CN114956125A - Method for improving yield of potassium chloride produced from fine-grain high-sodium carnallite - Google Patents
Method for improving yield of potassium chloride produced from fine-grain high-sodium carnallite Download PDFInfo
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- CN114956125A CN114956125A CN202210590971.0A CN202210590971A CN114956125A CN 114956125 A CN114956125 A CN 114956125A CN 202210590971 A CN202210590971 A CN 202210590971A CN 114956125 A CN114956125 A CN 114956125A
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- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 180
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 90
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 90
- 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 title claims abstract description 74
- 239000011734 sodium Substances 0.000 title claims abstract description 63
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 43
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 108
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 108
- 239000007788 liquid Substances 0.000 claims abstract description 95
- 239000011780 sodium chloride Substances 0.000 claims abstract description 54
- 238000005188 flotation Methods 0.000 claims description 31
- 238000005406 washing Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 7
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000007790 solid phase Substances 0.000 claims description 6
- 230000007246 mechanism Effects 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000012530 fluid Substances 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 239000013078 crystal Substances 0.000 abstract description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 5
- 230000003993 interaction Effects 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 description 27
- 239000000243 solution Substances 0.000 description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 9
- 239000013505 freshwater Substances 0.000 description 9
- 239000011591 potassium Substances 0.000 description 9
- 229910052700 potassium Inorganic materials 0.000 description 9
- 239000012452 mother liquor Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012267 brine Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for improving yield of potassium chloride produced by fine-grained high-sodium carnallite ore, which comprises the steps of respectively adding fine-grained high-sodium carnallite and decomposition liquid into a decomposition area of a crystallizer, wherein MgCl is contained in the decomposition liquid 2 The concentration of the sodium carnallite is 17-21%, the adding positions of the fine sodium carnallite and the decomposition liquid are two ends of the decomposition area which are farthest away, the fine sodium carnallite and the decomposition liquid are respectively added into the decomposition area through a sleeve, the upper end surface of the sleeve is higher than the liquid level in the decomposition area, and the lower end surface of the sleeve is positioned below the liquid level in the decomposition area. According to the invention, through the arrangement of the sleeve and the increase of the distance between the feeding position of the decomposition liquid and the feeding position of the high-fine-grain high-sodium carnallite, the local concentration can be improved, and then the dissolution and precipitation amount of sodium chloride can be reduced by increasing the concentration of the decomposition liquid and improving the local concentration, the degree of the interaction between potassium chloride and sodium chloride crystals can be reduced, and the grade of potassium chloride can be further improved.
Description
Technical Field
The invention relates to the technical field of processes for preparing potassium chloride by decomposing fine-grained high-sodium carnallite, in particular to a method for improving the yield of potassium chloride produced by fine-grained high-sodium carnallite ore.
Background
Potassium chloride is an important chemical product, has important application in the fields of agriculture, food and medicine, and especially has very important position in the field of agriculture as a potassium fertilizer. One of the processes for producing potassium chloride by using carnallite as a raw material is cold crystallization-direct flotation. The process of producing potassium chloride by the cold crystallization-direct flotation process requires decomposing carnallite with decomposition liquid, which is usually unsaturated mother liquor (MgCl at 25 deg.C) 2 Percent is less than or equal to 25 percent) and the main principle is that carnallite and water are in contact with each other and decomposed to form potassium chloride and magnesium chloride coexisting solution, potassium chloride is separated out from the solution to form potassium chloride crystals along with the increase of the concentration of the magnesium chloride, the decomposed potassium chloride and mother liquor are discharged out of a crystallizer along with underflow, the underflow separates potassium chloride and other salts through flotation, the flotation process is composed of three processes of roughing, primary concentration and secondary concentration in series, and the floated potassium chloride crystals are washed and dried to form potassium chloride products.
The salt lake brine is evaporated in a salt pan to obtain carnallite, wherein a certain amount of carnallite with 10-35% of sodium chloride and 70-90% of sodium chloride with the particle size of less than 0.25mm in the total sodium chloride is always formed, and the carnallite is called as fine-grain sodium chloride carnallite.
