CN117003259A - Production method of potassium chloride - Google Patents
Production method of potassium chloride Download PDFInfo
- Publication number
- CN117003259A CN117003259A CN202211209585.9A CN202211209585A CN117003259A CN 117003259 A CN117003259 A CN 117003259A CN 202211209585 A CN202211209585 A CN 202211209585A CN 117003259 A CN117003259 A CN 117003259A
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- Prior art keywords
- ore
- desliming
- potassium chloride
- crystallizer
- crystallization
- Prior art date
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 101
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 51
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- PALNZFJYSCMLBK-UHFFFAOYSA-K magnesium;potassium;trichloride;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-].[Cl-].[K+] PALNZFJYSCMLBK-UHFFFAOYSA-K 0.000 claims abstract description 28
- 238000002425 crystallisation Methods 0.000 claims abstract description 25
- 230000008025 crystallization Effects 0.000 claims abstract description 25
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000012452 mother liquor Substances 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000005188 flotation Methods 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 12
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 27
- 239000013078 crystal Substances 0.000 claims description 23
- 238000001953 recrystallisation Methods 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 3
- 239000002689 soil Substances 0.000 abstract description 15
- 238000005406 washing Methods 0.000 abstract description 12
- 230000002411 adverse Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009825 accumulation Methods 0.000 abstract description 2
- 239000004927 clay Substances 0.000 description 3
- 239000013505 freshwater Substances 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000012267 brine Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000010413 mother solution Substances 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C01D3/14—Purification
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a production method of potassium chloride, which comprises the following steps: crushing and desliming carnallite ore, and desliming the ore by using a saturated solution of magnesium chloride; and crystallizing, namely mixing the desliming ore, water and system mother liquor, and then feeding the mixture into a crystallizer for dissolution and crystallization. According to the invention, the ore is cleaned to remove the soil before the crystallization step, so that the soil of the ore entering the crystallization and flotation process can be timely removed, the accumulation of soil particles in the crystallization and flotation process and the adverse effect of the soil particles on the crystallization flotation process are avoided, and the whiteness of the potassium chloride product is improved. Meanwhile, the system mother liquor is adopted to desliming the ore, so that the washing water consumption can be reduced, the tail liquor treatment capacity is reduced, the ore is prevented from being decomposed in the desliming stage, and the dissolution in the crystallizer is completed at one time.
Description
Technical Field
The invention belongs to the field of extraction of potassium chloride, and particularly relates to a method for producing potassium chloride by using carnallite ore.
Background
Potassium chloride is an indispensable fertilizer for agricultural production, and is also an important ore in the industries of chemical engineering, metallurgy, medicine, food and the like. The ores for producing potassium chloride mainly comprise sylvite, carnallite and the like. The carnallite resources are rich, but the potassium content of the carnallite is generally lower than that of the potassium salt, the processing energy consumption is higher, and the proportion of the carnallite in the potassium chloride production is not large. Carnallite is largely classified into natural carnallite and salt lake carnallite according to the formation process of carnallite. The carnallite in salt lake is prepared by sun-curing for one year, and is easy to crush and dissolve. The natural carnallite, especially Laos carnallite, has been under the ground for over 6800 thousands of years, and the crushing and dissolving difficulties are about 10 times of those of salt lake carnallite. Most of carnallite ores utilized in the current production of potassium chloride are salt lake carnallite.
The existing process for producing potassium chloride by using carnallite raw ore generally comprises the steps of crushing, crystallizing, floating, then performing a brine washing process, and removing soil and insoluble impurities through brine washing to obtain the potassium chloride.
The existing method has the defects of low utilization rate of carnallite, large water consumption and low grade of prepared potassium chloride.
Disclosure of Invention
The improved production method of potassium chloride can improve the utilization rate of carnallite, reduce water consumption and improve the grade of potassium chloride.
