CN103980009B - Hydromica barium ion exchange process extracts soluble potassium ion - Google Patents
Hydromica barium ion exchange process extracts soluble potassium ion Download PDFInfo
- Publication number
- CN103980009B CN103980009B CN201410225653.XA CN201410225653A CN103980009B CN 103980009 B CN103980009 B CN 103980009B CN 201410225653 A CN201410225653 A CN 201410225653A CN 103980009 B CN103980009 B CN 103980009B
- Authority
- CN
- China
- Prior art keywords
- hydromica
- potassium ion
- ore
- potassium
- ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a kind of method extracting soluble potassium ion in hydromica ore, it comprises the following steps: (1) carries out acid treatment by after hydromica ore grinding; (2) hydromica after acid treatment and the aqueous solution of bariumchloride, regulate the pH value of mixture to react 1-5h at 2-5,30-70 DEG C, collecting by filtration is containing the filtrate of potassium ion.Method steps provided by the invention is simple, and potassium ion extraction yield high (being up to 75%), cost is low, and environmental pollution is little, and can keep hydromica ore laminate structure, is thus suitable for suitability for industrialized production.
Description
Technical field
The invention belongs to chemistry, metallurgical technology field, be specifically related to a kind of method that hydromica barium ion exchange process extracts soluble potassium ion.
Background technology
China is large agricultural country, and along with the continuous improvement of agricultural production conditions, crop yield improves constantly, and the potassium in soil reduces rapidly, therefore very huge to potash fertilizer demand.The present situation of current China Potash mineral resources is: soluble potassium resource is few, insoluble potassium resource rich reserves.The insoluble potassium resource mainly silicates that China is verified at present, its total reserves is more than 10,000,000,000 t.In silicates potassium resource, major part is for potassium-bearing shale (accounting for 70%), mainly hydrous mica ore or the higher shale of potassium felspar sand.
The constitutional features of hydromica ore is: 1. with the structural similitude of talcum, the ratio of silicon-oxy tetrahedron layer and alumina octahedral sheet is 2:1, difference be the Si of tetrahedrallayer about have 1/4 replace by Al, make Si:Al equal 3:1; 2. the unnecessary negative charge that the K Lithium ions compensation silicon-oxy tetrahedron existed by mica layer interlayer produces.Because K ion and OB layer are that valence link is connected, cause the leaching of potassium ion very difficult.General conventional extracting method be with high-temperature roasting or with strong acid as hydrofluoric acid removes destruction lattice silicate, thus cause potassium ion stripping.But after lattice silicate destroys, in other octahedral layers and tetrahedrallayer, the impurity such as a large amount of isomorph elements (manganese, aluminium, silicon, vanadium, titanium and iron) all can leach, and needs subsequent handling loaded down with trivial details in a large number simultaneously; And the use of a large amount of hydrofluoric acid, to environment and build-up of pressure of controlling cost, and the comprehensive utilization of resource can be unfavorable for.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, and provide a kind of method adopting barium ion exchange process to extract soluble potassium ion in hydromica, cost is low, and technique is simple, is suitable for scale operation.
The present invention is for solving the problems of the technologies described above by the following technical solutions:
Extract a method for soluble potassium ion in hydromica ore, it comprises the following steps:
(1) acid treatment is carried out by after hydromica ore grinding;
(2) hydromica after acid treatment and the aqueous solution of bariumchloride, regulate the pH value of mixture to react 1-5h at 2-5,30-70 DEG C, collecting by filtration is containing the filtrate of potassium ion.
Barium ion and the potassium ion ionic radius size when 12 coordination is similar, under doing the condition of activator, is conducive to barium ion and enters between mica layer and displace potassium ion at hydrogen ion.The charge number of barium ion is larger than potassium ion, barium ion enters while interlayer replaces the position of a potassium ion, a room can be produced, by vacancy defect diffusion theory, barium ion below can constantly enter between mica layer, potassium ion is constantly leached, whole process, and the laminate structure of mica remains unchanged.
By such scheme, in the described hydromica ore of step (1), potassium content is 3.0 ~ 10.5%.
By such scheme, step (1) described acid treatment is be the salt acid soak 2h of 10wt% by concentration.
By such scheme, the mass volume ratio of the aqueous solution of step (2) described hydromica and bariumchloride is 1:20-50g/mL.
By such scheme, the concentration of aqueous solution of step (2) described bariumchloride is 0.25 ~ 1.75mol/L.
The inventive method can be used for extracting directly potassium, and the method coupling also can extracting potassium with other, carries K+ efficiency.