Research shows that 'fine sodium chloride carnallite' is used as a raw material, a 'cold crystallization-direct flotation' process is adopted to produce potassium chloride, sodium chloride in the carnallite participates in the dissolving and separating-out process in the decomposition and crystallization process, the dissolution rate of the fine sodium chloride is high, the separation amount of sodium chloride crystals is large, when potassium chloride and sodium chloride are crystallized simultaneously, the two crystals are adhered and mixed due to interaction, the sodium chloride and potassium chloride crystals which interact with each other cannot be separated in the flotation process, and the sodium chloride crystals enter the potassium chloride along with the flotation, so that the grade of the potassium chloride is reduced. The standard of fertilizer grade potassium chloride GB/T37918-2019 has a new higher standard for the sodium chloride content in potassium chloride, and the sodium chloride content in powdery crystalline and granular potassium chloride is required to be less than or equal to 1 percent of type I, less than or equal to 3 percent of type II and less than or equal to 4 percent of type III. In order to obtain a qualified potassium chloride product, the amount of washing fresh water needs to be increased in the washing process to elute sodium chloride, and potassium chloride is dissolved simultaneously in the process, so that the potassium yield is reduced.
The technological scheme of producing potassium chloride with cold crystallization-positive floatation process includes 1 compounding decomposed liquid with mother liquid from tail salt pond or salt field, MgCl 2 The concentration is 10-15%; 2. decomposing carnallite in a crystallizer by adopting the decomposition liquid; 3. the feeding positions of the decomposition liquid and the carnallite ore are both in the middle of the decomposition area of the crystallizer; 4. separating potassium chloride and other salts from the decomposed bottom flow by flotation; 5. the flotation process consists of rough concentration, primary concentration and secondary concentration; 6. adding low-concentration mother liquor or fresh water to elute sodium chloride in the flotation process so as to improve the grade of potassium chloride; 7. separating the foam obtained by secondary selection by a belt conveyor to obtain crude potassium; 8. washing the crude potassium in a washing tank, wherein the washing liquid adopts low-sodium and low-magnesium mother liquor; 8. separating the washed slurry by a centrifugal machine to obtain potassium chloride; 9. drying the potassium chloride obtained by the separation of the centrifugal machine to obtain a potassium chloride product.
The prior art mainly has the following defects: (1) in the prior art, the low-concentration decomposition liquid is adopted, so that the speed control of the decomposition and crystallization process is not facilitated, the concentration of the decomposition liquid is low, the dissolution and crystallization rate of carnallite and sodium chloride is high, the adhesion, the intergrowth and the like of potassium chloride and sodium chloride crystals are increased, and the grade of potassium chloride is reduced; (2) limited by the volume, residence time and yield of the crystallizer, the prior art can not improve the product quality by improving the concentration of the decomposition liquid, if the concentration of the decomposition liquid is improved, the using amount of the decomposition liquid is increased sharply, the bearing capacity of the crystallizer is exceeded, the reaction residence time is shortened, the yield is reduced, and the production is not facilitated; (3) low-concentration mother liquor or fresh water is required to be added in the processes of rough concentration, primary concentration and secondary concentration to dissolve and elute sodium chloride, and potassium chloride is dissolved in the process, so that the potassium yield is reduced; (4) in the washing process, a large amount of washing liquid is needed to dissolve and elute sodium chloride, and potassium chloride is also dissolved, so that the potassium yield is further reduced.
Disclosure of Invention
The invention aims to provide a method for improving the yield of potassium chloride produced by high-fine-grain high-sodium carnallite ore, aiming at the technical problem of low yield of potassium chloride produced by high-fine-grain high-sodium carnallite ore in the prior art.
The technical scheme adopted for realizing the purpose of the invention is as follows:
a process for increasing the yield of potassium chloride from fine-grained high-sodium carnallite ore includes such steps as respectively adding fine-grained high-sodium carnallite and decomposing liquid to the decomposing region of crystallizer, and adding MgCl in said decomposing liquid 2 The concentration of the high-sodium carnallite and the decomposition liquid is 17-21%, the adding positions of the fine-sodium carnallite and the decomposition liquid are two ends which are farthest away on the same horizontal plane in a decomposition area, the fine-sodium carnallite and the decomposition liquid are respectively added into the decomposition area through a sleeve, the upper end surface of the sleeve is higher than the liquid level in the decomposition area, the lower end surface of the sleeve is positioned below the liquid level in the decomposition area, the fine-sodium carnallite and the decomposition liquid enter the decomposition area after passing through the corresponding sleeve, and MgCl is contained in mixed slurry in the decomposition area 2 The concentration is more than or equal to 24 percent.
