CN107012323A - A kind of extracting method of potassium rubidium cesium alum - Google Patents
A kind of extracting method of potassium rubidium cesium alum Download PDFInfo
- Publication number
- CN107012323A CN107012323A CN201611189192.0A CN201611189192A CN107012323A CN 107012323 A CN107012323 A CN 107012323A CN 201611189192 A CN201611189192 A CN 201611189192A CN 107012323 A CN107012323 A CN 107012323A
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- CN
- China
- Prior art keywords
- mother liquor
- lepidolite
- cesium alum
- potassium rubidium
- extracting method
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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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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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of extracting method of potassium rubidium cesium alum, using lepidolite as raw material, including：1) lepidolite and dilution heat of sulfuric acid are reacted, forms containing sulfate solid-liquid mixed solution；2) mixed solution is separated by filtration, filter residue is removed, obtains filtrate mother liquor 1；3) filtrate mother liquor 1 is separated by filtration through the freezing processing that cools, filter residue is potassium rubidium cesium alum.During extracting lithium salts by raw material of lepidolite, reclaim and extract potassium rubidium caesium metal and its salt, improve the comprehensive development and utilization rate of lepidolite.
Description
Technical field
The present invention relates to a kind of extracting method of potassium rubidium cesium alum, the side of potassium rubidium cesium alum is particularly extracted from lepidolite raw material
Method.
Background technology
The alum is the crystalline hydrate of each metal sulfate, and potassium, rubidium, cesium alum are potassium sulfate, rubidium sulfate, three kinds of things of cesium sulfate
The general designation of matter crystalline hydrate mixing, is important rare metal chemical raw material.
Lepidolite is a kind of important mineral resources, and it contains abundant Rare Metals Materials, lithium, sodium, potassium, rubidium, caesium, aluminium
Deng.With the growing tension of world energy sources, the common issue that new energy is the world is developed, lithium electricity new energy is used as new energy
One of important industry of development, is increasingly paid attention to by various countries；Lithium and its esters lithium carbonate, the salt such as lithium sulfate are the new energy of lithium electricity
The basic raw produce of source industry, and the basic material lithium metal containing the electric New Energy Industry of lithium in lepidolite, therefore to lithium
The development and application of mica turn into current heat subject.During development and application lithium and its salt, due to containing in lepidolite raw material
There are abundant other metallic elements, and only extract lithium metal and its salt, do not make the such significant wastage of development and application to remaining metal
Valuable mineral resources, and will also result in certain pollution to environment, therefore lithium in lepidolite raw material is extracted and its salt
During, the extraction to potassium, rubidium, caesium is also necessary；Such as extract lithium carbonate when, while extract remaining metallic potassium, rubidium,
The production cost of lithium carbonate can be greatly reduced in cesium salt.
The report of potassium rubidium cesium alum extraction it is not related to also at present, lithium, rubidium, cesium salt are extracted from lepidolite raw material to be had extremely
Extensive development prospect.
The content of the invention
The present invention is sought to provide a kind of extracting method of potassium rubidium cesium alum, and lithium salts is particularly extracted by raw material of lepidolite
During, reclaim and extract potassium rubidium caesium metal and its salt, improve the comprehensive development and utilization rate of lepidolite.
The extracting method of technical scheme potassium rubidium cesium alum, using lepidolite as raw material, including：
1) lepidolite and dilution heat of sulfuric acid are reacted, forms containing sulfate solid-liquid mixed solution；
2) mixed solution is separated by filtration, filter residue is removed, obtains filtrate mother liquor 1；
3) filtrate mother liquor 1 is separated by filtration through the freezing processing that cools, filter residue is potassium rubidium cesium alum.
The potassium rubidium cesium alum is extracted by following processing step：
1）Lepidolite is crushed to 80-300 mesh, impregnated with dilution heat of sulfuric acid, shape is reacted at a temperature of being heated to 110-130 DEG C
Into the solid-liquid mixed solution of containing sulfate；
2）Filtered fluid separates the mixed solution, and filter residue is removed, and filtrate mother liquor 1 is diluted with water；
3）Frozen cooling processing, by the mother liquor 1 after dilution, is cooled to 0-50 DEG C, forms crystallization solution；
4）Filtering for crystallizing solution, filter residue is potassium rubidium cesium alum product, and filtrate mother liquor 2 is reclaimed.