Beneficial effect of the present invention is: 1, the present invention adds the aqueous solution of bariumchloride in hydromica ore, activator is made with hydrochloric acid, the most of potassium ion being positioned at mica layer interlayer is become free potassium ion extract, preparation method is simple, potassium ion extraction yield high (being up to 75%), cost is low, and environmental pollution is little, is thus suitable for suitability for industrialized production; 2, the present invention leaches soluble potassium ion with " barium ion exchange process " and can keep hydromica ore laminate structure from hydromica, makes to carry potassium clout and still can be used for producing other byproducts as shale brick etc.While controlling cost, can also utilize resources synthetically.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 extracts barium ion displacement potassium ion schematic diagram in potassium process;
Fig. 2 is the XRD figure of embodiment 1 hydromica ore;
Fig. 3 is the XRD figure that embodiment 1 carries potassium clout.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment 1
(1) cross 200 mesh sieves with ball mill by after hydromica ore grinding, then carrying out acid treatment, is namely the salt acid soak 2h of 10wt% with concentration, and the sample thief rear XRF of oven dry (XRF) is analyzed gained sample and measured potassium content w wherein
0(KO
2) be 3.01%;
(2) hydromica after acid treatment and concentration are the aqueous solution of the bariumchloride of 0.25mol/L, the mass volume ratio of the aqueous solution of hydromica and bariumchloride is 1:20g/mL, the pH value to 2 of mixture is regulated with the hydrochloric acid soln that concentration is 10wt%, be placed in the water bath with thermostatic control stirring reaction 1h of 30 DEG C, collecting by filtration, containing the filtrate of potassium ion, measures the potassium content w in solid insoluble (carrying potassium clout)
1be 2.02%; Total de-potassium rate is 32.9%{w=(w
0-w
1)/w
0.
Fig. 1 is that the present embodiment extracts barium ion displacement potassium ion schematic diagram in potassium process, the potassium ion entering a replacement band positive charge of the barium ion with 2 positive charges, produce a corresponding room, theoretical by vacancy defect, barium ion can constantly to inter-level diffusion, the continuous stripping of potassium ion, whole process only occurs between mica layer, and the laminate structure of mica remains unchanged.Fig. 2 is the XRD figure of the present embodiment hydromica ore used, and the main year potassium mineral in ore sample is hydromica.Fig. 3 is the XRD figure that the present embodiment carries potassium clout, contrasts known with Fig. 2, carry potassium process complete after the dominant of sample be still mutually hydromica, very clearly can find out that the laminate structure of hydromica is not destroyed.
Embodiment 2
(1) cross 200 mesh sieves with ball mill by after hydromica ore grinding, then carrying out acid treatment, is namely the salt acid soak 2h of 10wt% with concentration, and the sample thief rear XRF of oven dry (XRF) is analyzed gained sample and measured potassium content w wherein
0(KO
2) be 6.72%;
(2) hydromica after acid treatment and concentration are the aqueous solution of the bariumchloride of 1.00mol/L, the mass volume ratio of the aqueous solution of hydromica and bariumchloride is 1:30g/mL, the pH value to 3 of mixture is regulated with the hydrochloric acid soln that concentration is 10wt%, be placed in the water bath with thermostatic control stirring reaction 3h of 50 DEG C, collecting by filtration, containing the filtrate of potassium ion, measures the potassium content w in solid insoluble
1be 2.89%; Total de-potassium rate 56.99%{w=(w0-w1)/w0}.
Embodiment 3
(1) cross 200 mesh sieves with ball mill by after hydromica ore grinding, then carrying out acid treatment, is namely the salt acid soak 2h of 10wt% with concentration, and the sample thief rear XRF of oven dry (XRF) is analyzed gained sample and measured potassium content w wherein
0(KO
2) be 10.54%;
(2) hydromica after acid treatment and concentration are the aqueous solution of the bariumchloride of 1.75mol/L, the mass volume ratio of the aqueous solution of hydromica and bariumchloride is 1:50g/mL, the pH value to 5 of mixture is regulated with the hydrochloric acid soln that concentration is 10wt%, be placed in the water bath with thermostatic control stirring reaction 5h of 70 DEG C, collecting by filtration, containing the filtrate of potassium ion, measures the potassium content w in solid insoluble
1be 2.66%; Total de-potassium rate 74.77%{w=(w
0-w
1)/w
0.
Method steps provided by the invention is simple as seen from the above embodiment, and potassium ion extraction yield high (being up to 75%), cost is low, and environmental pollution is little, and can keep hydromica ore laminate structure, is thus suitable for suitability for industrialized production.
Be understandable that, the illustrative embodiments that above embodiment is only used to principle of the present invention is described and adopts, but the present invention is not limited thereto.For those skilled in the art, without departing from the spirit and substance in the present invention, can make various modification and improvement, these modification and improvement are also considered as protection scope of the present invention.
Claims (5)
1. extract a method for soluble potassium ion in hydromica ore, it is characterized in that comprising the following steps:
(1) acid treatment is carried out by after hydromica ore grinding;
(2) hydromica after acid treatment and the aqueous solution of bariumchloride, regulate the pH value of mixture to react 1-5h at 2-5,30-70 DEG C, collecting by filtration is containing the filtrate of potassium ion.
2. extract the method for soluble potassium ion in hydromica ore according to claim 1, it is characterized in that: in the described hydromica ore of step (1), potassium content is 3.0 ~ 10.5%.
3. extract the method for soluble potassium ion in hydromica ore according to claim 1, it is characterized in that: step (1) described acid treatment is be the salt acid soak 2h of 10wt% by concentration.
