CN1109104A - Manufacture of lithium hydroxide from lithionite and lime stone by sintering - Google Patents
Manufacture of lithium hydroxide from lithionite and lime stone by sintering Download PDFInfo
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- CN1109104A CN1109104A CN94113302A CN94113302A CN1109104A CN 1109104 A CN1109104 A CN 1109104A CN 94113302 A CN94113302 A CN 94113302A CN 94113302 A CN94113302 A CN 94113302A CN 1109104 A CN1109104 A CN 1109104A
- Authority
- CN
- China
- Prior art keywords
- lithium hydroxide
- lithionite
- processing method
- roasting
- crystallization
- Prior art date
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- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 title claims abstract description 111
- 235000019738 Limestone Nutrition 0.000 title abstract description 9
- 239000006028 limestone Substances 0.000 title abstract description 9
- 238000005245 sintering Methods 0.000 title abstract description 9
- 238000004519 manufacturing process Methods 0.000 title description 11
- 238000000034 method Methods 0.000 claims abstract description 24
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 14
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 14
- 239000004571 lime Substances 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 13
- 230000008020 evaporation Effects 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000002425 crystallisation Methods 0.000 claims description 19
- 230000008025 crystallization Effects 0.000 claims description 19
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 16
- 239000000920 calcium hydroxide Substances 0.000 claims description 16
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 16
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 13
- 238000003672 processing method Methods 0.000 claims description 11
- 239000012452 mother liquor Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 4
- 238000002386 leaching Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N lithium oxide Chemical compound [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 3
- 229910001947 lithium oxide Inorganic materials 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims 1
- 238000004886 process control Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000029087 digestion Effects 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 2
- 229910052629 lepidolite Inorganic materials 0.000 abstract 4
- 239000000047 product Substances 0.000 description 12
- 239000002893 slag Substances 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 6
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 229910052792 caesium Inorganic materials 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 229910052701 rubidium Inorganic materials 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- -1 aluminum ion Chemical class 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The process for producing lithium hydroxide by sintering lepidolite and lime stone as raw materials includes high-temp. sintering lepidolite under existant steam, pressure digestion of ground sintered lepidolite, lime, returned partial mother liquid and liquid after washing dregs for dissolving, removing impurities from solution, and evaporation crystalline, and features less consumption of lime stone and energy, high decomposing rate of lepidolite, high recovery rate, and low cost.
Description
The present invention relates to a kind of is the processing method of raw material production lithium hydroxide with roasting lithionite and lime.
With the lithionite ore is the raw material production lithium hydroxide, has the people once to study directly and presses the method for boiling lithionite with lime, and it is levigate 200 orders that reach of lithionite, directly adds the water adding calcium hydroxide and presses in autoclave and boil lithionite: Ca(OH)
2: water=1:1.8: 10, temperature is 240 ℃-260 ℃, and pressure is 2.8MPa, reacts 4 hours, and rate of decomposition can reach 95%.But this method amount of lime is big, and energy-saving effect is not remarkable, presses and boils the temperature height, pressure height, high pressure leaching plant system cost height.Especially scab in the still, body refuse expands, and so the separating, washing difficulty is industrial being difficult to carry out.
It is at present industrial that what adopt is the limestone sintering method, this method is pressed lithionite: Wingdale=1:3 wet-milling of preparing burden, be milled down to-160 orders, slip is moisture about 36%, goes into rotary kiln sinteredly, and rate of decomposition is about 81%, again through the wet-milling stripping, after the removal of impurities, separate out the lithium hydroxide product through evaporative crystallization, its technical process as shown in Figure 1.Simple, cheap, the wide material sources of this method raw material, production process is simple.But it exists Wingdale proportioning height, need in rotary kiln, decompose a large amount of Wingdale (1 ton of product of every production need decompose about 40 tons) energy consumption height, mass flow is big, equipment capacity low (2.07 * 45 meters rotary kiln products of φ meter production capacity is 800 tons/year), the quantity of slag big (42 tons of slag/ton products), the low problems such as (about 67%) of the rate of recovery.
What the invention provides that a kind of amount of lime is few, energy consumption is low, the quantity of slag is few, the rate of recovery significantly improves is the processing method of raw material production lithium hydroxide with roasting lithionite and lime.