Sulfuric acid solution concentration of the present invention is 40-60wt%.
The present invention controls lepidolite and sulfuric acid solution reaction temperature is 118-128 DEG C, reaction time 4-12 hour.
Rate-determining steps 2 of the present invention）Each chemical substance composition in filter residue（wt%）For the O 0.25-0.29 of Li 2, K 2
O0.8-0.99、Na 2 O 0.35-0.405、Al 2 O 3 7.0-7.51、SiO 2 90.1-91.2、Rb 2 O 0.09-
0.097、Cs 2 O0.015-0.0155。
The present invention is diluted to mother liquor 1 to be diluted with the water of the 2-3 times of volume ratio of mother liquor 1.
Step 4 of the present invention）Control Rb+ concentration≤0.006g/L in the filtrate mother liquor 2, Cs+ concentration≤0.005-0.008g/L,
K+ concentration≤4.83g/L.
The present invention produces potassium rubidium caesium using lepidolite as raw material during lithium metal in extracting lepidolite raw material and lithium salts
Alum, particularly during lithium carbonate or lithium sulfate is prepared, you can realize production potassium rubidium cesium alum product.Potassium rubidium cesium alum is sulfuric acid
Potassium, rubidium sulfate, the crystalline hydrate of cesium sulfate, according to GB3885-83 examination criterias and method, have in the crystalline hydrate after testing
It is respectively potassium sulfate 27.8wt%, rubidium sulfate 7.18wt%, cesium sulfate 1.12wt% to imitate content.
Primary chemical equation of the present invention：
K 2 O+H 2 SO 4 → K 2 SO 4 +H 2 O Rb 2 O+H 2 SO 4 → Rb 2 SO 4 +H 2 O Cs
2 O+H 2 SO 4 → Cs 2 SO 4 +H 2 O
The crystalline hydrate of the three is potassium rubidium cesium alum.
It is mass concentration to be related to concentration in embodiment embodiment.
Embodiment 1：
Take its primary chemical composition such as following table of the lepidolite raw material of Yichuan tantalum niobium lithium ore deposit production（wt%）
1）Above-mentioned lepidolite ore is crushed to 200 mesh, impregnated with concentration 50wt% sulfuric acid solutions, general control lepidolite：
Sulfuric acid mass ratio is 1：2.5, and it is heated to 120 DEG C, stirring reaction 4-10 hours, and fluorine removal processing is carried out, form sulfur-bearing
The solid-liquid mixed solution of hydrochlorate；
2）Above-mentioned solid-liquid mixed solution is separated through centrifugal filtration, remove filter residue, control filter residue in each component composition be respectively with
Wt% is counted
Filtrate is mother liquor 1, and mother liquor 1 is diluted with water；Mother liquor 1 and water volume ratio are 1：2 ；Use the volume of mother liquor 1
2 times of water dilution；
3）The frozen cooling of mother liquor 1 after upper step is diluted is to 0-50 DEG C, and this example is cooled to 25 DEG C, and knot is formed while stirring
Brilliant solution；
4）To 3）Step crystallization solution is separated by filtration, and filter residue is potassium rubidium cesium alum product, and filtrate is mother liquor 2, and controls filtrate
Rb+concentration≤0.006g/L in mother liquor 2, Cs+concentration≤0.005g/L, K+concentration≤4.8g/L.
Claims (7)
1. the extracting method of potassium rubidium cesium alum, it is characterized in that using lepidolite as raw material, including：
1) lepidolite and dilution heat of sulfuric acid are reacted, forms containing sulfate solid-liquid mixed solution；
2) mixed solution is separated by filtration, filter residue is removed, obtains filtrate mother liquor 1；
3) by filtrate mother liquor 1 through the freezing processing that cools, filter residue is separated by filtration for potassium rubidium cesium alum.
