CN106702139A - Method for extracting sylvite from non-water-soluble potassium-containing rock - Google Patents
Method for extracting sylvite from non-water-soluble potassium-containing rock Download PDFInfo
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- CN106702139A CN106702139A CN201510452200.5A CN201510452200A CN106702139A CN 106702139 A CN106702139 A CN 106702139A CN 201510452200 A CN201510452200 A CN 201510452200A CN 106702139 A CN106702139 A CN 106702139A
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- sylvite
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Abstract
The invention relates to the field of efficient development and utilization of resources and mineral products in chemical engineering, in particular to a method for extracting sylvite from non-water-soluble potassium-containing rock. Aiming at the current situation that a large amount non-water-soluble potassium-containing rock in China are far not effectively utilized, and the domestic sylvite market is in short supply, a novel mixed fluxing agent calcinations-short process potassium-containing rock treatment process is provided, and sodium salt is by-produced while a sylvite product is obtained. After ore is subjected to ore grinding, intermediate-temperature calcinations and hot water leaching, the leaching rate of potassium exceeds 90%, and meanwhile the drag amount is only 1-1.2 times of the original drag amount. Lixivium is subjected to evaporative crystallization, the sylvite product can be obtained, meanwhile, sodium salt is by-produced, and filter residues can serve as building materials and molecular sieve raw materials. The technological process is simple and clean, energy consumption is relatively low, and the method is suitable for large-scale production of the non-water-soluble potassium-containing rock.
Description
Technical field
Field is utilized the present invention relates to the mineral products Efficient Development in resource, chemical industry, it is more particularly to a kind of from non-aqueous
Property potassium bearing rock in extract sylvite method.
Background technology
The water-insoluble potassium bearing rock resource of China extremely enrich, and species it is many, distribution extensively, volcanic rock, sedimentary rock,
All there is potassium bearing rock in metamorphic rock.There was only K in the past2Potassium bearing rock of the O content more than 12% is just considered to have one
Fixed commercial development value, and a large amount of K2O content is asked due to development cost, environment in the potassium bearing rock of 8%-12%
Topic etc. factor and it is ignored.As domestic water solubility potassium resource is gradually deficient, the sylvite market demand increases year by year, right
The Efficient Development of such low grade potassium-containing rock is very urgent, therefore, develop new, cleaning, efficient non-aqueous
Dissolubility potassium bearing rock treatment technology can not only alleviate domestic Potash mineral resources supply deficiency, external dependence degree reality high
Problem, while also for the green of regional characteristics resource, Efficient Development provide an outlet.
Exploitation of the China to water-insoluble potassium ore resources start from the 1950's, it is proposed that various to produce potassium
The scheme and method of salt, summing up can be divided into pyrogenic process and the major class of wet method two.At present, existing thermal process is more
Number decomposed as auxiliary agent with single or mixed inorganic, exist sintering temperature it is too high (>1000 DEG C), resolution ratio compared with
Low (<90%) while the larger (slag/raw ore of the quantity of slag>2) defect.Its improved hydrofluoric acid route, although treatment temperature
Degree is greatly reduced, but hydrofluoric acid corrosivity is too strong and price is relatively expensive, while also there is certain environmental problem；
It is higher to the requirement of the potassium content of raw material and wet processing is mostly carried out under the hydrothermal system of highly basic, and highly basic into
This is also higher, and these problems all annoying the industrialized production that water-insoluble potassium bearing rock extracts sylvite.Therefore, open
Send out short route a kind of, low cost, the environment-friendly technique that sylvite is extracted from water-insoluble potassium bearing rock, be to realize
The basis of the water-insoluble potassium bearing rock production sylvite that reserves are huge, grade is relatively low, and the wherein choosing of flux
Select particularly critical.
The content of the invention
Deficiency of the present invention for existing water-insoluble potassium bearing rock development technology route, there is provided a kind of both to improve
The leaching rate of potassium can suitably reduce sintering temperature and environment amenable extract potassium from water-insoluble potassium bearing rock again
The new method of salt.
The method that sylvite is extracted from water-insoluble potassium bearing rock of the invention, comprises the following steps：
1) with water-insoluble potassium bearing rock as raw material, CaCl is added2And Na2CO3As mixed flux, by original
Material is sufficiently mixed with mixed flux；Wherein, the raw material and CaCl2And Na2CO3By 1：(0.2-0.8)：
The mass ratio mixing of (0.05-0.3)；
2) by step 1) mixed material below 950 DEG C under conditions of be calcined 2-6 hours, the product after roasting
Gone out with water logging under the conditions of below 90 DEG C, leachate and filter residue are obtained through filtering；
3) by step 2) leachate obtain sylvite by evaporative crystallization.
