CN102180502B - Method for extracting alum from lepidolite raw material - Google Patents
Method for extracting alum from lepidolite raw material Download PDFInfo
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- CN102180502B CN102180502B CN2011100740055A CN201110074005A CN102180502B CN 102180502 B CN102180502 B CN 102180502B CN 2011100740055 A CN2011100740055 A CN 2011100740055A CN 201110074005 A CN201110074005 A CN 201110074005A CN 102180502 B CN102180502 B CN 102180502B
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- raw material
- alum
- lithionite
- mother liquor
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Abstract
The invention discloses a method for extracting alum from a lepidolite raw material, comprising the following processing steps of: (1) dipping the lepidolite in a sulphuric acid solution to obtain a solid-liquid mixed solution by using the lepidolite as the raw material; (2) filtering and separating the mixed solution to obtain a mother liquid 1 and filter residues 1; (3) mixing the mother liquid1 for cooling down and freezing; and (4) filtering a frozen liquid, and dehydrating the filter residues to obtain the album. The method for extracting the alum from the lepidolite raw material, disclosed by the invention, has the advantages of mild process conditions, high utilization rate of equipment, low energy consumption, low production cost, environment friendliness and less three-waste discharge because a roasting method is not utilized.
Description
Technical field: the present invention relates to the process for extracting of alum, particularly a kind of method of from the lithionite raw material, extracting alum.
Background technology:Alum is a kind of important chemical material, and it is meant that mainly potassium alum is potassium aluminium sulfate KAl (SO
4)
2Existing alum generally is that to be raw material carry out a word used in place name to it fires and be equipped with alunite or the mine tailing that contains alunite, number is that 201010115907.4 " a kind of chloridizing roasting method of material containing alunite " promptly adopts after the roasting of this method elder generation with chemical process Processing of Preparation alum product like one Chinese patent application.
Do not see at present that having with the lithionite is the report that raw material extracts alum; And in the lithionite raw material, contain multiple metallic element; Be used to as the one of which prepare lithium salts products material such as Quilonum Retard, Lithium Sulphate etc., and in the lithionite raw material content of aluminium sesquioxide up to more than 23%.When being raw material other metallic element of extraction such as lithium product, producing the alum product and can significantly reduce the production cost of alum, and do not adopt a word used in place name firing method, non-exhaust emission with the lithionite.
Summary of the invention: the present invention will provide a kind of method of from the lithionite raw material, extracting alum; Adopt chemical process to prepare alum; When being raw material other metallic element of extraction such as lithium product with the lithionite; Produce the alum product and can significantly reduce the production cost of alum, and do not adopt a word used in place name firing method, non-exhaust emission.
The present invention will provide a kind of method of from the lithionite raw material, extracting alum, and it comprises following process step:
(1) with the lithionite is raw material, gets the solid-liquid mixing solutions with sulphuric acid soln dipping lithionite;
(2) the said mixing solutions of filtering separation gets mother liquor 1 and filter residue 1;
(3) mother liquor 1 is stirred cooling, freezing;
(4) refrigerating fulid filters, and the filter residue dehydration is alum KAl (SO
4)
212H
2The O product.
The method of from the lithionite raw material, extracting alum of the present invention, be by following process step: (1) is raw material with the lithionite, and lithionite is crushed to the 100-300 order; Flood with dilution heat of sulfuric acid; Under 100-150 ℃ of temperature, react, and separate defluorination, get sulfur-bearing hydrochlorate solid, liquid mixing solutions;
(2) filter said mixing solutions and get mother liquor 1 and filter residue 1;
(3) control mother liquor 1 is K
+, Al
3+Saturated solution, stir cooling control saturated solution temperature 0 ℃-50 ℃ following filtering separation slagging-off, must filtrate is mother liquor 2;
(4) mother liquor 2 under agitation is cooled to 0 ℃ ~-30 ℃, filtering separation is filtrated and is reclaimed then, and filter residue is handled through cleaning and dewatering, promptly gets KAlSO
412H
2The O product.
