CN113003588A - Nuclear pure grade Li2CO3Chemical conversion method - Google Patents
Nuclear pure grade Li2CO3Chemical conversion method Download PDFInfo
- Publication number
- CN113003588A CN113003588A CN201911327233.1A CN201911327233A CN113003588A CN 113003588 A CN113003588 A CN 113003588A CN 201911327233 A CN201911327233 A CN 201911327233A CN 113003588 A CN113003588 A CN 113003588A
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- Prior art keywords
- lioh
- powder
- reaction
- conversion method
- chemical conversion
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Links
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 33
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 58
- 239000000843 powder Substances 0.000 claims abstract description 33
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001868 water Inorganic materials 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000012544 monitoring process Methods 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000010902 jet-milling Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 3
- 229910010092 LiAlO2 Inorganic materials 0.000 abstract description 2
- 239000000919 ceramic Substances 0.000 abstract description 2
- 239000008188 pellet Substances 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005137 deposition process Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium;hydroxide;hydrate Chemical compound [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003758 nuclear fuel Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
Classifications
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention belongs to LiAlO2The technical field of ceramic pellet preparation, in particular to nuclear pure grade Li2CO3Chemical conversion method. Raw material LiOH. H2Dissolving O in water, removing impurities insoluble in water, filtering, heating, and adding seed crystal to obtain LiOH. H2Recrystallizing O to obtain recrystallized high-purity LiOH & H2O crystals; high purity LiOH H2Dissolving O crystal in a reaction vessel, introducing CO2Gas, appropriately heated, to create LiOH solution and CO2The reaction environment with sufficient contact of gas ensures that the reaction fully occurs, whether the reaction reaches the end point is judged by monitoring the whole PH value of the solution, and Li is obtained after the reaction reaches the end point2CO3Washing the powder with deionized water and drying; drying Li2CO3Grinding and crushing the powder, controlling the granularity and the morphology, and crushing to obtain a finished product Li2CO3And (3) powder. The inventionMainly applied to nuclear pure grade Li2CO3The purity of the prepared powder can reach more than 99.99 percent.
Description
Technical Field
The invention belongs to LiAlO2The technical field of ceramic pellet preparation, in particular to nuclear pure grade Li2CO3Chemical conversion method.
Background
Currently used Li2CO3The chemical conversion method has low conversion efficiency, small single conversion yield and insufficient control means for purity, and is improved on the basis.
Disclosure of Invention
The invention aims to provide nuclear pure grade Li2CO3Chemical conversion method, mainly applied to nuclear pure grade Li2CO3The purity of the prepared powder can reach more than 99.99 percent, and the method for preparing Li through single conversion2CO3The powder can be adjusted according to the used equipment, can realize small-scale engineering application, and provides a raw material basis for the engineering of special material preparation.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
nuclear pure grade Li2CO3A chemical conversion method,
firstly, raw material LiOH.H2Dissolving O in water, removing impurities insoluble in water, filtering, heating, and adding seed crystal to obtain LiOH. H2Recrystallizing with oxygen to obtain recrystallizedThe high-purity LiOH H2O crystals;
high purity LiOH H2Dissolving O crystal in a reaction vessel, introducing CO2Gas, appropriately heated, to create LiOH solution and CO2The reaction environment with sufficient contact of gas ensures that the reaction fully occurs, whether the reaction reaches the end point is judged by monitoring the whole PH value of the solution, and Li is obtained after the reaction reaches the end point2CO3Washing the powder with deionized water and drying;
drying Li2CO3Grinding and crushing the powder, controlling the granularity and the morphology, and crushing to obtain a finished product Li2CO3And (3) powder.
After completely dissolving, removing impurities insoluble in water by using a fine filtration method.
Obtaining recrystallized high-purity LiOH & H by adopting a centrifugal separation method2And (4) O crystals.
Creating LiOH solution and CO by stirring and microbubble dispersion method2The reaction environment in which the gases are in sufficient contact ensures that the reaction takes place adequately.