In the technical scheme, the sodium chloride in the fine-grain high-sodium carnallite accounts for 10% -35%, and the sodium chloride with the grain diameter of less than 0.25mm accounts for 70% -90% of the total sodium chloride.
In the above technical solution, the ratio of parts by mass of the fine-grained high-sodium carnallite put into the corresponding casing pipe to enter the decomposing field of the crystallizer, parts by volume of the decomposing fluid put into the corresponding casing pipe to enter the decomposing field of the crystallizer, and parts by volume of the underflow discharge amount of the crystallizer is (9.07-14.51): (6.68-23.55): (6.37-10.20), wherein the unit of the mass parts is Kg, and the unit of the volume parts is L.
In the technical scheme, the retention time of the material in the crystallizer is 2.5-4 h.
In the above technical solution, the sleeve is a square, circular or oval tube.
In the technical scheme, the ratio of the length L of the sleeve below the liquid level to the height H of the inner sleeve of the decomposition area in the crystallizer below the liquid level is (0.1-1): 10.
In the technical scheme, the ratio of the diameter or the side length of the sleeve to the diameter of the sleeve in the decomposing area of the crystallizer is (0.5-1.5): 10.
In the technical scheme, the underflow is subjected to flotation, the solid-liquid ratio of slurry is 25% -30% during flotation, then, the potassium chloride subjected to flotation is washed according to the solid-liquid ratio of 35% -50%, the washing time is 10-30min, and the potassium chloride product is prepared by filtering and drying the solid phase.
In another aspect of the present invention, a crystallizer comprises a decomposition region, a crystal growth region and an overflow region in sequence from inside to outside, wherein a stirring mechanism is arranged in the decomposition region, two sleeves are arranged in the decomposition region, the distance between the horizontal planes of the two sleeves is the maximum distance on the horizontal plane in the decomposition region, one sleeve is used for adding fine-grained high-sodium carnallite, and the other sleeve is used for adding decomposition liquid.
In the technical scheme, the ratio of the length L of the sleeve below the liquid level to the height H of the inner sleeve of the decomposition area in the crystallizer below the liquid level is (0.1-1): 10; the ratio of the diameter or the side length of the sleeve to the diameter of the sleeve in the decomposing area of the crystallizer is (0.5-1.5): 10.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, through the arrangement of the sleeve in the crystallizer and the increase of the distance between the feeding position of the decomposition liquid and the feeding position of the high-fine-grain high-sodium carnallite, the local concentration can be improved, the concentration of the decomposition liquid is improved, the local concentration is improved to reduce the dissolving and precipitation amount of sodium chloride, the interaction degree between potassium chloride and sodium chloride crystals is reduced, the sodium chloride carried in potassium chloride crystals is reduced, and the grade of the subsequent potassium chloride flotation product is improved;
2. the invention aims at controlling the decomposition and crystallization process by improving the concentration of the decomposition liquid by taking fine sodium chloride carnallite as a raw material, reducing the precipitation amount of sodium chloride crystals and reducing the adhesion and intergrowth conditions of potassium chloride and sodium chloride crystals, thereby improving the grade of potassium chloride, further reducing the usage amount of washing liquid in the washing process and reducing the dissolution of potassium chloride, and further improving the potassium yield.
3. Fresh water is not introduced in the flotation process, and the concentration of the mother solution is strictly controlled; the solid-liquid ratio is increased and the fresh water consumption is reduced in the washing process to improve the utilization rate of potassium resources.
Drawings
Fig. 1 shows a schematic structural view of the crystallizer of the present invention.
Fig. 2 is a sectional view taken along line a-a in fig. 1.
