CN104310430A - Impurity removal method for lithium hydroxide preparation process - Google Patents
Impurity removal method for lithium hydroxide preparation process Download PDFInfo
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- CN104310430A CN104310430A CN201410521934.XA CN201410521934A CN104310430A CN 104310430 A CN104310430 A CN 104310430A CN 201410521934 A CN201410521934 A CN 201410521934A CN 104310430 A CN104310430 A CN 104310430A
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- Prior art keywords
- lithium hydroxide
- filtration
- impurity
- sodium
- freezing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
Abstract
The invention discloses an impurity removal method for a lithium hydroxide preparation process, which belongs to the field of a method for removing Ca and Mg in the lithium hydroxide preparation process. The method comprises the steps of converting lithium sulfate to lithium hydroxide by virtue of alkalization and freezing precipitation of sodium, separating the freezing liquid after the sodium sulfate is crystallized by virtue of the freezing precipitation of sodium, and the method is characterized by also comprising the steps: directly and roughly filtering the freezing liquid under a low-temperature condition, and fine filtering the freezing liquid after the fine filter condition is satisfied so as to remove the impurity. The impurity removal method is applied to the lithium hydroxide preparation process, the Ca/Mg impurities can be simply and efficiently removed, and the product quality can be greatly improved.
Description
Technical field
The invention belongs to the method field except Ca, Mg in lithium hydroxide technique.
Background technology
The lithium hydroxide preparation technology of existing extensive employing is by obtaining lithium hydroxide to lithium sulfate solution alkalization and the freezing technique analysing sodium, namely by adding sodium hydroxide alkalization in lithium sulfate solution, simultaneously under cryogenic freezing condition, sodium sulfate crystal is separated out, and lithium and hydroxide radical are combined into lithium hydroxide, thus Lithium Sulphate to be converted into lithium hydroxide.Analyse the refrigerating fulid after sodium fractional crystallization sodium sulfate through freezing, temperature is now usually below-5 °.
By alkalization deliming mode: under lithium sulfate solution condition, heating, adds sodium hydroxide and sodium carbonate, the Ca/Mg in filter press removing solution.After current technology adds sodium hydroxide and sodium carbonate when alkalizing workshop section, though through filter press, a part of calcium magnesium can be removed, but due to method (filter press) and the hot conditions of process, the impurity that can not remove is still higher, at 0.025-0.035g/L, the calcium magnesium in product is finally caused to be in Near The Critical Point.To further improving product quality, existing technique will be difficult to accomplish something.
Summary of the invention
The object of the invention is to: propose a kind of in lithium hydroxide preparation technology, Ca/Mg impurity can be removed simply, efficiently, significantly improve the method for product quality.
The object of the invention is realized by following technical proposals:
A kind of for the impurity-removing method in lithium hydroxide preparation technology, comprise through alkalization and freezingly analyse after Lithium Sulphate is converted into lithium hydroxide by sodium, the refrigerating fulid after sodium fractional crystallization sodium sulfate is analysed through freezing, further comprising the steps of: to described refrigerating fulid directly under its cold condition, first carry out after coarse filtration meets smart filtration condition, carry out essence and filter and realize removal of impurities.
In such scheme, analyse the refrigerating fulid after sodium fractional crystallization sodium sulfate through freezing, temperature now usually below-5 °, now impurity CaCO
3, Mg (OH)
2solubleness is low, carries out smart Filtration Filtration separation with this understanding, can make the Ca in filtrate to solution
2+, Mg
2+, concentration reduces further, product quality is improved significantly.The program directly utilizes existing system condition, both without the need to heating, also without the need to adding extra impurity removal reagents, except miscellaneous operation can not bring extra impurity and loss.
When the solution system after freezing is in low-temperature condition, stay impurity concentration in the solution to reduce further, thus obtain better solution quality.If impurity is not separated under cryogenic, after subsequent handling temperature raises, partial impurities enters solution with the form of ion again, more, accurate again filters is also helpless.
As selection, described freezing sodium temperature of analysing is-5 ~ 10 °, described smart Filtration Filtration more than 2 microns impurity.
In such scheme, adopt this temperature and filtration condition effectively can realize removal of impurities, owing to being reduced by large for impurity concentration radian, significantly improve product quality.
As selection, described coarse filtration adopts Plate Filtration, and described essence is filtered and adopted membrane filtration.
In such scheme, can utilize existing Plate Filtration device, realize coarse filtration, the system after Plate Filtration just in time meets again the requirement of the membrane filtration that essence is filtered, and the membrane filtration that final essence is filtered meets high-quality removal of impurities requirement.
The main scheme of aforementioned the present invention and each further selection scheme thereof can independent assortment to form multiple scheme; be the present invention can adopt and claimed scheme: as the present invention; each selection can select arbitrary combination with other; those skilled in the art can understand there is multiple combination according to prior art and common practise after understanding the present invention program; be the claimed technical scheme of the present invention, do not do exhaustive at this.
Beneficial effect of the present invention: scheme is simple, conveniently efficient, major impurity Ca, Mg total impurities is effectively controlled, reduce Ca, Mg total amount in product lithium hydroxide, thus improving product quality, the actual detected result of impurity is far below current industrial goods standard-required.Solution system after filtration, in evaporative crystallization thereafter, heavily dissolves and can not consider Ca, Mg impurity effect completely.
Embodiment
Following non-limiting examples is for illustration of the present invention.