The method for extracting sylvite of the invention, wherein it is preferred to, step 1) raw material and CaCl2With
Na2CO3By 1：(0.3-0.6)：The mass ratio mixing of (0.1-0.3).
The method for extracting sylvite of the invention, wherein it is preferred to, step 2) sintering temperature is
750-900 DEG C, more preferably, 800-850 DEG C.Step 2) roasting time is preferably 3-5 hours.
The method for extracting sylvite of the invention, wherein, step 2) the solid mass ratio of liquid of the leaching is preferably
(0.5-4)：1, more preferably (1-3)：1.Step 2) temperature of the leaching is preferably 70-90 DEG C, leaching
The preferably 2-4 hours time for going out.
The method that sylvite is extracted from water-insoluble potassium bearing rock of the invention, is the matter for further improving sylvite product
Amount, can be in step 3) leachate is carried out except Calcium treatment before leachate evaporative crystallization, deliming mode can be ability
The conventional calcium removal methods in domain, for example, be passed through CO2Precipitated calcium etc..
Water-insoluble potassium bearing rock of the present invention can be the water-insoluble potassium bearing rock of any kind, be not limited to
Common potassium feldspar, biotite, nepheline etc..The present invention can process the relatively low insoluble potassium ore of grade, especially
Can be to process potassium content (with K2O remembers) it is less than 9% low grade potassium ore deposit.
The present invention has found calcium chloride with sodium carbonate as composite fluxing agent pair by contrasting different flux collocation experiment
The leaching effect that sylvite is extracted in the relatively low water-insoluble potassium bearing rock of grade is especially desirable, in sintering temperature
For less than 950 DEG C when, the leaching rate of potassium is up to more than 90%, and slag ore deposit is than only 1-1.2, the process route (figure
1) for water-insoluble potassium bearing rock large-scale industrial production provides possibility.
Brief description of the drawings
Fig. 1 is of the invention to extract sylvite process chart from water-insoluble potassium bearing rock.
Fig. 2 is the X-ray diffraction pattern of water-insoluble potassium bearing rock sample ore.
Fig. 3 is the gained potassium chloride sample photo of embodiment 1.
Specific embodiment
Disclosed in this specification any feature, unless specifically stated otherwise, can be equivalent or with similar purpose by other
Alternative features replaced.Unless specifically stated otherwise, during each feature is a series of equivalent or similar characteristics
One example.It is described to understand the present invention just for the sake of help, should not be considered as to concrete restriction of the invention.
Embodiment 1
The water-insoluble potassium bearing rock that potassium content is 8.47% is crushed to 149 microns (100 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.4:0.05 mass ratio is sufficiently mixed, and 3 is calcined under conditions of 850 DEG C small
When, the product after roasting is gone out with water logging, with liquid-solid ratio 1 under the conditions of 80 DEG C:1 carries out magnetic agitation 2 hours, so
After filter, filtrate is through the isolated sylvite product of evaporative crystallization.
X-ray diffraction pattern (XRD) result of water-insoluble potassium bearing rock shows (Fig. 2), the thing phase composition master of sample
To be quartz and potassium feldspar.The content of potassium is 8.47 in the X-ray fluorescence spectra analysis result display raw ore of sample,
And the potassium content of tailings is only 0.63 (table 1).The leaching rate of the route potassium is 91.8%；The quality of the quantity of slag and raw ore
Than being 1.1.Potassium chloride sample is obtained after the crystallized separation of water lotion as shown in figure 3, its KCE content is more than 95%；
Washing slag can be used as the raw material of building materials or molecular sieve.
X-ray fluorescence spectra (XRF) analysis result of table 1, water-insoluble potassium bearing rock raw ore and tailings
Embodiment 2
The water-insoluble potassium bearing rock that potassium content is 8.47% is crushed to 74 microns (200 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.4:0.05 mass ratio is sufficiently mixed, and 4 is calcined under conditions of 800 DEG C small
When, the product after roasting is gone out with water logging, with liquid-solid ratio 1 under the conditions of 80 DEG C:1 carries out magnetic agitation 2 hours, so
After filter, filtrate through evaporation, Crystallization Separation obtain sylvite product.The leaching rate of this example potassium is 90.1%.The quantity of slag with
The mass ratio of raw ore is 1.15：1.
