the sinker Recycling Mother Solution is used to join sodium carbonate solution production Quilonum Retard.
Background technology:
Lithium is a scarce resource, and the compound of lithium and lithium but is extensive use of by growing field, how to utilize lithium resource fully, and also taking into account energy-saving and cost-reducing simultaneously is enterprise and social questions of common interest.
Traditional Production By Sulfuric Acid Process Quilonum Retard, technology liquid amount balance are the key issues that solves the lithium rate of recovery.The liquid measure imbalance, the water yield of band lithium runs off manyly, and the loss of lithium is also many; The water yield round-robin route of band lithium is long more, and the loss of lithium is also big more.So the Production By Sulfuric Acid Process Quilonum Retard, solving sinker mother liquor problem is one of key of Technology.
Traditional method the earliest is that the sinker mother liquor adds sulfuric acid earlier and neutralizes, and then evaporation concentration isolates sodium sulfate, and mother liquor goes back to the lithium system of soaking.This also is the sinker mother liquor processing method that is nowadays adopted by most of enterprise.
The method of improvement is that the sinker mother liquor is earlier freezing, isolates sal glauberi then, again mother liquor is carried out evaporation concentration and isolates Quilonum Retard, and mother liquor carries out freezing again, so self-circulation.This method is used for reference by part in the monohydrate lithium hydroxide production technology.The only indivedual enterprises of this method adopt.
The treatment process of the sinker mother liquor that small part producer adopts is: the freezing sodium sulfate of separating out of elder generation, and mother liquor separated into two parts is again walked, and major part is added to and participates in the leach liquor purifying leach liquor and then evaporation concentration, and another part soaks the lithium system to the ore deposit.This processing mode steam consumption quantity is equally very big, and gets back to the ore deposit and soak the part of lithium system makes lithium owing to circulation route is long loss increase.
Summary of the invention:
The object of the present invention is to provide a kind of method simple, that sodium carbonate solution production Quilonum Retard is joined in high, the energy-conservation sinker Recycling Mother Solution is used to of the rate of recovery of producing.
Technical solution of the present invention is:
A kind of the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: comprise the following steps: successively
(1) sinker mother liquor freezing treatment: the sinker mother liquor is separated out ten current acid sodium by freezing reduction temperature, and centrifugation is sal glauberi and analyses mother liquid of sodium then;
Reaction principle: 2Na
++ SO
4 2-+ 10H
2O → Na
2SO
410H
2O ↓
(2) analyse the mother liquid of sodium filtration treatment: analyse mother liquid of sodium and carry out filtration treatment and remove solid impurity, must analyse the mother liquid of sodium scavenging solution;
(3) analysing the mother liquid of sodium scavenging solution heats up and analyses lithium: analyse the mother liquid of sodium scavenging solution and separate out most of Quilonum Retard through intensification, carry out solid-liquid separation then and get Quilonum Retard and sweat mother liquor;
Reaction principle: Li
++ CO
3 2-→ Li
2CO
3↓
(4) sweat mother liquor preparation sodium carbonate solution: in the sweat mother liquor, drop into the yellow soda ash solid and fully dissolve after-filtration, get sodium carbonate solution;
(5) sodium carbonate solution and lithium sulfate solution reaction sinker: lithium sulfate solution is joined reaction generation Quilonum Retard in the sodium carbonate solution, get Quilonum Retard and sinker mother liquor then after the solid-liquid separation, the sinker mother liquor that obtains recycles repeatedly.
Reaction principle: Li
++ CO
3 2-→ Li
2CO
3↓
Have in the step (4) and join the surplus mother liquid of sodium of analysing that goes out of sodium carbonate solution and go back to the purification of leaching liquor system, be used to remove wherein calcium, magnesium, iron ion.
Freezing temp in the step (1) during sinker mother liquor freezing treatment be-5～6 ℃, controls and analyses mother liquor SO behind the sodium
4 2-＜60g/L.
Temperature when analysing the hyperthermic treatment of mother liquid of sodium scavenging solution in the step (3) is 80-100 ℃, and is incubated 5-30 minute, mother liquor Li after the control sweat
2O content＜6g/L.
