CN112299450B - Method for preparing potassium chloride by grading crude potassium and potassium chloride prepared by applying method - Google Patents
Method for preparing potassium chloride by grading crude potassium and potassium chloride prepared by applying method Download PDFInfo
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- CN112299450B CN112299450B CN202011290711.9A CN202011290711A CN112299450B CN 112299450 B CN112299450 B CN 112299450B CN 202011290711 A CN202011290711 A CN 202011290711A CN 112299450 B CN112299450 B CN 112299450B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/22—Preparation in the form of granules, pieces, or other shaped products
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- 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
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Abstract
The invention discloses a method for preparing potassium chloride by crude potassium in a grading manner, which comprises the following steps: performing primary screening on coarse potassium ore pulp produced by a crystallizer of a reverse flotation-cold crystallization process through a first screening device to obtain primary oversize products and primary undersize products; the primary undersize is subjected to secondary screening through a second screening device to obtain secondary oversize containing sylvine and secondary undersize containing potassium chloride, and the secondary undersize is sent to a crude potassium thickener for producing potassium chloride; crushing the primary oversize material, and sending the crushed material into a feeding port of a reverse flotation-cold crystallization process after the crushed material reaches the feeding particle size standard of the reverse flotation-cold crystallization process; and (4) feeding the secondary oversize product into a recovery crystallizer, and feeding the secondary oversize product into a crude potassium thickener for producing potassium chloride after recrystallization. The invention divides the crude potassium ore pulp into two stages of screening, respectively carries out different treatments, and then carries out the production of potassium chloride, thereby recycling the potassium chloride in the crude potassium ore pulp and improving the recovery rate of KCl in the crude potassium ore pulp to be more than 90 percent.
Description
Technical Field
The invention relates to the technical field of potassium chloride production, in particular to a method for preparing potassium chloride by grading crude potassium and potassium chloride prepared by applying the method.
Background
The potassium resource of China widely exists in remote areas such as Qinghai and the like, wherein the reserves of Qinghai account for more than 50 percent of the reserves of China, the representative resource is salt lake resource, the salt lake resource mainly comprises deposition resource and brine resource, the salt lake brine belongs to liquid chloride mineral resource and is rich in various components, the salt lake brine utilizes carnallite with rich content to process and prepare potassium chloride to produce the potassium fertilizer, the potassium fertilizer is one of three chemical fertilizers of nitrogen and phosphorus and potassium, the potassium element has obvious effect on regulating the life process in plants, the potassium fertilizer is favorable for improving the absorption condition of water in the plants and the synthesis and transfer of saccharides, and the yield and the quality of crops can be effectively improved by using the potassium fertilizer.
The processes for producing the potash fertilizer by using the carnallite raw ore in the salt lake brine are various, and the reverse flotation-cold crystallization process is an advanced process in large-scale production. The raw ore comprises pure carnallite and a certain amount of sodium chloride, when the potash fertilizer is produced, a flotation reagent is added into a saturated flotation medium of the raw ore, the hydrophobicity of the surface of the sodium chloride is selectively increased without increasing the hydrophobicity of the carnallite, the sodium chloride is separated out along with foam, the carnallite is left in ore pulp, the low-sodium carnallite with lower sodium content is obtained after dehalogenation, the low-sodium carnallite enters a crystallizer, water is added for decomposition and crystallization, the decomposition condition is controlled, the potassium chloride in the solution is supersaturated, the supersaturation degree of a carnallite decomposition system is utilized to grow potassium chloride crystal particles to obtain crude potassium slurry, and the crude potassium slurry is obtained through the processes of filtering, washing and the like, so that the produced potassium chloride product has large content, high particle size and low moisture.
The crystallizer is a core procedure in the reverse flotation-cold crystallization process, and the quality of the crude potassium after crystallization directly influences the product yield and the product quality of the whole process. Because of different natural growth periods and different sizes of crystal grain sizes of raw ores, the raw ores with larger grain sizes are difficult to be completely decomposed in the process of decomposing the raw ores by the crystallizer, in order to ensure the quality of the crude potassium ore pulp, the crude potassium ore pulp produced by the crystallizer is usually screened into undersize and oversize, the undersize is used as crude potassium slurry to enter a crude potassium thickener to be subjected to subsequent processes for producing potassium chloride, the oversize and overflow liquid of the crude potassium thickener are discharged to a tail salt pond together, the recovery rate of potassium chloride in the process is only 60%, and 40% of potassium chloride is discharged to the tail salt pond along with the overflow of the crude potassium thickener.
Disclosure of Invention
The invention aims to provide a method for preparing potassium chloride by grading crude potassium and potassium chloride, and aims to solve the problem of low potassium chloride recovery rate caused by directly discharging oversize products of the crude potassium to a tail salt pool in the existing potassium fertilizer production method.