The present invention is achieved in that the processing method of producing lithium hydroxide with roasting lithionite and lime, and it is a raw material with lithionite and Wingdale only, earlier lithionite is carried out roasting in the presence of high temperature and steam and becomes the roasting lithionite; Wingdale becomes lime to be digested to slaked lime again through calcination; Partial mother liquid, the residue wash water of levigated roasting lithionite after slaked lime, the lithium hydroxide crystallization returned are separated out pressed boil stripping, this process need be controlled concentration of potassium hydroxide, the control liquid-solid ratio is (2-6): 1, temperature is 80-180 ℃, under constantly stirring, reacted 0.5-7 hour, lithionite is decomposed, wherein Lithium Oxide 98min is become the lithium hydroxide stripping; Dissolution fluid removes carbonate with slaked lime, and except that behind the aluminium, lithium hydroxide is separated out in the multi-stage evaporation crystallization of carrying out returning with lithium hydroxide; Through washing, dry qualified lithium hydroxide product.Its technical process such as Fig. 2 show.
With lithionite roasting in rotary kiln, and directly spray water in kiln, to keep having a large amount of water vapors to exist in the roasting kiln, maturing temperature is 900 ℃-1000 ℃, and lithionite improves and the grindability index coefficient improves 5 times greatly through roasting afterreaction performance.The roasting lithionite is the 80-350 order through being finely ground to fineness, presses with slaked lime, the partial mother liquid of returning, residue wash water three and boils stripping, and pressing and boiling stripping is proceed step by step, and slaked lime and wash water also substep add; Pressure is boiled the partial mother liquid that utilization is returned in the process in leaching and is adjusted potassium hydroxide in the solution (KOH) concentration, controlling concn is at the 8-40 grams per liter, and the slaked lime of adding 50-90%, the wash water of 30-90%, the slaked lime that adds 10-50% during stripping, the wash water of 10-70%, under constantly stirring, pressing and boiling temperature is 130-180 ℃, reaction times is 0.5-7 hour, it is fully decomposed, and rate of decomposition can reach more than 97%, and stirring velocity is 80-360 rev/min.Its separation performance of residue that pressure is boiled in the process in leaching is good, does not have the phenomenon that scabs in the still, and the residue water after the separation carries out backflush 6-7 time, the wash water Returning utilization.The net digestion efficiency of Lithium Oxide 98min is more than 90% in the ore deposit.Dissolution fluid adds a small amount of slaked lime except that carbonate, except that behind the aluminium, separate out lithium hydroxide through the multi-stage evaporation crystallization, controlling first section evaporation terminal temperature is 102-130 ℃, latter end evaporation terminal temperature is 130-150 ℃, the lithium hydroxide Tc is 40-80 ℃, and before the lithium hydroxide that the latter end crystallization is separated out turned back to first section evaporative crystallization, the lithium hydroxide amount of returning for evaporation before the 10-150% of lithium hydroxide amount in the solution, separate out qualified lithium hydroxide in first section crystallization.Through washing the dry finished product that gets.Mother liquor part after the lithium hydroxide crystallization is separated out is returned to press and is boiled stripping, remainder carries out carbonating, makes wherein lithium become Quilonum Retard and pays product, and the mother liquor after the carbonization can further fully utilize, the major product lithium hydroxide accounts for more than 90%, the quality first grade requirement that is up to state standards.The total consumption of whole process medium-slaking lime is (0.7-1.5) with the ratio of roasting lithionite: 1.Production process need be with other any Chemicals.
The present invention compares with the limestone sintering method of existing industrial application, having significantly has superiority: amount of lime of the present invention few 60%, handle one ton of lithionite in the limestone sintering method and need three tons of Wingdales, and one ton of lithionite of this law processing only needs 1.25 tons of Wingdales, not only save big content of starting materials, and make energy consumption reduce about 45%, make residue reduce about 50% simultaneously, one ton of lithium hydroxide product of every production, the lithionite consumption is 10 tons, amount of lime is 12.6 tons, the dried quantity of slag is 21 tons, and one ton of lithium hydroxide product of the every production of limestone sintering method, the lithionite consumption is 12.3 tons, amount of lime is about 40 tons, and the dried quantity of slag is 42 tons.Lithionite is after roasting, and the grindability index coefficient improves 5 times, makes its throughput of same grinding machine can improve 5 times, because reactivity worth is improved greatly, the lithionite rate of decomposition is brought up to more than 97% by 81%, and the rate of recovery of lithium is brought up to about 80% by about 67%.Because the partial mother liquid Returning utilization after the raising of the rate of decomposition and the rate of recovery and crystallization are separated out increases the output of major product lithium hydroxide, pay product Quilonum Retard output and reduce.Because the minimizing of amount of lime makes the throughput of rotary kiln bring up to 4 times by product.Therefore low, the explanation the present invention of this law less investment, cost has very remarkable economic efficiency.