In the figure: 1-crystallizer, 2-decomposition zone, 3-crystal growth zone, 4-overflow zone, 5-sleeve and 6-inner sleeve.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In the following examples, fine-grained high-sodium carnallite is used as a raw material, the sodium chloride in the fine-grained high-sodium carnallite accounts for 10-35%, and the sodium chloride with the grain size of less than 0.25mm accounts for 70% -90% of the total sodium chloride.
MgCl 2 The saturated concentration of (A) was 25.65%, the saturated concentration of NaCl was 1.49%, and the saturated concentration of KCl was 3.22%.
Example 1
The utility model provides a crystallizer, includes decomposition area 2, crystal growth district 3 and overflow area 4 from inside to outside in proper order, wherein, be equipped with rabbling mechanism in the decomposition area, be equipped with two sleeve pipes 5 in the decomposition area, the interval of two sleeve pipes 5 between the horizontal plane is the biggest interval on the horizontal plane in the decomposition area, and one of them sleeve pipe 5 is used for adding the high sodium carnallite of fine grain, and another sleeve pipe 5 is used for adding the decomposition liquid. The ratio of the length L of the sleeve 5 below the liquid level to the height H of the inner sleeve 6 below the liquid level in the decomposition area in the crystallizer is (0.1-1) to 10; the ratio of the diameter or the side length of the sleeve 5 to the diameter of the inner sleeve 6 in the decomposing area of the crystallizer is (0.5-1.5): 10.
The fine-grained high-sodium carnallite and the decomposition liquid are respectively added through a sleeve 5, the sleeve 5 can effectively prolong the material dispersion time and improve the local concentration, and in the decomposition area 2, under the action of the decomposition liquid with high concentration (17% -21%), NaCl and potassium chloride are firstly dissolved, the NaCl dissolution speed is slow, so that only a small amount of NaCl is dissolved, and then MgCl is added 2 Completely dissolved, MgCl 2 Under the stirring of the stirring mechanism, the materials are lifted in the decomposition zone 2 and enter the crystal growth zone 3, and the materials are stirred in the high-concentration MgCl 2 Under the salting-out action of the solution, potassium chloride is separated out, potassium chloride particles gradually grow larger, in an overflow area 4, mother liquor overflows from the top, large-particle potassium chloride is settled and discharged as underflow, and MgCl is also discharged as underflow 2 The solution, a small amount of NaCl and potassium chloride solution, undissolved NaCl particles and potassium chloride particles separated out later are reduced in adhesion degree, so that subsequent flotation separation is facilitated, NaCl entrainment is avoided, and the potassium chloride grade is improved.
Examples 2-4 below were all conducted in the crystallizer of this example 1.
Example 2
In this example, the composition of the fine-grained high-sodium carnallite was 18.28% KCl, 16.79% NaCl, and MgCl 2 28.12 percent, wherein the ratio of sodium chloride with the particle size of less than 0.25mm to the total sodium chloride is 81.53 percent, MgCl is prepared in advance 2 100L of 17% decomposition liquid.
The method for improving the yield of potassium chloride produced by the fine-grained high-sodium carnallite ore comprises the step of feeding 14.51Kg/h of fine-grained high-sodium carnallite into a decomposition zone 2 of a crystallizer 1, wherein a sleeve 6 in the decomposition zone 2 has the diameter of 14cm and the height of 45 cm. Mixing MgCl 2 The decomposed liquid with the concentration of 17 percent is fed into the decomposition area 2 of the crystallizer 1 according to the volume of 10.69L/h, the decomposed liquid and the fine-grain high-sodium carnallite are respectively added into the decomposition area 2 through a sleeve 5, the sleeve 5 added with the decomposed liquid is arranged at the leftmost end of the decomposition area 2, and a sleeve added with the fine-grain high-sodium carnallite is arrangedThe pipe 5 is arranged at the rightmost end of the decomposition area 2, the sleeve 5 adopted in the embodiment is a plastic circular pipe with the inner diameter of 2cm, the length of the sleeve 5 below the liquid surface is 5cm, the height above the liquid surface is 1.5cm, the retention time of materials in the crystallizer is 2.5h, the underflow discharge amount of the crystallizer is 10.20L/h, the experimental process lasts for 8h, after the completion, potassium chloride is prepared by flotation, the solid-liquid ratio of flotation slurry is 25%, the potassium chloride after flotation is washed for 15min according to the solid-liquid ratio of 40%, the washing liquid is fresh water, the potassium chloride product is prepared by solid phase drying after filtration, and the grade of the prepared potassium chloride is 84.3%.