In order to achieve the above purpose, the invention provides the following technical scheme: a method for preparing potassium chloride by crude potassium classification comprises the following steps:
s1, performing primary screening on coarse potassium ore pulp produced by a crystallizer in a reverse flotation-cold crystallization process through a first screening device to obtain primary oversize products and primary undersize products;
s2, performing secondary screening on the primary undersize product through a second screening device to obtain a secondary oversize product containing sylvite and a secondary undersize product containing potassium chloride, and feeding the secondary undersize product into a crude potassium thickener for producing potassium chloride;
s3, crushing the primary oversize products by a crushing device, and sending the crushed primary oversize products into a feed inlet of the reverse flotation-cold crystallization process after the crushed primary oversize products reach the feed particle size standard of the reverse flotation-cold crystallization process;
and S4, feeding the secondary oversize product into a recovery crystallizer, and feeding the secondary oversize product into the crude potassium thickener for producing potassium chloride after recrystallization.
Further, in step S1, the first screening device is a first vibrating screen.
Further, the screen mesh diameter of the first vibrating screen is not less than 0.8mm.
Further, in step S2, the second screening device is a second vibrating screen.
Further, the screen mesh diameter of the second vibrating screen is not more than 0.6mm.
Further, the second screening device is arranged below the first screening device.
Further, in step S2, the feeding the secondary undersize to a crude potassium thickener for producing potassium chloride includes:
feeding the secondary undersize product into a crude potassium thickener to obtain a first underflow and a first overflow liquid, feeding the first underflow into a first solid-liquid separation device, and merging the first overflow liquid into the secondary oversize product;
the first underflow is subjected to solid-liquid separation by the first solid-liquid separation device to obtain a first solid phase and a first liquid phase;
the first solid phase and water are repulped and washed in a repulping and washing device to obtain serous fluid, and the serous fluid is sent to a second solid-liquid separation device;
and performing solid-liquid separation on the slurry by using the second solid-liquid separation device to obtain a second solid phase and a second liquid phase, wherein the second solid phase is a potassium chloride finished product.
Further, the first liquid phase is returned to the crude potassium thickener.
And further, feeding the second liquid phase into a refined potassium thickener to obtain a second underflow and a second overflow liquid, feeding the second underflow into the repulping washing device, and feeding the second overflow liquid into the crystallizer.
The invention also provides potassium chloride produced by the method for preparing the potassium chloride by grading the crude potassium according to any one of the above methods.
Compared with the prior art, the method for preparing the potassium chloride by grading the crude potassium has the following advantages:
the coarse potassium ore pulp is divided into two stages for screening to obtain a primary oversize product containing large-particle-size carnallite raw ore, a secondary oversize product containing sylvinite and a secondary undersize product containing potassium chloride, the large-particle-size particles are crushed, the medium-particle-size particles are subjected to cold crystallization, the small-particle-size particles are concentrated, different treatments are respectively carried out, and then the potassium chloride is produced, so that the potassium chloride in the potassium ore pulp is recovered, the recovery rate of KCl in the coarse potassium can be improved to more than 90%, the production efficiency is improved, and the loss of potassium resources is reduced.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. In the drawings:
fig. 1 is a process flow diagram of a method for preparing potassium chloride by crude potassium classification according to a preferred embodiment of the invention.
Reference numerals:
1 crystallizer, 2 first screening device, 3 second screening device, 4 coarse potassium thickener, 41 first solid-liquid separation device, 42 repulping and washing device, 43 second solid-liquid separation device, 44 fine potassium thickener, 5 feeding port, 6 recovery crystallizer and 7 crushing device.
Detailed Description
The present invention provides many applicable inventive concepts that can be embodied in a wide variety of specific contexts. The specific examples described in the following embodiments of the present invention are merely illustrative of specific embodiments of the present invention and do not limit the scope of the invention.
The invention is further described with reference to the following figures and detailed description of embodiments.
As shown in fig. 1, fig. 1 is a process flow chart of a method for preparing potassium chloride by crude potassium classification according to a preferred embodiment of the invention.
The method for preparing the potassium chloride by grading the crude potassium comprises the following steps:
s1, performing primary screening on the coarse potassium ore pulp produced by the crystallizer 1 of the reverse flotation-cold crystallization process through a first screening device 2 to obtain primary oversize products and primary undersize products;
s2, performing secondary screening on the primary undersize product through a second screening device 3 to obtain a secondary oversize product containing sylvine and a secondary undersize product containing potassium chloride, and feeding the secondary undersize product into a crude potassium thickener 4 for producing potassium chloride;
s3, crushing the primary oversize products by a crushing device 7, and sending the crushed primary oversize products into a material inlet 5 of the reverse flotation-cold crystallization process after the crushed primary oversize products reach the material inlet particle size standard of the reverse flotation-cold crystallization process;
and S4, sending the secondary oversize product into a recovery crystallizer 6, and sending the secondary oversize product into the crude potassium thickener 4 for producing potassium chloride after recrystallization.