Fig. 1 is a limestone sintering method process flow sheet
Fig. 2 is a process flow sheet of the present invention
Embodiment:
Raw material lithionite ore contains Li
2O 4.51%, Na
2O 1.38%, K
2O 8.03%, Rb
2O 1.4%, Cs
2O 0.25%, F 6.57%, attached water 0.83%, igloss 4.37%, surplus is other.With the roasting in rotary kiln of above-mentioned lithionite, maturing temperature is 980 ℃, directly sprays water in kiln, and lithionite contains Li after the roasting
2O 4.8%, Na
2O 1.41%, K
2O 8.52%, Rb
2O 1.44%Cs
2O 0.28%, F0.71%, igloss 0.76%, surplus is other.Above-mentioned roasting lithionite ground in ball mill two hours, and fineness reaches 300 orders, residual on the sieve＜1%.
With 10 kilograms of above-mentioned levigated lithionites, add mother liquor, wash water, slaked lime and press and boil stripping, its residue is through 7 backflushs, and new water consumption is 120 liters, and the dried slag in washing back weighs 21 kilograms, contains Li in the slag
2O 0.236%(is comprising solvable Li
2O 0.17%), Na
2O 0.084%, K
2O 1.21%, Rb
2O 0.45%, Cs
2O 0.11%.Li in the ore
2The rate of decomposition of O is 96.67%, and net digestion efficiency is 90%, K
2The O net digestion efficiency is 70%.Pressure is boiled 83 liters of dissolution fluids, contains Li
2O 5.2 grams per liters, K
2O 17.2 grams per liters, Al
2O
30.33 grams per liter, CO
a0.87 grams per liter adds 0.4 kilogram of slaked lime under 80 ℃, stir after 2 hours, clarified 12 hours, and removed carbonate and aluminum ion, filter rear filtrate through the multi-stage evaporation crystallization, get 1.09 kilograms of lithium hydroxides, it consists of: LiOH57.28%, Na0.024%, K0.13%, SO
4＜0.001%, Cl
-0.0081%, CaO 0.01%Fe
2O
30.0015%CO
20.11%, acid non-soluble substance＜0.001%, the first grade requirement that is up to state standards gets 8.36 liters in mother liquor after crystallization is separated out, contain Li
2O 11.7 grams per liters, K
2The O424 grams per liter, lithium hydroxide crystallization eduction rate is 91%, with this mother liquor carbonating, getting content is 0.08 kilogram of 97% thick Quilonum Retard, gets 2.3 liters in carbonating mother liquor, wherein contains Li
2O 3 grams per liters, K
2O 620 grams per liters, this process Quilonum Retard deposition rate is 82%.
Claims (8)
1, a kind of processing method of producing lithium hydroxide with roasting lithionite and lime is characterized in that this method is a raw material with lithionite and Wingdale only, earlier lithionite is carried out roasting in the presence of high temperature and steam and becomes the roasting lithionite; Partial mother liquid, the residue wash water of levigated roasting lithionite after slaked lime, the lithium hydroxide crystallization returned are separated out pressed boil stripping, the concentration of potassium hydroxide of this process control solution, the control liquid-solid ratio is (2-6): 1, temperature is 80-180 ℃, under constantly stirring, reacted 0.5-7 hour, lithionite is decomposed, with Lithium Oxide 98min (Li wherein
2O) become lithium hydroxide (LiOH) stripping; Dissolution fluid removes carbonate, removes the multi-stage evaporation crystallization of carrying out returning with lithium hydroxide behind the aluminium and separate out lithium hydroxide with slaked lime; Through washing, dry qualified lithium hydroxide product.
2, processing method according to claim 1, the maturing temperature that it is characterized in that lithionite are 900 ℃-1000 ℃, and adopt and directly spray water in kiln, with existing of a large amount of water vapors in the maintenance roasting kiln.
3, processing method according to claim 1, the fineness that it is characterized in that the roasting lithionite is the 80-350 order.
4, processing method according to claim 1 is characterized in that pressing to boil controlling potassium hydroxide (KOH) concentration in the process at the 8-40 grams per liter, utilizes the mother liquor that returns to adjust.