After the reaction reaches the end point, obtaining Li by a filter pressing or natural sedimentation method2CO3And (3) powder.
Drying Li2CO3And (3) carrying out jet milling on the powder.
The beneficial effects obtained by the invention are as follows:
the method can realize the pure grade Li of the nucleus2CO3And (3) preparing powder. By chemical reaction and Li2CO3The characteristic of slightly soluble in water completes the deposition process, thereby achieving the purpose of preparing powder. The conversion method is characterized in that Li is prepared by dissolving and recrystallizing raw materials, controlling important parameters in the reaction process and performing subsequent fluidized crushing and cleaning2CO3The powder has controllable granularity and purity of over 99.99 percent, and meets the use standard of nuclear fuel elements. The method can be applied in a laboratory-level environment and can also meet the requirements of engineering production.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The method mainly comprises the key process methods of raw material dissolution and recrystallization, reaction preparation, crushing and screening and the like.
Firstly, raw material LiOH.H2Dissolving O in water, removing impurities insoluble in water by fine filtration, heating the filtered solution, and adding seed crystal to make LiOH. H2Recrystallizing O, and centrifuging to obtain high-purity LiOH & H2And (4) O crystals.
High purity LiOH H2Dissolving O crystal in a reaction vessel, introducing CO2Gas, properly heated, created by stirring and micro-bubble dispersion to make LiOH solution and CO2The reaction environment with sufficient contact of gas ensures that the reaction fully occurs, whether the reaction reaches the end point is judged by monitoring the whole PH value of the solution, and Li is obtained by a filter pressing or natural sedimentation method after the reaction reaches the end point2CO3And (3) washing the powder by using deionized water and then drying.
Drying Li2CO3The powder is grinded by air flow, and the granularity and the shape of the powder are controlled by the method. Crushing to obtain finished product Li2CO3And (3) powder.
The method controls the purity of raw material LiOH by a dissolution recrystallization process, and uses the raw material LiOH. H2Dissolving O in water, removing water-insoluble impurities by fine filtration, heating the mother liquor, adding appropriate additive to promote LiOH crystallization, filtering by centrifugal separation method, and filtering to obtain high-purity LiOH H2O crystal, in this case LiOH. H2The purity of O can be controlled to be more than 99.999 percent.
The method is carried out by using LiOH. H2O and CO2Principle of reaction to prepare Li2CO3During the reaction preparation process, LiOH solution and CO are generated by stirring and microbubble dispersion method2The reaction environment with sufficient contact of gas ensures that the reaction is fully performed by controlling CO2Flow and pH in the reaction vessel to the produced Li2CO3The purity is controlled to ensure that the reaction product is free from other substances.
Filtering to obtain Li2CO3Powder, milling by means of air flow to the Li produced2CO3Crushing the powder, and controlling corresponding parameters to Li2CO3Controlling the granularity of the powder, further cleaning the powder by using deionized water after the powder is finished, and drying to obtain the finished product of the nuclear pure grade Li2CO3The powder has various indexes meeting related industrial standards through detection, and the total purity is over 99.99 percent.
The method can realize the pure grade Li of the nucleus2CO3And (3) preparing powder. By chemical reaction and Li2CO3The characteristic of slightly soluble in water completes the deposition process, thereby achieving the purpose of preparing powder. The conversion method is characterized in that Li is prepared by dissolving and recrystallizing raw materials, controlling important parameters in the reaction process and performing subsequent fluidized crushing and cleaning2CO3The powder has controllable granularity and purity of over 99.99 percent, and meets the use standard of nuclear fuel elements. The method can be applied in a laboratory-level environment and can also meet the requirements of engineering production.