2. according to the extracting method of potassium rubidium cesium alum described in claim 1, it is characterized in that being carried out by following processing step：
1）Lepidolite is crushed to 80-300 mesh, impregnated with dilution heat of sulfuric acid, formation is reacted at a temperature of 110-130 DEG C and is contained
The solid-liquid mixed solution of sulfate；
2）The mixed solution is separated by filtration, filter residue is removed, and filtrate mother liquor 1 is diluted with water；
3）Frozen cooling processing, by the mother liquor 1 after dilution, is cooled to 0-50 DEG C, to crystallization solution；
4）Filtering for crystallizing solution, filter residue is potassium rubidium cesium alum product, and filtrate mother liquor 2 is reclaimed.
3. according to the extracting method of potassium rubidium cesium alum described in claim 1 or 2, it is characterized in that step 1）Sulfuric acid solution concentration
For 40-60wt%.
4. according to the extracting method of potassium rubidium cesium alum described in claim 1 or 2, it is characterized in that control lepidolite and sulfuric acid solution
118-128 DEG C of reaction temperature, reaction time 4-12 hour.
5. according to the extracting method of potassium rubidium cesium alum described in claim 1 or 2, it is characterized in that step 2）Each chemistry in filter residue
Material composition（wt%）For the O 0.25-0.29 of Li 2, K 2 O 0.8-0.99, Na 2 O 0.35-0.405, Al 2 O 3
7.0-7.51、SiO 290.1-91.2、Rb 2 O 0.09-0.097、Cs 2 O 0.015-0.0155。
6. according to the extracting method of potassium rubidium cesium alum described in claim 1 or 2, it is characterized in that step 2）Female is used to mother liquor 1
The water dilution of 2-3 times of volume ratio of liquid 1.
7. according to the extracting method of potassium rubidium cesium alum described in claim 2, it is characterized in that step 4）Control the filtrate mother liquor 2
Middle Rb+concentration≤0.006g/L, Cs+concentration≤0.005-0.008g/L, K+concentration≤4.8g/L.
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| CN201611189192.0A CN107012323A (en) | 2016-12-21 | 2016-12-21 | A kind of extracting method of potassium rubidium cesium alum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108996532A (en) * | 2018-09-12 | 2018-12-14 | 江西海汇龙洲锂业有限公司 | The method of rubidium, caesium, aluminium, potassium is recycled from lepidolite extracted lithium byproduct mixing alum |
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| CN102010992A (en) * | 2010-10-29 | 2011-04-13 | 江西本源新材料科技有限公司 | Method for removing fluorine from lithium mica raw material |
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| CN104313349A (en) * | 2014-10-10 | 2015-01-28 | 李宇龙 | Method of extracting lithium salt from lepidolite |
| CN106148730A (en) * | 2016-07-05 | 2016-11-23 | 广东道氏技术股份有限公司 | One extracts alkali-metal method from lepidolite |
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- 2016-12-21 CN CN201611189192.0A patent/CN107012323A/en active Pending
Patent Citations (6)
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|---|---|---|---|---|
| CN102010992A (en) * | 2010-10-29 | 2011-04-13 | 江西本源新材料科技有限公司 | Method for removing fluorine from lithium mica raw material |
| CN102206748A (en) * | 2011-04-13 | 2011-10-05 | 江西本源新材料科技有限公司 | Method for extracting potassium, rubidium, caesium and vanadium |
| CN102828052A (en) * | 2012-08-27 | 2012-12-19 | 张勇 | Method for separating potassium, rubidium, cesium and vitriol after extracting lithium from lepidolite |
| CN103014317A (en) * | 2012-12-04 | 2013-04-03 | 宜春银锂新能源有限责任公司 | Method for extracting lithium salt from lepidolite |
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| CN108996532A (en) * | 2018-09-12 | 2018-12-14 | 江西海汇龙洲锂业有限公司 | The method of rubidium, caesium, aluminium, potassium is recycled from lepidolite extracted lithium byproduct mixing alum |
| CN108996532B (en) * | 2018-09-12 | 2020-07-24 | 江西海汇龙洲锂业有限公司 | Method for recovering rubidium, cesium, aluminum and potassium from mixed vanadium of by-products of lithium extraction from lepidolite |
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Application publication date: 20170804 |