Technical scheme of the present invention is through in mother liquor 1, adding Al
2(SO
4)
3Or Al (OH)
3, control mother liquor 1 and be K
+, Al
3+Saturated solution.
The present invention controls that each chemical substance quality is Li than content in the filter residue 1
2O 0.55-0.62%, K
2O 0.9-1.08%, NaO 0.4-0.45%, Al
2O
38-8.01%, SiO
288.9-89.74%, Rb
2O 0.11-0.123%, CS
2O 0.015-0.018%.
Step of the present invention (1) control dilution heat of sulfuric acid dipping lithionite reaction 4-10 hour.
The present invention is raw material with the lithionite, with the method for dilute sulphuric acid dipping lithionite, need not carry out roasting to raw material; Non-exhaust emission; It prepares from the lithionite raw material in the process of alum, and the solution of recovery also can extract multiple metallic element product, like lithium salts; The products such as Quilonum Retard and Lithium Sulphate that are used for lithium cell so just reduce the alum production cost significantly.And improved the lithionite comprehensive utilization ratio.
Following through detecting alum product each item technical indicator of utilizing present method to produce:
Table 1
| Interventions Requested | Standard value | Measured value | Conclusion |
| KAl(SO 4) 2·12H 2O | ≥97.6 | 99.5 | Qualified |
| Iron (Fe) | ≤0.05 | 0.0068 | Qualified |
| Heavy metal (Pb) | ≤0.005 | 0.00015 | Qualified |
| Arsenic | ≤0.001 | ＜0.00006 | Qualified |
| Water-insoluble | ≤0.2 | 0.001 | Qualified |
| Moisture | ≤1.0 | 0.02 | Qualified |
The technological process of production of the present invention is following:
Lithionite+dilute sulphuric acid → reaction → defluorination → separating slag → mother liquor is freezing → and separation → solution is freezing → separation → slag cleaning → alum product.
Embodiment: followingly the present invention is done further explain with embodiment.
Embodiment 1: relate to concentration among the embodiment and be mass concentration;
(1) be raw material with the lithionite, lithionite is crushed to 200 orders, placing reaction unit and adding concentration is 50% sulphuric acid soln; Lithionite raw material and vitriolic mass ratio are 1:2-3; Under heat temperature raising to the 120 ℃ temperature, reacted 6 hours, and adopt the distillation for processing defluorination; Obtain the solid-liquid mixing solutions;
Main chemical compositions in the lithionite raw material such as following table (wt%)
| Li 2O | K 2O | Na 2O | AL 2O 3 | SiO 2 | Fe 2O 3 | Rb 2O | Cs 2O | F |
| 4.5 | 6.3 | 2.7 | 23.5 | 52.84 | 0.18 | 1.45 | 0.22 | 4.1 |
(2) with (1) step solid-liquid mixing solutions, carry out spinning, make filtrating mother liquor 1 and filter residue 1 with whizzer; And control detects main chemical compositions content in the filter residue 1;
| Li 2O | K 2O | Na 2O | AL 2O 3 | SiO 2 | Rb 2O | Cs 2O |
| 0.61 | 1.07 | 0.45 | 8.01 | 89.74 | 0.123 | 0.018 |
(3) mother liquor 1 is carried out freezing treatment, under constantly stirring, detect K in the mother liquor 1
+, Al
3+Concentration is through adding Al
2(SO
4)
3Or Al (OH)
3Control K in the mother liquor 1
+, Al
3+Concentration is in state of saturation, forms K
+, Al
3+Saturated solution makes mother liquor 1 solution temperature reduce to then and is not higher than 50 ℃, generally at 25 ℃, carries out the filtering separation slagging-off with whizzer again, and filtrating is mother liquor 2;
(4) mother liquor 2 that (3) step is extracted is cooled to 0 ℃～-30 ℃ under whipped state, this instance is controlled at-10 ℃, forms the solid-liquid mixed solution; Use the whizzer spinning then, filtrating recovery is used to prepare lithium salts, like Lithium Sulphate or Quilonum Retard; The filter residue water cleans, and is alum KAl (SO
4)
212H
2The O product.