When dropping into the yellow soda ash solid in the step (4) in the sweat mother liquor, the temperature of sweat mother liquor is 70-100 ℃, behind the input yellow soda ash solid, is incubated 20～50 minutes with abundant dissolving down in 70-100 ℃; Sodium carbonate solution control concentration of sodium carbonate is at 230～320g/L.
The sweat mother liquor contains Li before adding yellow soda ash
2O amount is at≤6.0g/L, adds after yellow soda ash becomes sodium carbonate solution solution Li
2O content will descend to some extent.Reason is because after the sweat mother liquor is made into sodium carbonate solution, liquor capacity will increase about 10%, so in being made into the process of sodium carbonate solution, the lithium ion in the former sweat mother liquor generally can not separated out again, but all be dissolved in the sodium carbonate solution, this moment sodium carbonate solution Li
2CO
3Near the saturated solution state.
When lithium sulfate solution joined in the sodium carbonate solution in the step (5), the temperature of sodium carbonate solution was 90-100 ℃.
The present invention is to the processing of sinker mother liquor, adopt first subzero fractionation to go out sal glauberi, again the mother liquor of analysing behind the sodium is carried out solids removed by filtration impurity, heat up then and separate out Quilonum Retard, solid-liquid separation goes out Quilonum Retard and sweat mother liquor, and the sweat mother liquor is used for joining sodium carbonate solution, and then in order to carry out sinker, the freezing again sodium of analysing of mother liquor behind the sinker, so circulation.Join the sodium carbonate solution mother liquid of sodium of analysing more than needed on a small quantity and be used for adding to advance in the leach liquor, be used for removing calcium, magnesium, the iron of leach liquor, play purification function.Not only reduced energy consumption thus, reclaimed the yellow soda ash of remnants in the mother liquor, shortened sinker Recycling Mother Solution route (being water circulation line) again, also saved former preparation sodium carbonate solution required water simultaneously fully, improve the system-wide liquid amount balance of whole production greatly, and the Quilonum Retard quality grade of producing can reach the battery-level lithium carbonate technical requirements fully.
The present invention utilizes the sinker mother liquor dexterously, analysing mother liquid of sodium adopts and to be used for joining sodium carbonate solution after the sweat again, avoided can separating out Quilonum Retard behind the adding yellow soda ash and entered in the slag, the Quilonum Retard that sweat simultaneously obtains also is the good Quilonum Retard of purity, and the sodium carbonate solution that the sweat mother liquor is made into is Li
2CO
3Saturated solution, when adding the lithium sulfate solution sinker of measuring together, the sinker rate can be improved relatively.Add that sweat also can obtain some Quilonum Retards, so total sinker rate can be greatly improved, and remaining yellow soda ash also is fully used in the mother liquor, the short loss of Recycling Mother Solution route is few, having only seldom, a part enters the purification of leaching liquor system, by the evaporation amount seldom, so steam consumption quantity reduces greatly comparatively speaking.In a word, the present invention has sinker rate height, technology is simple, product is stable, production efficiency is high, the rate of recovery is high, yellow soda ash consumes the characteristics low, that energy consumption is low, cost is low.
The invention will be further described below in conjunction with embodiment.
Embodiment:
Embodiment 1:
Present embodiment comprises the steps:
1. 3500L sinker mother liquor is refrigerated to-3 ℃, carries out centrifugation then and go out ten current acid sodium, must analyse mother liquid of sodium, record and analyse mother liquid of sodium SO
4 2-Content is 26g/L;
2. carry out press filtration analysing mother liquid of sodium, remove the solid dregs;
3. the mother liquid of sodium of analysing after filtering is warming up to 95 ℃, and is incubated 15 minutes, separate out Quilonum Retard.Isolate Quilonum Retard and sweat mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
4. get 550 kilograms of yellow soda ash and fully be dissolved in the 1900L sweat mother liquor, filter then, get sodium carbonate solution 2000L, recording the sodium carbonate solution concentration of sodium carbonate is 290g/L;
5. there is a small amount of surplus sweat mother liquor that goes out to go to the purification of leaching liquor system;
6. sodium carbonate solution is warmed up to 90 ℃, and to keep about 90 ℃ slowly adding the 2600L oxide containing lithium be the lithium sulfate solution of 60g/L, centrifugation goes out Quilonum Retard and sinker mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
7. the sinker mother liquor circulates again and is used to join sodium carbonate solution through freezing after analysing the sodium sweat, circulation so repeatedly.