Embodiment 3
The water-insoluble potassium bearing rock that potassium content is 7.96% is crushed to 149 microns (100 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.6:0.05 mass ratio is sufficiently mixed, and 4 is calcined under conditions of 900 DEG C small
When, the product after roasting is gone out with water logging, with liquid-solid ratio 3 under the conditions of 80 DEG C:1 carries out magnetic agitation 2 hours, so
After filter, filtrate through evaporation, Crystallization Separation obtain sylvite product.The leaching rate of this example potassium is 96.1%.The quantity of slag with
The mass ratio of raw ore is 1：1.
Embodiment 4
The water-insoluble potassium bearing rock that potassium content is 7.96% is crushed to 149 microns (100 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.7:0.05 mass ratio is sufficiently mixed, and 4 is calcined under conditions of 850 DEG C small
When, the product after roasting is gone out with water logging, with liquid-solid ratio 2 under the conditions of 70 DEG C:1 carries out magnetic agitation 3 hours, so
After filter, filtrate through evaporation, Crystallization Separation obtain sylvite product.The leaching rate of this example potassium is 92.6%.The quantity of slag with
The mass ratio of raw ore is 1.1：1.
Embodiment 5
The water-insoluble potassium bearing rock that potassium content is 8.34% is crushed to 74 microns (200 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.4:0.1 mass ratio is sufficiently mixed, and is calcined 4 hours under conditions of 800 DEG C,
Product after roasting is gone out with water logging, with liquid-solid ratio 1 under the conditions of 90 DEG C:1 carries out magnetic agitation 2 hours, then mistake
Filter, filtrate obtains sylvite product through evaporation, Crystallization Separation.The leaching rate of this example potassium is 91.6%.The quantity of slag and raw ore
Mass ratio be 1.15：1.
Embodiment 6
The water-insoluble potassium bearing rock that potassium content is 8.34% is crushed to 149 microns (100 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.5:0.05 mass ratio is sufficiently mixed, and 5 is calcined under conditions of 800 DEG C small
When, the product after roasting is gone out with water logging, with liquid-solid ratio 0.5 under the conditions of 85 DEG C:1 carries out magnetic agitation 4 hours,
Then filter, to being passed through CO in filtrate2Filtered again after precipitated calcium, secondary filtrate is isolated through evaporative crystallization
Sylvite product.The leaching rate of this example potassium is 90.5%.The quantity of slag is 1.2 with the mass ratio of raw ore：1.
Embodiment 7
The water-insoluble potassium bearing rock that potassium content is 8.54% is crushed to 74 microns (200 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.5:0.2 mass ratio is sufficiently mixed, and is calcined 3 hours under conditions of 950 DEG C,
Product after roasting is gone out with water logging, with liquid-solid ratio 4 under the conditions of 80 DEG C:1 carries out magnetic agitation 2 hours, then mistake
Filter, to being passed through CO in filtrate2Filtered again after precipitated calcium, secondary filtrate is obtained into sylvite through evaporation, Crystallization Separation
Product.The leaching rate of this example potassium is 98.3%.The quantity of slag is 1 with the mass ratio of raw ore：1.
Embodiment 8
The water-insoluble potassium bearing rock that potassium content is 7.96% is crushed to 149 microns (100 mesh) below, Ran Houyu
Auxiliary agent CaCl2、Na2CO3By 1:0.4:0.3 mass ratio is sufficiently mixed, and is calcined 3 hours under conditions of 900 DEG C,
Product after roasting is gone out with water logging, with liquid-solid ratio 4 under the conditions of 80 DEG C:1 carries out magnetic agitation 2 hours, then mistake
Filter, filtrate obtains sylvite product through evaporation, Crystallization Separation.The leaching rate of this example potassium is 90.8%.The quantity of slag and raw ore
Mass ratio be 1.15：1.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from spirit of the invention and its essence,
Those of ordinary skill in the art can disclosure of the invention make various corresponding changes and deformation, but these phases
The change and deformation answered should all belong to scope of the claims of the invention.
Claims (10)
1. a kind of method that sylvite is extracted from water-insoluble potassium bearing rock, comprises the following steps：
1) with water-insoluble potassium bearing rock as raw material, CaCl is added2And Na2CO3As mixed flux, by original
Material is sufficiently mixed with mixed flux；Wherein, the raw material and CaCl2And Na2CO3By 1：(0.2-0.8)：
The mass ratio mixing of (0.05-0.3)；
2) by step 1) mixed material below 950 DEG C under conditions of be calcined 2-6 hours, the product after roasting
Gone out with water logging under the conditions of below 90 DEG C, leachate and filter residue are obtained through filtering；
3) by step 2) leachate obtain sylvite by evaporative crystallization.