In the related technology, oversize products (the screening particle size is 0.6 mm) obtained after screening the crude potassium ore pulp produced by the crystallizer are directly discharged to a tailing pond, and the recovery rate of potassium chloride is lower by 60 percent, and the research of the invention finds that particles with large particle size (the particle size is more than 0.8 mm) in the oversize products are carnallite raw ore and still contain large content of potassium chloride and sodium chloride as shown in table 1; the medium size (between 0.6 and 0.8 mm) particles are sylvite, still containing a significant amount of potassium chloride and sodium chloride.
Therefore, the coarse potassium ore pulp is divided into two stages for sieving to obtain a primary oversize product containing the carnallite raw ore with large particle size, a secondary oversize product containing sylvite and a secondary undersize product containing potassium chloride, the particles with large particle size are crushed, the particles with medium particle size are subjected to cold crystallization, the particles with small particle size are concentrated and respectively subjected to different treatments, and then the potassium chloride is produced, so that the potassium chloride in the potassium ore pulp is recovered, the recovery rate of KCl in the coarse potassium ore pulp can be increased to more than 90%, the production efficiency is improved, and the loss of potassium resources is reduced.
The invention aims at the crude potassium ore pulp produced by a special process, namely a reverse flotation-cold crystallization process, and the crude potassium ore pulp is found to be different components according to different particle sizes and is classified by screening devices with different sizes, wherein the particles with small particle sizes have the highest content of potassium chloride, the particles with medium particle sizes are sylvite and have the second highest content of potassium chloride, the particles with large particle sizes are carnallite raw ore and have the highest content of potassium chloride; if the coarse potassium ore pulp is completely thickened and potassium chloride is produced, the particles with medium particle size and large particle size cannot be decomposed and utilized, the potassium chloride is wasted, and the recovery rate of the potassium chloride is low; if all the particles in the coarse potassium ore pulp are crushed, the particles with small particle size and medium particle size are not needed, and the complex process and material loss are caused; if the particles in the coarse potassium ore pulp are screened for the first time, part of potassium chloride is wasted, and the recovery rate of the potassium chloride is reduced.
TABLE 1 screening data
| Range of particle size | Particle size% | KCl％ | MgCl 2 ％ | CaSO 4 ％ | NaCl％ |
| 2-2.4mm | 0.67％ | 21.57 | 31.69 | 0.26 | 21.39 |
| 0.8-2mm | 5.36％ | 19.36 | 27.46 | 0.24 | 17.09 |
| 0.6-0.8mm | 20.66％ | 33.08 | 17.46 | 0.48 | 39.63 |
| ＜0.6mm | 73.31％ | 75.41 | 4.85 | 0.13 | 5.69 |
| Fixed weight | 100.00％ | - | - | - | - |
| Not sieved | - | 66.92 | 7.65 | 0.16 | 8.81 |
In the step S1, the reverse flotation-cold crystallization process comprises the following steps: carnallite raw ore reaching the feed particle size standard enters the feed inlet 5, the feed inlet 5 is a feed inlet of a raw ore thickener or a feed inlet of a flotation pulp mixing tank, low-sodium carnallite with low sodium content is obtained after reverse flotation, the low-sodium carnallite enters the crystallizer 1 again, and water is added for decomposition and crystallization to obtain the crude potassium slurry.
The feeding particle size standard is set according to a process, and in the embodiment, the feeding particle size standard is that the particle size of the carnallite raw ore is not more than 0.8mm, and the ratio is not less than 80%.
The first screening device 2 is a first vibrating screen. The particles with different particle diameters are separated through the vibrating screen, so that the damage of large-particle materials to the screen is avoided when the large-particle materials are centrifugally separated through a centrifugal machine.
The screen mesh diameter of the first vibrating screen is not less than 0.8mm. The screen mesh aperture of the first vibrating screen is set according to actual production, in this embodiment, the screen mesh aperture of the first vibrating screen is 0.8mm, and the primary oversize product obtained after primary screening is carnallite raw ore with larger particle size and which is not utilized.
In step S2, the second screening device 3 is a second vibrating screen. The particles with different particle diameters are separated through the vibrating screen, so that the damage of large-particle materials to the screen is avoided when the large-particle materials are centrifugally separated through a centrifugal machine.
The screen mesh diameter of the second vibrating screen is not more than 0.6mm. The screen mesh size of the second vibrating screen is set according to actual production, in this embodiment, the screen mesh size of the second vibrating screen is 0.6mm, and the secondary oversize product obtained after secondary screening is sylvite with a medium particle size and is not utilized.