5, processing method according to claim 1 is characterized in that it is proceed step by step that pressure is boiled process in leaching, and slaked lime and wash water also substep add, and press the slaked lime that adds 50-90% when boiling, the wash water of 30-90%; The slaked lime that adds 10-50% during stripping, the wash water of 10-70%; It is 130-180 ℃ that pressure is boiled temperature, and the reaction times is 0.5-7 hour, and stirring velocity is 80-360 rev/min.
6, processing method according to claim 1 is characterized in that pressing the residue that boils after the stripping to carry out backflush 6-7 time, the wash water Returning utilization.
7, processing method according to claim 1 is characterized in that first section evaporation terminal temperature of multi-stage evaporation crystallization processes is 102-130 ℃, and latter end evaporation terminal temperature is 130-150 ℃, and the lithium hydroxide Tc is 40-80 ℃.
8, processing method according to claim 1, it is characterized in that the multi-stage evaporation crystallization processes is before the lithium hydroxide that the latter end crystallization is separated out is turned back to first section evaporative crystallization, the lithium hydroxide amount of returning is separated out qualified lithium hydroxide product for the 10-150% of lithium hydroxide amount in the preceding solution of evaporation in first section crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94113302A CN1043155C (en) | 1994-12-29 | 1994-12-29 | Manufacture of lithium hydroxide from lithionite and lime stone by sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94113302A CN1043155C (en) | 1994-12-29 | 1994-12-29 | Manufacture of lithium hydroxide from lithionite and lime stone by sintering |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1109104A true CN1109104A (en) | 1995-09-27 |
| CN1043155C CN1043155C (en) | 1999-04-28 |
Family
ID=5036661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94113302A Expired - Fee Related CN1043155C (en) | 1994-12-29 | 1994-12-29 | Manufacture of lithium hydroxide from lithionite and lime stone by sintering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1043155C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134087A (en) * | 2011-01-25 | 2011-07-27 | 宜春学院 | Method for preparing alum from lepidolite in tantalum and niobium tailings |
| CN108163874A (en) * | 2018-01-11 | 2018-06-15 | 宜春市云威新材料有限公司 | A kind of method of High-temperature water heat treatment lepidolite production lithium hydroxide |
| WO2019220003A1 (en) * | 2018-05-18 | 2019-11-21 | Outotec (Finland) Oy | Method for recovering lithium hydroxide |
| WO2021094647A1 (en) * | 2019-11-15 | 2021-05-20 | Outotec (Finland) Oy | Arrangement and method for recovering lithium hydroxide |
| CN116789151A (en) * | 2023-01-10 | 2023-09-22 | 浙江永正锂电股份有限公司 | Preparation method of anhydrous lithium hydroxide |
| US12385003B2 (en) | 2016-03-01 | 2025-08-12 | The Fynder Group, Inc. | Filamentous fungal biomats, methods of their production and methods of their use |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1029112C (en) * | 1992-06-23 | 1995-06-28 | 中南工业大学 | Method for extracting alkali metal compound from lepidolite concentrate |
-
1994
- 1994-12-29 CN CN94113302A patent/CN1043155C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134087A (en) * | 2011-01-25 | 2011-07-27 | 宜春学院 | Method for preparing alum from lepidolite in tantalum and niobium tailings |
| US12385003B2 (en) | 2016-03-01 | 2025-08-12 | The Fynder Group, Inc. | Filamentous fungal biomats, methods of their production and methods of their use |
| CN108163874A (en) * | 2018-01-11 | 2018-06-15 | 宜春市云威新材料有限公司 | A kind of method of High-temperature water heat treatment lepidolite production lithium hydroxide |
| WO2019220003A1 (en) * | 2018-05-18 | 2019-11-21 | Outotec (Finland) Oy | Method for recovering lithium hydroxide |
| CN112272654A (en) * | 2018-05-18 | 2021-01-26 | 奥图泰(芬兰)公司 | Process for recovering lithium hydroxide |
| US11292725B2 (en) | 2018-05-18 | 2022-04-05 | Metso Outotec Finland Oy | Method for recovering lithium hydroxide |
| CN112272654B (en) * | 2018-05-18 | 2024-03-15 | 美卓奥图泰芬兰有限公司 | Method for recovering lithium hydroxide |
| WO2021094647A1 (en) * | 2019-11-15 | 2021-05-20 | Outotec (Finland) Oy | Arrangement and method for recovering lithium hydroxide |
| CN116789151A (en) * | 2023-01-10 | 2023-09-22 | 浙江永正锂电股份有限公司 | Preparation method of anhydrous lithium hydroxide |
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| Publication number | Publication date |
|---|---|
| CN1043155C (en) | 1999-04-28 |
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