Claims (4)
1. from the lithionite raw material, extract the method for alum; It is characterized in that: undertaken by following technology: (1) is raw material with the lithionite, and lithionite is crushed to the 100-300 order and with dilution heat of sulfuric acid dipping, under 100-150 ℃ of temperature, reacts; Separate defluorination, get sulfur-bearing hydrochlorate solid, liquid mixing solutions;
(2) filter said mixing solutions and get mother liquor 1 and filter residue 1;
(3) control mother liquor 1 is K
+, Al
3+Saturated solution, stir cooling control saturated solution temperature 0 ℃-50 ℃ following filtering separation slagging-off, must filtrate is mother liquor 2;
(4) mother liquor 2 under agitation is cooled to 0 ℃～-30 ℃, filtering separation is filtrated and is reclaimed then, and filter residue is handled through cleaning and dewatering, promptly gets alum KAl (SO
4)
212H
2The O product.
2. according to the described method of from the lithionite raw material, extracting alum of claim 1, it is characterized in that (3) step is through in mother liquor 1, adding Al
2(SO
4)
3Or Al (OH)
3, control mother liquor 1 and be K
+, Al
3+Saturated solution.
3. according to the described method of from the lithionite raw material, extracting alum of claim 1, it is characterized in that controlling that each chemical material components quality is Li than content in the filter residue 1
2O 0.55-0.62%, K
2O 0.9-1.08%, Na
2O 0.4-0.45%, Al
2O
38-8.01%, SiO
288.9-89.74%, Rb
2O 0.11-0.123%, Cs
2O 0.015-0.018%.
4. according to the described method of from the lithionite raw material, extracting alum of claim 1, it is characterized in that step (1) control dilution heat of sulfuric acid dipping lithionite reaction 4-10 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100740055A CN102180502B (en) | 2011-03-27 | 2011-03-27 | Method for extracting alum from lepidolite raw material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100740055A CN102180502B (en) | 2011-03-27 | 2011-03-27 | Method for extracting alum from lepidolite raw material |
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| Publication Number | Publication Date |
|---|---|
| CN102180502A CN102180502A (en) | 2011-09-14 |
| CN102180502B true CN102180502B (en) | 2012-07-25 |
Family
ID=44566829
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|---|---|---|---|
| CN2011100740055A Active CN102180502B (en) | 2011-03-27 | 2011-03-27 | Method for extracting alum from lepidolite raw material |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN103613110A (en) * | 2013-11-25 | 2014-03-05 | 江西本源新材料科技有限公司 | Method for preparing aluminum potassium sulfate dodecahydrate, aluminum rubidium sulfate dodecahydrate and aluminum cesium sulfate dodecahydrate |
| CN107963646B (en) * | 2017-12-07 | 2020-01-03 | 中国科学院新疆理化技术研究所 | Method for rapidly preparing aluminum potassium sulfate by using vermiculite |
| CN111573703A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for preparing ammonium alum by using sulfuric acid method lithium extraction leaching solution |
| CN111573702A (en) * | 2020-05-29 | 2020-08-25 | 贵州省贵金属矿产资源综合利用工程技术研究中心有限公司 | Method for preparing potassium alum by using sulfuric acid method lithium extraction leaching solution |
| CN114634355A (en) * | 2022-03-11 | 2022-06-17 | 苏州大学 | Treatment method for recycling ferrous lepidolite leaching residues |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB190706626A (en) * | 1907-03-19 | 1908-03-19 | William Phillips Thompson | Improvements in the Process of Treating Ores containing Lithia. |
| CN100503849C (en) * | 2006-11-24 | 2009-06-24 | 江西赣锋锂业股份有限公司 | Method for producing refined lithium sulfate solution used in lepidolite lithium-extracting technique by sulfuric acid process |
| CN102139894A (en) * | 2011-01-25 | 2011-08-03 | 宜春银锂新能源有限责任公司 | Novel method for preparing battery grade lithium carbonate by using tantalum niobium tailings lithium mica |
| CN102134087A (en) * | 2011-01-25 | 2011-07-27 | 宜春学院 | Method for preparing alum from lepidolite in tantalum and niobium tailings |
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