Get 360 kilograms of lithium carbonate products after sweat Quilonum Retard and Lithium Sulphate sinker Quilonum Retard are dried together, record lithium carbonate product: Na
+Be 0.017%, SO
4 2-Be 0.054%.
Embodiment 2:
Present embodiment comprises the steps:
1. 3500L sinker mother liquor is refrigerated to 6 ℃, carries out centrifugation then and go out ten current acid sodium, must analyse mother liquid of sodium, record and analyse mother liquid of sodium SO
4 2-Content is 58g/L;
2. carry out press filtration analysing mother liquid of sodium, remove the solid dregs;
3. the mother liquid of sodium of analysing after filtering is warming up to 98 ℃, and is incubated 10 minutes, separate out Quilonum Retard.Isolate Quilonum Retard and sweat mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
4. get 500 kilograms of yellow soda ash and fully be dissolved in the 1900L sweat mother liquor, filter then, get sodium carbonate solution 2000L, recording the sodium carbonate solution concentration of sodium carbonate is 260g/L;
5. a small amount of surplus sweat mother liquor that goes out goes to the purification of leaching liquor system;
6. sodium carbonate solution is warmed up to 95 ℃, and to keep about 95 ℃ slowly adding the 2400L oxide containing lithium be the lithium sulfate solution of 58g/L, centrifugation goes out Quilonum Retard and sinker mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
7. the sinker mother liquor circulates again and is used to join sodium carbonate solution through freezing after analysing the sodium sweat, circulation repeatedly.
Get 319 kilograms of lithium carbonate products after sweat Quilonum Retard and Lithium Sulphate sinker Quilonum Retard are dried together, record lithium carbonate product: Na
+Be 0.018%, SO
4 2-Be 0.055%.
Embodiment 3:
Present embodiment comprises the steps:
1. 3500L sinker mother liquor is refrigerated to 4 ℃, carries out centrifugation then and go out ten current acid sodium, must analyse mother liquid of sodium, record and analyse mother liquid of sodium SO
4 2-Content is 40g/L;
2. carry out press filtration analysing mother liquid of sodium, remove the solid dregs;
3. the mother liquid of sodium of analysing after filtering is warming up to 100 ℃, and is incubated 5 minutes, separate out Quilonum Retard.Isolate Quilonum Retard and sweat mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
4. get 450 kilograms of yellow soda ash and fully be dissolved in the 1900L sweat mother liquor, filter then, get sodium carbonate solution 2000L, recording the sodium carbonate solution concentration of sodium carbonate is 240g/L;
5. a small amount of surplus sweat mother liquor that goes out goes to the purification of leaching liquor system;
6. sodium carbonate solution is warmed up to 100 ℃, and keeping 95-100 ℃, slowly to add the 2000L oxide containing lithium be the lithium sulfate solution of 64g/L, centrifugation goes out Quilonum Retard and sinker mother liquor then, and to Quilonum Retard with a small amount of water of condensation drip washing;
7. the sinker mother liquor circulates again and is used to join sodium carbonate solution through freezing after analysing the sodium sweat, circulation repeatedly.
Get 290 kilograms of lithium carbonate products after sweat Quilonum Retard and Lithium Sulphate sinker Quilonum Retard are dried together, record lithium carbonate product: Na
+Be 0.017%, SO
4 2-Be 0.056%.
Claims (6)
1, a kind of the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: comprise the following steps: successively
(1) sinker mother liquor freezing treatment: the sinker mother liquor is separated out ten current acid sodium by freezing reduction temperature, and centrifugation is sal glauberi and analyses mother liquid of sodium then;
(2) analyse the mother liquid of sodium filtration treatment: analyse mother liquid of sodium and carry out filtration treatment and remove solid impurity, must analyse the mother liquid of sodium scavenging solution;
(3) analysing the mother liquid of sodium scavenging solution heats up and analyses lithium: analyse the mother liquid of sodium scavenging solution and separate out Quilonum Retard through intensification, carry out solid-liquid separation then and get Quilonum Retard and sweat mother liquor;
(4) sweat mother liquor preparation sodium carbonate solution: in the sweat mother liquor, drop into the yellow soda ash solid and fully dissolve after-filtration, get sodium carbonate solution;
(5) sodium carbonate solution and lithium sulfate solution reaction sinker: lithium sulfate solution is joined reaction generation Quilonum Retard in the sodium carbonate solution, get Quilonum Retard and sinker mother liquor then after the solid-liquid separation, the sinker mother liquor that obtains recycles repeatedly.