The invention provides a production method of potassium chloride, which comprises the following steps: crushing and desliming carnallite ore, and desliming the ore by using a saturated solution of magnesium chloride; crystallizing, namely mixing the desliming ore, water and system mother liquor, and then feeding the mixture into a crystallizer for dissolution and crystallization.
According to an embodiment of the present invention, in the crushing and desliming step, the carnallite ore is crushed to have a particle size of 20mm or less, and then desliming is performed thereon, and then the desliming ore is subjected to rod milling to form particles of 1mm or less.
According to another embodiment of the invention, the saturated solution of magnesium chloride is a system mother liquor.
According to another embodiment of the invention, the solids mass content in the desliming step is 50% -60%.
According to another embodiment of the present invention, in the crystallization step, overflow of the crystallizer enters a solid-liquid separation device to perform solid-liquid separation, the separated solids enter a recrystallization device to further crystallize, and both bottom flow of the crystallizer and bottom flow of the recrystallization device enter a flotation step to perform flotation.
According to another embodiment of the invention, in the crystallization step, the mass ratio of the desliming ore, water and system mother liquor in the crystallizer is 1:0.2-0.35:4-6.5; preferably 1:0.25 to 0.35:4 to 6.
According to another embodiment of the invention, the saturated solution of magnesium chloride is a system mother liquor.
According to another embodiment of the invention, the recrystallization vessel is replenished with liquid by means of a system mother liquor.
According to another embodiment of the invention, the potassium chloride grain size in the crystallizer and the recrystallization underflow is greater than 0.15mm over 70%.
According to the invention, the ore is cleaned to remove the soil before the crystallization step, so that the soil of the ore entering the crystallization and flotation process can be timely removed, the accumulation of soil particles in the crystallization and flotation process and the adverse effect of the soil particles on the crystallization flotation process are avoided, and the whiteness of the potassium chloride product is improved. Meanwhile, the system mother liquor is adopted to desliming the ore, so that the washing water consumption can be reduced, the tail liquor treatment capacity is reduced, the ore is prevented from being decomposed in the desliming stage, and the dissolution in the crystallizer is completed at one time.
Drawings
FIG. 1 is a schematic flow chart of an embodiment of the present invention.
Fig. 2 is a schematic flow chart of another embodiment of the present invention.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The inventor finds that carnallite ore inevitably carries soil, soil particles are crystal nuclei after the soil enters a crystallization process, and the excessive crystal nuclei influence the production of potassium chloride crystal nuclei, thereby influencing the granularity of the potassium chloride. In the flotation process, in order to avoid the influence of soil particles on the positive flotation, a clay sludge inhibitor and the like are added to inhibit the adverse influence of soil on the flotation process, and even if the soil particles are mixed into the potassium chloride, the whiteness of the potassium chloride product is affected inevitably. Meanwhile, a large amount of water is needed for removing the inhibitor in the subsequent cleaning of the crude potassium chloride, and the washing process using a large amount of water not only consumes a large amount of water, but also causes dissolution of the potassium chloride to be lost, thereby resulting in low yield of the potassium chloride. The inventor improves the prior art through research, and desliming is carried out on crushed ore by using system mother liquor, so that the clay particles are prevented from entering crystallization and floatation processes, adverse effects of the clay particles on the two processes are avoided, whiteness can be improved, water consumption is reduced, and the yield of potassium chloride is improved.
As shown in FIG. 1, the method for producing potassium chloride provided by the invention comprises the following steps: crushing and desliming carnallite ore, and desliming the ore by using a saturated solution of magnesium chloride; and crystallizing, namely mixing the desliming ore, water and system mother liquor, and then feeding the mixture into a crystallizer for crystallization.
The term "system mother liquor" in this patent refers to the liquid discharged from the system, such as the liquid separated from the crude potassium band pass, the liquid separated from the tail salt band pass, and the historically retained liquid discharged from the system. The "system mother liquor" is a saturated solution of magnesium chloride.