Example 3
In this example, the composition of the fine-grained high-sodium carnallite was 18.28% KCl, 16.79% NaCl, and MgCl 2 28.12 percent of sodium chloride with the particle size of less than 0.25mm accounting for 81.53 percent of the total sodium chloride, and MgCl is prepared in advance 2 The concentration is 150L of 19% decomposition liquid.
The method for improving the yield of potassium chloride produced by the fine-grained high-sodium carnallite ore comprises the step of feeding 14.51Kg/h of fine-grained high-sodium carnallite into a decomposition zone 2 of a crystallizer 1, wherein a sleeve 6 in the decomposition zone 2 has the diameter of 14cm and the height of 45 cm. Mixing MgCl 2 The decomposition liquid with the concentration of 19 percent is fed into the decomposition area 2 of the crystallizer 1 according to 13.59L/h, the decomposition liquid and the fine-grain high-sodium carnallite are respectively added into the decomposition area 2 through a sleeve 5, the sleeve 5 added with the decomposition liquid is arranged at the leftmost end of the decomposition area 2, the sleeve 5 added with the fine-grain high-sodium carnallite is arranged at the rightmost end of the decomposition area 2, the sleeve 5 adopted in the embodiment is a plastic round pipe, the inner diameter is 2cm, the length of the sleeve 5 under the liquid surface is 5cm, the height above the liquid level is 1.5cm, the retention time of the materials in the crystallizer is 2.5h, the underflow discharge amount of the crystallizer is 10.20L/h, the experimental process lasts for 8h, after the operation is finished, potassium chloride is prepared by flotation, the solid-to-liquid ratio of flotation slurry is 25%, the potassium chloride after flotation is washed for 15min according to the solid-to-liquid ratio of 40%, the washing liquid is fresh water, the potassium chloride product is prepared by filtering and then drying the solid phase, and the grade of the prepared potassium chloride is 87.1%.
Example 4
In this example, the composition of the fine-grained high-sodium carnallite was 18.28% KCl, 16.79% NaCl, and MgCl 2 28.12 percent, wherein the sodium chloride with the grain diameter of less than 0.25mm accounts for the total chlorinationThe sodium ratio was 81.53%, MgCl was prepared in advance 2 200L of 21% decomposition liquid.
The method for improving the yield of potassium chloride produced by the fine-grained high-sodium carnallite ore comprises the step of feeding 14.51Kg/h of fine-grained high-sodium carnallite into a decomposition zone 2 of a crystallizer 1, wherein a sleeve 6 in the decomposition zone 2 has the diameter of 14cm and the height of 45 cm. Mixing MgCl 2 Decomposition liquid with the concentration of 21 percent is fed into a decomposition area 2 of a crystallizer 1 according to the volume of 18.86L/h, the decomposition liquid and fine-grain high-sodium carnallite are respectively added into the decomposition area 2 through a sleeve 5, the sleeve 5 added with the decomposition liquid is arranged at the leftmost end of the decomposition area 2, the sleeve 5 added with the fine-grain high-sodium carnallite is arranged at the rightmost end of the decomposition area 2, the sleeve 5 adopted in the embodiment is a plastic round pipe, the inner diameter is 2cm, the length of the sleeve 5 under the liquid surface is 5cm, the height above the liquid surface is 1.5cm, the retention time of the materials in the crystallizer is 2.5h, the underflow discharge amount of the crystallizer is 8.5L/h, the experimental process lasts for 8h, potassium chloride is prepared by flotation after the completion of the experimental process, the solid-liquid ratio of the flotation slurry is 25%, the potassium chloride after the flotation is washed for 15min according to the solid-liquid ratio of 40%, the washing liquid is fresh water, the potassium chloride product is prepared by drying the solid phase after the filtration, and the grade of the prepared potassium chloride is 92.7%.