2, according to claim 1 the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: have in the step (4) and join the surplus mother liquid of sodium of analysing that goes out of sodium carbonate solution and go back to the purification of leaching liquor system.
3, according to claim 1 and 2 the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: the freezing temp in the step (1) during sinker mother liquor freezing treatment is-5～6 ℃.
4, according to claim 1 and 2 the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: the temperature when analysing the hyperthermic treatment of mother liquid of sodium scavenging solution in the step (3) is 80-100 ℃, and insulation 5-30 minute.
5, the method that the sinker Recycling Mother Solution is used to join sodium carbonate solution production Quilonum Retard according to claim 1 and 2, it is characterized in that: when in the sweat mother liquor, dropping into the yellow soda ash solid in the step (4), the temperature of sweat mother liquor is 70-100 ℃, and sodium carbonate solution control concentration of sodium carbonate is at 230～320g/L.
6, according to claim 1 and 2 the sinker Recycling Mother Solution is used to join the method that sodium carbonate solution is produced Quilonum Retard, it is characterized in that: when lithium sulfate solution joined in the sodium carbonate solution in the step (5), the temperature of sodium carbonate solution was 90-100 ℃.
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| CN101481125B CN101481125B (en) | 2011-05-04 |
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|---|---|---|---|---|
| CN102491378A (en) * | 2011-10-14 | 2012-06-13 | 陈兆华 | Producing method for preparing lithium carbonate by taking carbonate type brine and sulphate type brine as raw material and by repeatedly mixing brine |
| CN103318925A (en) * | 2013-06-19 | 2013-09-25 | 海门容汇通用锂业有限公司 | Method for producing high-purity lithium carbonate by using lithium concentrate |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| CN103787374A (en) * | 2012-10-31 | 2014-05-14 | 西藏国能矿业发展有限公司 | Method for extracting lithium carbonate from salt lake bittern |
| CN103964474A (en) * | 2014-05-22 | 2014-08-06 | 甘孜州泸兴锂业有限公司 | Method for recovering lithium in mother liquor of process for producing lithium carbonate from spodumene through sulfuric acid process |
| CN104310430A (en) * | 2014-09-30 | 2015-01-28 | 甘孜州泸兴锂业有限公司 | Impurity removal method for lithium hydroxide preparation process |
| CN106517259A (en) * | 2016-12-19 | 2017-03-22 | 天齐锂业股份有限公司 | Spherical lithium carbonate and preparation method thereof |
| CN106882822A (en) * | 2017-03-15 | 2017-06-23 | 江苏容汇通用锂业股份有限公司 | A kind of method that lithium is recycled into battery-level lithium carbonate in sinker mother liquor |
| CN109576499A (en) * | 2019-01-30 | 2019-04-05 | 广东省稀有金属研究所 | A method of recycling lithium from battery electrode material leachate |
| CN110040750A (en) * | 2019-04-26 | 2019-07-23 | 核工业北京化工冶金研究院 | A kind of processing method of lithium carbonate mother liquor of precipitation of ammonium |
| CN112978769A (en) * | 2021-05-08 | 2021-06-18 | 雅化锂业(雅安)有限公司 | Method for removing potassium from anhydrous sodium sulfate in lithium hydroxide production |
| CN113120931A (en) * | 2019-12-30 | 2021-07-16 | 中核北方核燃料元件有限公司 | Nuclear pure grade Li2CO3Chemical conversion device |
| CN113716587A (en) * | 2021-09-07 | 2021-11-30 | 江苏容汇通用锂业股份有限公司 | Preparation method of lithium fluoride with high lithium yield |
| CN113800541A (en) * | 2021-11-08 | 2021-12-17 | 江苏瑞达环保科技有限公司 | Processing technology for refining lithium chloride by lithium carbonate precipitation and conversion |