4. extract the method for soluble potassium ion in hydromica ore according to claim 1, it is characterized in that: the mass volume ratio of the aqueous solution of step (2) described hydromica and bariumchloride is 1:20-50g/mL.
5. extract the method for soluble potassium ion in the hydromica ore according to claim 1 or 4, it is characterized in that: the concentration of aqueous solution of step (2) described bariumchloride is 0.25 ~ 1.75mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410225653.XA CN103980009B (en) | 2014-05-26 | 2014-05-26 | Hydromica barium ion exchange process extracts soluble potassium ion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410225653.XA CN103980009B (en) | 2014-05-26 | 2014-05-26 | Hydromica barium ion exchange process extracts soluble potassium ion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103980009A CN103980009A (en) | 2014-08-13 |
| CN103980009B true CN103980009B (en) | 2016-04-13 |
Family
ID=51272214
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410225653.XA Expired - Fee Related CN103980009B (en) | 2014-05-26 | 2014-05-26 | Hydromica barium ion exchange process extracts soluble potassium ion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103980009B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109504857B (en) * | 2018-11-30 | 2020-11-27 | 武汉工程大学 | Method for extracting soluble potassium ions from biotite by magnesium ion exchange method |
| CN112375920A (en) * | 2020-11-12 | 2021-02-19 | 董启林 | Potassium extraction process |
| CN115725856A (en) * | 2022-11-10 | 2023-03-03 | 中南大学 | Method for strengthening rubidium leaching in rubidium-containing mica concentrate based on ion exchange |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999423A (en) * | 2006-12-31 | 2007-07-18 | 合肥工业大学 | Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar |
| CN103114211A (en) * | 2013-02-19 | 2013-05-22 | 宁波莲华环保科技股份有限公司 | Method for extracting lithium from primary lithium extraction solution of lithium ore |
-
2014
- 2014-05-26 CN CN201410225653.XA patent/CN103980009B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999423A (en) * | 2006-12-31 | 2007-07-18 | 合肥工业大学 | Method of preparing nitrogen phosphorus potassium complex fertilizer using potash feldspar |
| CN103114211A (en) * | 2013-02-19 | 2013-05-22 | 宁波莲华环保科技股份有限公司 | Method for extracting lithium from primary lithium extraction solution of lithium ore |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103980009A (en) | 2014-08-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109879301B (en) | Method for efficiently separating magnesium and lithium from salt lake brine and simultaneously preparing high-purity magnesium oxide and battery-grade lithium carbonate | |
| CN113443640B (en) | Method for preparing battery-grade lithium carbonate and battery-grade iron phosphate by using waste positive and negative electrode powder of lithium iron phosphate battery | |
| CN100567144C (en) | A kind ofly fully utilize the method that ilmenite prepares ferric lithium phosphate precursor | |
| CN101613803B (en) | Method for recovering lead from lead paste of waste lead-acid battery | |
| CN102828025B (en) | Method for extracting V2O5 from stone coal navajoite | |
| CN101709374B (en) | Method for preparing precursors of lithium titanate and lithium iron phosphate by comprehensively using ilmenite | |
| CN101264876B (en) | Method for preparing ferric lithium phosphate precursor by comprehensive utilization of ilmenite | |
| CN106086471B (en) | A kind of method that lepidolite defluorinate and valuable metal leach | |
| CN108004391B (en) | A method of processing lepidolite extracts metallic element | |
| CN101275187A (en) | Process for extracting vanadium by stone coal wet method | |
| CN107098365B (en) | A method of extracting lithium carbonate from lepidolite ore | |
| CN113292057B (en) | Recovery method of waste lithium iron phosphate battery | |
| CN102146513A (en) | Method for extracting vanadium from vanadium-containing ore by oxidation acid-leaching wet method | |
| CN103980009B (en) | Hydromica barium ion exchange process extracts soluble potassium ion | |
| CN105036159A (en) | Method for preparing lithium carbonate with high-lithium salt lake bittern | |
| CN110129587A (en) | A kind of method that spodumene vacuum metling extracts lithium metal and prepares alusil alloy | |
| CN103022491A (en) | Method for preparing lithium iron phosphate precursor for positive pole material of lithium-ion battery | |
| CN107964597B (en) | Method for extracting alkali metal by treating lepidolite | |
| CN114436300A (en) | Method for acidifying and leaching lithium by spodumene | |
| CN107267754B (en) | A method of extracting alkali metal salt using sulfuric acid and lepidolite low-temperature solid phase reaction | |
| CN103160696B (en) | Method for carrying out microwave heating on stone coal containing vanadium to extract vanadium | |
| CN102851521A (en) | Method for extracting vanadium through oxidation conversion of vanadium-containing ores | |
| CN109504857A (en) | The method that magnesium ion exchange process extracts soluble potassium ion from biotite | |
| CN109055737A (en) | A kind of method of sulfuric acid leaching lepidolite ore | |
| CN108516569B (en) | Method for preparing lithium sulfate solution by roasting lepidolite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160413 Termination date: 20190526 |