Embodiment 1:
A kind of for the impurity-removing method in lithium hydroxide preparation technology, lithium sulfate solution is after alkalization deliming, index is CaO0.022g/L, Li2O 34.5g/L, freezingly analyse after Lithium Sulphate is converted into lithium hydroxide by sodium, Li2O is 38.6g/L, the refrigerating fulid after sodium fractional crystallization sodium sulfate is analysed through freezing, chilled liquid temperature is-5 °, to refrigerating fulid directly under its cold condition, after the coarse filtration of advanced row Plate Filtration meets smart filtration condition, carry out the filtration of membrane filtration essence and realize removal of impurities, removing Ca, Mg impurity, membrane filtration precision is <2 micron.Last impurity-eliminating effect data are CaO 0.002g/L.The testing method of aforementioned index: volumetry.
Embodiment 2:
For the impurity-removing method in lithium hydroxide preparation technology, lithium sulfate solution is after alkalization deliming, and index is Li
2o25g/L, CaO 0.015g/L, freezingly analyse after Lithium Sulphate is converted into lithium hydroxide by sodium, analyse the refrigerating fulid after sodium fractional crystallization sodium sulfate through freezing, chilled liquid temperature is-4 °, to refrigerating fulid directly under its cold condition, after the coarse filtration of advanced row Plate Filtration meets smart filtration condition, carry out the filtration of membrane filtration essence and realize removal of impurities, removing Ca, Mg impurity, membrane filtration precision is <2 micron.Last impurity-eliminating effect data are CaO 0.0011 g/L.The testing method of aforementioned index: volumetry.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (3)
1. one kind for the impurity-removing method in lithium hydroxide preparation technology, comprise through alkalization and freezingly analyse after Lithium Sulphate is converted into lithium hydroxide by sodium, the refrigerating fulid after sodium fractional crystallization sodium sulfate is analysed through freezing, characterized by further comprising following steps: to described refrigerating fulid directly under its cold condition, first carry out after coarse filtration meets smart filtration condition, carry out essence and filter and realize removal of impurities.
2. as claimed in claim 1 for the impurity-removing method in lithium hydroxide preparation technology, it is characterized in that: described freezing sodium temperature of analysing is-5 ~ 10 °, described smart Filtration Filtration more than 2 microns impurity.
3. as claimed in claim 1 or 2 for the impurity-removing method in lithium hydroxide preparation technology, it is characterized in that: described coarse filtration adopts Plate Filtration, described essence is filtered and is adopted membrane filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410521934.XA CN104310430A (en) | 2014-09-30 | 2014-09-30 | Impurity removal method for lithium hydroxide preparation process |
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| CN201410521934.XA CN104310430A (en) | 2014-09-30 | 2014-09-30 | Impurity removal method for lithium hydroxide preparation process |
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| CN104310430A true CN104310430A (en) | 2015-01-28 |
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ID=52365784
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| CN201410521934.XA Pending CN104310430A (en) | 2014-09-30 | 2014-09-30 | Impurity removal method for lithium hydroxide preparation process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046264A (en) * | 2016-06-13 | 2016-10-26 | 王金明 | Preparation of lithium hydroxide adsorbent |
| CN107986301A (en) * | 2017-12-27 | 2018-05-04 | 江西赣锋锂业股份有限公司 | A kind of method using battery-level lithium carbonate sinker mother liquor production LITHIUM BATTERY lithium hydroxide |
| CN110127729A (en) * | 2019-05-27 | 2019-08-16 | 四川思达能环保科技有限公司 | Lithium hydroxide production technology |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481125A (en) * | 2009-02-13 | 2009-07-15 | 海门容汇通用锂业有限公司 | Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate |
| CN102115101A (en) * | 2011-01-05 | 2011-07-06 | 屈俊鸿 | Novel method for producing lithium carbonate and lithium hydroxide |
| CN102659144A (en) * | 2012-04-26 | 2012-09-12 | 雅安华汇锂业科技材料有限公司 | Method for preparing high purity level lithium hydroxide monohydrate |
| CN102838140A (en) * | 2012-09-14 | 2012-12-26 | 四川国润新材料有限公司 | Method for directly producing environment-friendly lithium hydroxide monohydrate from spodumene |
-
2014
- 2014-09-30 CN CN201410521934.XA patent/CN104310430A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481125A (en) * | 2009-02-13 | 2009-07-15 | 海门容汇通用锂业有限公司 | Method for cyclically using lithium deposition for preparing sodium carbonate solution to produce lithium carbonate |
| CN102115101A (en) * | 2011-01-05 | 2011-07-06 | 屈俊鸿 | Novel method for producing lithium carbonate and lithium hydroxide |
| CN102659144A (en) * | 2012-04-26 | 2012-09-12 | 雅安华汇锂业科技材料有限公司 | Method for preparing high purity level lithium hydroxide monohydrate |
| CN102838140A (en) * | 2012-09-14 | 2012-12-26 | 四川国润新材料有限公司 | Method for directly producing environment-friendly lithium hydroxide monohydrate from spodumene |
Non-Patent Citations (3)
| Title |
|---|
| 伊文涛等: "高纯碳酸锂的应用与制备方法评述", 《IM&P 化工矿物与加工》 * |
| 化学工业部设备涉及技术中心站: "《化工设备设计参考资料 微孔管式过滤器资料汇编》", 30 September 1979, 化学工业部设备涉及技术中心站 * |
| 罗合春等: "《生物制药工程原理与设备》", 28 February 2007, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106046264A (en) * | 2016-06-13 | 2016-10-26 | 王金明 | Preparation of lithium hydroxide adsorbent |
| CN107986301A (en) * | 2017-12-27 | 2018-05-04 | 江西赣锋锂业股份有限公司 | A kind of method using battery-level lithium carbonate sinker mother liquor production LITHIUM BATTERY lithium hydroxide |
| CN110127729A (en) * | 2019-05-27 | 2019-08-16 | 四川思达能环保科技有限公司 | Lithium hydroxide production technology |
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Application publication date: 20150128 |