Claims (6)
1. Nuclear pure grade Li2CO3The chemical conversion method is characterized in that:
firstly, raw material LiOH.H2Dissolving O in water, removing impurities insoluble in water, filtering, heating, and adding seed crystal to obtain LiOH. H2Recrystallizing O to obtain recrystallized high-purity LiOH & H2O crystals;
high purity LiOH H2Dissolving O crystal in a reaction vessel, introducing CO2Gas, appropriately heated, to create LiOH solution and CO2The reaction environment with sufficient contact of gas ensures that the reaction fully occurs, whether the reaction reaches the end point is judged by monitoring the whole PH value of the solution, and Li is obtained after the reaction reaches the end point2CO3Powder ofWashing the powder with deionized water and drying;
drying Li2CO3Grinding and crushing the powder, controlling the granularity and the morphology, and crushing to obtain a finished product Li2CO3And (3) powder.
2. Nuclear grade pure Li according to claim 12CO3The chemical conversion method is characterized in that: after completely dissolving, removing impurities insoluble in water by using a fine filtration method.
3. Nuclear grade pure Li according to claim 12CO3The chemical conversion method is characterized in that: obtaining recrystallized high-purity LiOH & H by adopting a centrifugal separation method2And (4) O crystals.
4. Nuclear grade pure Li according to claim 12CO3The chemical conversion method is characterized in that: creating LiOH solution and CO by stirring and microbubble dispersion method2The reaction environment in which the gases are in sufficient contact ensures that the reaction takes place adequately.
5. Nuclear grade pure Li according to claim 12CO3The chemical conversion method is characterized in that: after the reaction reaches the end point, obtaining Li by a filter pressing or natural sedimentation method2CO3And (3) powder.
6. Nuclear grade pure Li according to claim 12CO3The chemical conversion method is characterized in that: drying Li2CO3And (3) carrying out jet milling on the powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911327233.1A CN113003588A (en) | 2019-12-20 | 2019-12-20 | Nuclear pure grade Li2CO3Chemical conversion method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911327233.1A CN113003588A (en) | 2019-12-20 | 2019-12-20 | Nuclear pure grade Li2CO3Chemical conversion method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113003588A true CN113003588A (en) | 2021-06-22 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911327233.1A Pending CN113003588A (en) | 2019-12-20 | 2019-12-20 | Nuclear pure grade Li2CO3Chemical conversion method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113003588A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115872422A (en) * | 2022-10-28 | 2023-03-31 | 中国科学院过程工程研究所 | Method for preparing battery-grade lithium carbonate by using microbubbles to strengthen carbon dioxide reaction crystallization |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4207297A (en) * | 1978-03-27 | 1980-06-10 | Foote Mineral Company | Process for producing high purity lithium carbonate |
| JPS61251511A (en) * | 1985-04-30 | 1986-11-08 | Sumitomo Chem Co Ltd | Production of lithium carbonate powder |
| JP2004196607A (en) * | 2002-12-19 | 2004-07-15 | Nippon Chem Ind Co Ltd | Method for manufacturing high purity lithium carbonate |
| CN102020295A (en) * | 2010-12-22 | 2011-04-20 | 四川天齐锂业股份有限公司 | Preparation method of high-purity lithium carbonate |
| CN102826576A (en) * | 2011-09-19 | 2012-12-19 | 四川长和华锂科技有限公司 | Method for industrially producing industrial, cell-grade or high-purity lithium hydroxide monohydrate |
| CN103351010A (en) * | 2013-06-29 | 2013-10-16 | 西北矿冶研究院 | Preparation process of battery-grade lithium carbonate |
| CN106315625A (en) * | 2016-08-26 | 2017-01-11 | 成都开飞高能化学工业有限公司 | Method for composite production of high-purity lithium hydroxide monohydrate, high-purity lithium carbonate and battery grade lithium carbonate |
| CN106830020A (en) * | 2017-03-15 | 2017-06-13 | 江苏容汇通用锂业股份有限公司 | A kind of preparation method of 4N pure Lithium Carbonates |
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-
2019
- 2019-12-20 CN CN201911327233.1A patent/CN113003588A/en active Pending
Patent Citations (9)
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115872422A (en) * | 2022-10-28 | 2023-03-31 | 中国科学院过程工程研究所 | Method for preparing battery-grade lithium carbonate by using microbubbles to strengthen carbon dioxide reaction crystallization |
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Application publication date: 20210622 |