Specifically, in the crushing and desliming step, ore is crushed and sieved first, and the undersize (the undersize may be selected to have an appropriate crushing particle size, for example, but not limited to, 20mm or less, 15mm or less, 10mm or less, 5mm or less, etc. as required) is washed, and the oversize is returned to the crushing process again to continue crushing. And (3) washing the crushed ore by adopting a system mother solution in the washing process.
The system mother liquor is adopted to desliming the crushed ore, so that the washing water consumption can be reduced, the tail liquid treatment capacity is reduced, and meanwhile, the ore can be prevented from being decomposed in the desliming stage, so that the dissolution is completed in the crystallizer at one time.
After washing, the ore is sieved, and the oversize (1 mm or more) is further crushed. Crushing is preferably a rod mill by which the ore is crushed into particles of less than 1mm to facilitate dissolution of the ore in the crystallizer. The undersize (less than or equal to 1 mm) flows into a solid-liquid separation device, the solid enters a crystallization unit, the liquid flows into a filtering device for filtering and desliming, and the liquid after mud cake removal is returned to the washing process for reuse. Since the underflow from each step will carry away a portion of the mother liquor, the wash process can be liquid replenished by the system mother liquor. The mass content of the solid in the washing process is 50-60%, so that the ore can be fully washed to the maximum extent.
In alternative embodiments, the crystallization step may comprise the reuse of fine grains in the overflow of the crystallizer. This embodiment is explained in detail with reference to fig. 2. As shown in fig. 2, the steps of crushing and desliming are the same as those of the embodiment shown in fig. 1, and the detailed description thereof will not be repeated.
The undersize (less than or equal to 1 mm) after rod milling enters a crystallizer, the ore washed in the crystallizer is decomposed, and potassium chloride is separated out under the action of saturated solution of magnesium chloride. The precipitated potassium chloride grows up gradually and flows from the underflow into the flotation unit. The overflow of the crystallizer comprises fine crystals of not-grown and fine crystal grains, and the fine crystals enter the recrystallization device through underflow after solid-liquid separation. In the recrystallization device, fine crystals grow secondarily, and after reaching a preset size, the fine crystals enter a flotation unit from the bottom flow for flotation. Since the underflow contains a certain amount of mother liquor, after the crystallizer underflow and the recrystallization underflow are discharged, the liquid content in the crystallizer and the recrystallization are reduced, and the crystallizer and the recrystallization can be replenished with liquid by the system mother liquor.
In the crushing and desliming step, the washed undersize can enter a crystallizer after being filtered and thickened, also enter a recrystallization device, also can enter a crystallizer partially, and can enter the recrystallization device partially, and can be determined according to actual operation conditions. The fine grains are reused in the recrystallization device, so that the yield of the potassium chloride can be improved.
The invention washes ore and supplements liquid for crystallizer and recrystalliser by system mother liquid, which can fully utilize system mother liquid and avoid the 'explosion crystal' generated by supplementing fresh water in crystallization process, thereby affecting the crystal nucleus growth and the production efficiency of potassium chloride. The process of 'bursting crystal' refers to that fresh water is added to separate the crystal into more fine crystal grains, so that the number of crystal nuclei is rapidly increased, and further growth of the crystal nuclei is not facilitated.
The liquid separated by the solid-liquid separation device contains finer potassium chloride, and after the liquid enters the fine-grain tank, fresh water is added to dissolve potassium chloride crystals in the liquid to form unsaturated solution of potassium chloride, and the solution enters the crystallizer to dissolve crushed ore entering the crystallizer. The mass ratio of the crushed ore to the saturated solution of water and magnesium chloride in the crystallizer is 1:0.2-0.35:4-6.5. Preferably 1:0.25 to 0.35:4 to 6.
In an alternative embodiment, the saturated solution of magnesium chloride may be the system mother liquor.
In an alternative embodiment, the potassium chloride grain size in the crystallizer and recrystallization underflow is greater than 0.15mm over 70%.
In an alternative embodiment, the carnallite ore may be an ore such as laos carnallite ore.