2. it is according to claim 1 extract sylvite method, it is characterised in that step 1) raw material with
CaCl2And Na2CO3By 1：(0.3-0.6)：The mass ratio mixing of (0.1-0.3).
3. it is according to claim 1 extract sylvite method, it is characterised in that step 2) it is described roasting temperature
Spend is 750-900 DEG C.
4. it is according to claim 3 extract sylvite method, it is characterised in that step 2) it is described roasting temperature
Spend is 800-850 DEG C.
5. the method for the extraction sylvite according to claim 1,3 or 4, it is characterised in that step 2) it is described
Roasting time is 3-5 hours.
6. the method for extracting sylvite according to claim 1, it is characterised in that step 2) leaching
The solid mass ratio of liquid is (0.5-4)：1.
7. the method for extracting sylvite according to claim 6, it is characterised in that step 2) leaching
The solid mass ratio of liquid is (1-3)：1.
8. the method for the extraction sylvite according to claim 1,6 or 7, it is characterised in that step 2) it is described
The temperature of leaching is 70-90 DEG C.
9. the method for the extraction sylvite according to claim 1,6 or 7, it is characterised in that step 2) it is described
The time of leaching is 2-4 hours.
10. it is according to claim 1 extract sylvite method, it is characterised in that step 3) leachate is steamed
Deliming treatment is carried out before hair crystallization.
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| CN201510452200.5A CN106702139B (en) | 2015-07-28 | 2015-07-28 | A kind of method that sylvite is extracted from water-insoluble potassium bearing rock |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451528A (en) * | 2019-08-14 | 2019-11-15 | 包头钢铁（集团）有限责任公司 | A kind of nothing for extracting potassium chloride from k-rich slate is useless to utilize method |
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|---|---|---|---|---|
| CN1261601A (en) * | 1999-11-19 | 2000-08-02 | 乔希海 | Process for producing potassium chloride from alkaline slag and potassium feldspar |
| CN1298848A (en) * | 2001-01-17 | 2001-06-13 | 刘世永 | Process for preparing K fertilizer from non-soluble potassium ore and waste ammonia-soda solution |
| CN1298838A (en) * | 1999-12-04 | 2001-06-13 | 乔希海 | Process for preparing potassium chloride from alkali dregs and rock containing potassium |
| CN1321610A (en) * | 2000-04-30 | 2001-11-14 | 乔希海 | Method for preparing potassium chloride from adkaline residue and potassium-containing rock |
| CN1613762A (en) * | 2003-11-06 | 2005-05-11 | 乔希海 | Method for preparing molecular sieve by alkaline slag and potash feldspar |
| CN101062777A (en) * | 2006-04-28 | 2007-10-31 | 刘洪旺 | Technical method for extracting potassium chloride by comprehensive utilization of straw power generation ash slag and soda alkali waste slag |
| CN103937976A (en) * | 2014-02-26 | 2014-07-23 | 化工部长沙设计研究院 | Method used for preparing dissoluble potassium via decomposition desilication of potash feldspar |
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2015
- 2015-07-28 CN CN201510452200.5A patent/CN106702139B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1261601A (en) * | 1999-11-19 | 2000-08-02 | 乔希海 | Process for producing potassium chloride from alkaline slag and potassium feldspar |
| CN1298838A (en) * | 1999-12-04 | 2001-06-13 | 乔希海 | Process for preparing potassium chloride from alkali dregs and rock containing potassium |
| CN1321610A (en) * | 2000-04-30 | 2001-11-14 | 乔希海 | Method for preparing potassium chloride from adkaline residue and potassium-containing rock |
| CN1298848A (en) * | 2001-01-17 | 2001-06-13 | 刘世永 | Process for preparing K fertilizer from non-soluble potassium ore and waste ammonia-soda solution |
| CN1613762A (en) * | 2003-11-06 | 2005-05-11 | 乔希海 | Method for preparing molecular sieve by alkaline slag and potash feldspar |
| CN101062777A (en) * | 2006-04-28 | 2007-10-31 | 刘洪旺 | Technical method for extracting potassium chloride by comprehensive utilization of straw power generation ash slag and soda alkali waste slag |
| CN103937976A (en) * | 2014-02-26 | 2014-07-23 | 化工部长沙设计研究院 | Method used for preparing dissoluble potassium via decomposition desilication of potash feldspar |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110451528A (en) * | 2019-08-14 | 2019-11-15 | 包头钢铁（集团）有限责任公司 | A kind of nothing for extracting potassium chloride from k-rich slate is useless to utilize method |
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