The second screening device 3 is arranged below the first screening device 2. During the classifying and screening, the crude potassium ore pulp can flow through the first screening device 2 and the second screening device 3 from top to bottom, and first-level undersize materials are rapidly screened without being transported, so that the screening time is shortened.
In step S2, the step of feeding the secondary undersize into the crude potassium thickener 4 for producing potassium chloride includes:
feeding the secondary undersize product into a crude potassium thickener 4 to obtain a first underflow and a first overflow liquid, feeding the first underflow into a first solid-liquid separation device 41, and merging the first overflow liquid into the secondary oversize product;
the first underflow is subjected to solid-liquid separation by the first solid-liquid separation device 41 to obtain a first solid phase and a first liquid phase; the first liquid phase is returned to the crude potassium thickener 4 for recycling;
the first solid phase and water are repulped and washed in a repulping and washing device 42 to obtain a slurry, and the slurry is sent to a second solid-liquid separation device 43;
and performing solid-liquid separation on the slurry by using the second solid-liquid separation device 43 to obtain a second solid phase and a second liquid phase, wherein the second solid phase is a potassium chloride finished product.
And feeding the second liquid phase into a refined potassium thickener 44 to obtain a second underflow and a second overflow liquid, feeding the second underflow into the repulping and washing device 42, and feeding the second overflow liquid into the crystallizer 1.
In the step S3, the primary oversize products are crushed by the crushing device 7, processed into particles with small particle size, and re-enter the reverse flotation-cold crystallization process to recycle potassium chloride in the particles.
In step S4, the secondary oversize product is subjected to cold crystallization by the recovery crystallizer 6 to recycle potassium chloride therein.
In this embodiment, the liquid phase in each stage is recovered, on one hand, the unused potassium chloride in the liquid phase can be recovered and utilized again, the flotation reagent carried by the coarse potassium ore pulp in the reverse flotation process can be recovered and utilized, and of course, the liquid phase in a certain stage can be discharged to the tailing salt pond according to the requirements of the production process.
The invention also provides potassium chloride produced by the method for preparing the potassium chloride by grading the crude potassium.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and that those skilled in the art will be able to design alternative embodiments without departing from the scope of the appended claims. In the claims, any reference signs placed between parentheses shall not be construed as limiting the claim. The word "comprising" does not exclude the presence of elements or steps not listed in a claim.
Claims (3)
1. A method for preparing potassium chloride by crude potassium in a grading manner is characterized by comprising the following steps: the method comprises the following steps:
s1, performing primary screening on the coarse potassium ore pulp produced by the crystallizer (1) of the reverse flotation-cold crystallization process through a first screening device (2) to obtain primary oversize products and primary undersize products;
s2, performing secondary screening on the primary undersize product through a second screening device (3) to obtain a secondary oversize product containing sylvine and a secondary undersize product containing potassium chloride, sending the secondary undersize product into a crude potassium thickener (4) to obtain a first bottom flow and a first overflow liquid, sending the first bottom flow into a first solid-liquid separation device (41), and merging the first overflow liquid into the secondary oversize product,
the first underflow is subjected to solid-liquid separation by the first solid-liquid separation device (41) to obtain a first solid phase and a first liquid phase,
the first solid phase and water are repulped and washed in a repulping and washing device (42) to obtain serous fluid, the serous fluid is sent into a second solid-liquid separation device (43) for solid-liquid separation to obtain a second solid phase and a second liquid phase, the second solid phase is a potassium chloride finished product,
said first liquid phase is returned to said crude potassium thickener (4);
s3, crushing the primary oversize material by using a crushing device (7), and sending the crushed material into a feeding port (5) of the reverse flotation-cold crystallization process after the crushed material reaches the feeding particle size standard of the reverse flotation-cold crystallization process;
s4, feeding the secondary oversize product and the first overflow liquid into a recovery crystallizer (6), re-crystallizing, feeding into the crude potassium thickener (4) for producing potassium chloride,
wherein in the step S1, the first screening device (2) is a first vibrating screen, the aperture of the screen mesh of the first vibrating screen is 0.8mm,
in the step S2, the second screening device (3) is a second vibrating screen, and the screen mesh diameter of the second vibrating screen is 0.6mm.
2. The method for preparing potassium chloride by crude potassium classification as claimed in claim 1, characterized in that: wherein the second screening device (3) is arranged below the first screening device (2).
3. The method for preparing potassium chloride by crude potassium classification as claimed in claim 1, characterized in that: and feeding the second liquid phase into a refined potassium thickener (44) to obtain a second underflow and a second overflow liquid, feeding the second underflow into the repulping washing device (42), and feeding the second overflow liquid into the crystallizer (1).
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