The invention is further described below by means of specific examples. These examples are merely exemplary and are not intended to limit the scope of the present invention in any way.
In the following examples and comparative examples, reagents, materials and instruments used, unless otherwise specified, were commercially available.
Example 1
Crushing 10kg of Laos carnallite into particles with the particle size of 5-20 mm in a crushing unit. And desliming the crushed ore by using a system mother solution, wherein the mass content of solids in the desliming step is 60%. The ore subjected to desliming is further subjected to rod grinding to form particles smaller than or equal to 1mm, the particles enter a crystallizer for crystallization, the crystallization process is dissolving in a central cylinder of the crystallizer, fine crystals enter a crystallization area through a guide cylinder, a part of potassium chloride crystal nuclei grow, and the potassium chloride crystal nuclei fall to the bottom of the crystallizer due to gravity and are sent to a size mixing tank through underflow; and discharging a part of potassium chloride crystal nucleus to solid-liquid separation equipment through an overflow port under the action of fluid to perform solid-liquid separation, enabling potassium chloride fine crystals to enter a recrystallization device, and enabling the potassium chloride fine crystals to enter a slurry mixing tank through a bottom flow port after recrystallization. The crystallizer underflow enters a flotation unit. The grain diameter of potassium chloride in the bottom flow of the crystallizer is more than 0.15mm and the ratio is 70 percent.
And in a flotation unit, performing flotation by taking octadecylamine as a flotation agent, and finally washing, drying, weighing and testing the purity of the obtained crude potassium chloride.
The yield of potassium chloride in this example was calculated to be 82.0% and the water usage was 2.8kg. The purity of the obtained potassium chloride was 98.2%.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
1. A method for producing potassium chloride, comprising:
crushing and desliming carnallite ore, and desliming the ore by using a saturated solution of magnesium chloride; and
Crystallizing, namely mixing the desliming ore, water and system mother liquor, and then feeding the mixture into a crystallizer for dissolution and crystallization.
2. The production method according to claim 1, wherein in the crushing and desliming step, the carnallite ore is crushed to a particle size of 20mm or less, and then desliming is performed thereon, and thereafter the desliming ore is subjected to rod milling to form particles of 1mm or less.
3. The method of claim 1, wherein the saturated solution of magnesium chloride is a system mother liquor.
4. The method of claim 1, wherein the solids content in the desliming step is 50-60% by mass.
5. The production method according to claim 1, wherein in the crystallization step, overflow of the crystallizer enters a solid-liquid separation device for solid-liquid separation, and the separated solid enters a recrystallization device for further crystallization.
6. The method according to claim 5, wherein in the crystallization step, the mass ratio of the desliming ore, water and system mother liquor in the crystallizer is 1:0.2-0.35:4-6.5; preferably 1:0.25 to 0.35:4 to 6.
7. The method for producing potassium chloride according to claim 5, wherein said saturated solution of magnesium chloride is a system mother liquor.
8. The method for producing potassium chloride according to claim 5, wherein said recrystallization vessel is supplemented with a liquid by a system mother liquor.
9. The method for producing potassium chloride according to claim 5, wherein both the underflow of the crystallizer and the underflow of the recrystallization vessel are subjected to a flotation step for flotation.
10. The method for producing potassium chloride according to claim 9, wherein the crystal grain diameter of potassium chloride in the underflow of said crystallizer and said recrystallization is more than 0.15mm and 70% or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211209585.9A CN117003259A (en) | 2022-09-30 | 2022-09-30 | Production method of potassium chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211209585.9A CN117003259A (en) | 2022-09-30 | 2022-09-30 | Production method of potassium chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117003259A true CN117003259A (en) | 2023-11-07 |
Family
ID=88562487
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211209585.9A Pending CN117003259A (en) | 2022-09-30 | 2022-09-30 | Production method of potassium chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117003259A (en) |
-
2022
- 2022-09-30 CN CN202211209585.9A patent/CN117003259A/en active Pending
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