| CN115744942A (en) * | 2022-11-28 | 2023-03-07 | 江西永兴特钢新能源科技有限公司 | Method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor |
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2009
- 2009-02-13 CN CN200910024433XA patent/CN101481125B/en active Active
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| CN102491378A (en) * | 2011-10-14 | 2012-06-13 | 陈兆华 | Producing method for preparing lithium carbonate by taking carbonate type brine and sulphate type brine as raw material and by repeatedly mixing brine |
| CN103787374A (en) * | 2012-10-31 | 2014-05-14 | 西藏国能矿业发展有限公司 | Method for extracting lithium carbonate from salt lake bittern |
| CN103787374B (en) * | 2012-10-31 | 2015-05-06 | 西藏国能矿业发展有限公司 | Method for extracting lithium carbonate from salt lake bittern |
| CN103318925A (en) * | 2013-06-19 | 2013-09-25 | 海门容汇通用锂业有限公司 | Method for producing high-purity lithium carbonate by using lithium concentrate |
| CN103318925B (en) * | 2013-06-19 | 2015-01-21 | 海门容汇通用锂业有限公司 | Method for producing high-purity lithium carbonate by using lithium concentrate |
| CN103408041A (en) * | 2013-08-22 | 2013-11-27 | 四川国理锂材料有限公司 | Lithium carbonate production technology |
| 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 |
| CN103964474A (en) * | 2014-05-22 | 2014-08-06 | 甘孜州泸兴锂业有限公司 | Method for recovering lithium in mother liquor of process for producing lithium carbonate from spodumene through sulfuric acid process |
| CN104310430A (en) * | 2014-09-30 | 2015-01-28 | 甘孜州泸兴锂业有限公司 | Impurity removal method for lithium hydroxide preparation process |
| CN106517259B (en) * | 2016-12-19 | 2018-07-10 | 天齐锂业股份有限公司 | A kind of spherical Lithii carbonate and preparation method thereof |
| CN106517259A (en) * | 2016-12-19 | 2017-03-22 | 天齐锂业股份有限公司 | Spherical lithium carbonate and preparation method thereof |
| CN106882822A (en) * | 2017-03-15 | 2017-06-23 | 江苏容汇通用锂业股份有限公司 | A kind of method that lithium is recycled into battery-level lithium carbonate in sinker mother liquor |
| CN109576499A (en) * | 2019-01-30 | 2019-04-05 | 广东省稀有金属研究所 | A method of recycling lithium from battery electrode material leachate |
| CN110040750A (en) * | 2019-04-26 | 2019-07-23 | 核工业北京化工冶金研究院 | A kind of processing method of lithium carbonate mother liquor of precipitation of ammonium |
| CN110040750B (en) * | 2019-04-26 | 2021-10-22 | 核工业北京化工冶金研究院 | Method for treating lithium carbonate precipitation mother liquor |
| CN113120931A (en) * | 2019-12-30 | 2021-07-16 | 中核北方核燃料元件有限公司 | Nuclear pure grade Li2CO3Chemical conversion device |
| CN112978769A (en) * | 2021-05-08 | 2021-06-18 | 雅化锂业(雅安)有限公司 | Method for removing potassium from anhydrous sodium sulfate in lithium hydroxide production |
| CN113716587A (en) * | 2021-09-07 | 2021-11-30 | 江苏容汇通用锂业股份有限公司 | Preparation method of lithium fluoride with high lithium yield |
| CN113800541A (en) * | 2021-11-08 | 2021-12-17 | 江苏瑞达环保科技有限公司 | Processing technology for refining lithium chloride by lithium carbonate precipitation and conversion |
| CN115744942A (en) * | 2022-11-28 | 2023-03-07 | 江西永兴特钢新能源科技有限公司 | Method for removing lepidolite leaching brine impurities by using lithium precipitation mother liquor |
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Address after: 226121 Haimen Jiangsu three factory town street, Daqing Road, No. 42 Patentee after: JIANGSU RONGHUI GENERAL LITHIUM INDUSTRY CO., LTD. Address before: 226121 Haimen North Road, three factory town, Haimen, Jiangsu Province, Daqing Patentee before: Haimen Ronghui General Lithium Co., Ltd. |