Comparative example 1
In this comparative example, the composition of the fine high-sodium carnallite was 18.28% KCl, 16.79% NaCl, and MgCl 2 28.12 percent, wherein the ratio of sodium chloride with the particle size of less than 0.25mm to the total sodium chloride is 81.53 percent, MgCl is prepared in advance 2 100L of 17% decomposition liquid.
A process for producing potassium chloride from fine-grained high sodium carnallite comprising the steps of: charging the fine-grained high-sodium carnallite into a crystallizer decomposition zone of a crystallizer according to 14.51Kg/h, and adding the MgCl 2 Adding 17% decomposition liquid into the crystallizer decomposition area according to 10.69L/h, simultaneously adding the decomposition liquid and the fine-grain high-sodium carnallite into the center position of the crystallizer decomposition area, keeping the material in the crystallizer for 2.5h, keeping the underflow discharge amount of the crystallizer at 10.20L/h, continuing the experimental process for 8h, then preparing potassium chloride by flotation, wherein the solid-liquid ratio of the flotation slurry is 25%, washing the potassium chloride after flotation for 15min according to the solid-liquid ratio of 40%, and the washing liquid is fresh water, filtering and drying the solid phase to prepare the potassium chlorideThe grade of the obtained potassium chloride product is 71.7 percent.
Description of the drawings: in the above embodiment, the concentration of the decomposed solution can be increased continuously, and the grade of potassium chloride can be increased accordingly, but in the actual implementation process, when the concentration of the decomposed solution is increased, the decomposed solution is MgCl 2 The concentration is more than or equal to 22 percent, and the dosage of the decomposition liquid is increased sharply, which is not beneficial to practical implementation.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The method for improving the yield of potassium chloride produced by the fine-grained high-sodium carnallite ore is characterized in that the fine-grained high-sodium carnallite and decomposition liquid are respectively added into a decomposition area of a crystallizer, and MgCl in the decomposition liquid 2 The concentration of the fine-grain high-sodium carnallite and the decomposition liquid is 17-21 percent, the adding positions of the fine-grain high-sodium carnallite and the decomposition liquid are two ends which are farthest away from each other on the same horizontal plane in the decomposition area, the fine-grain high-sodium carnallite and the decomposition liquid are respectively added into the decomposition area through a sleeve, the upper end surface of the sleeve is higher than the liquid level in the decomposition area, the lower end surface of the sleeve is positioned below the liquid level in the decomposition area, the fine-grain high-sodium carnallite and the decomposition liquid enter the lower part of the liquid level in the decomposition area after passing through the corresponding sleeves, and MgCl is contained in the mixed slurry in the decomposition area 2 The concentration is more than or equal to 24 percent.
2. The method for increasing the yield of potassium chloride from fine-grained high-sodium carnallite ores as claimed in claim 1 wherein the fine-grained high-sodium carnallite has a sodium chloride content of 10% to 35% and a sodium chloride particle size of 0.25mm or less of 70% to 90% of the total sodium chloride.
3. The method for increasing the yield of potassium chloride from fine-grained high-sodium carnallite ore according to claim 1, wherein the ratio of parts by mass per hour of the fine-grained high-sodium carnallite put into the corresponding casing to enter the decomposing field of the crystallizer, the parts by volume of the decomposing fluid put into the corresponding casing to enter the decomposing field of the crystallizer, and the underflow discharge amount of the crystallizer is (9.07-14.51): (6.68-23.55): (6.37-10.20), wherein the unit of the mass parts is Kg, and the unit of the volume parts is L.
4. The method for increasing the yield of potassium chloride from fine-grained high-sodium carnallite ore as claimed in claim 1 wherein the residence time of the material in the crystallizer is between 2.5 and 4 hours.
5. The method for increasing the yield of potassium chloride from fine-grained high-sodium carnallite ore of claim 1 wherein the casing is a square, circular or oval shaped tube.
6. The method for improving the yield of potassium chloride from fine-grained high-sodium carnallite ore according to claim 1, wherein the ratio of the length L of the sleeve below the liquid surface to the height H of the inner sleeve of the decomposition zone in the crystallizer below the liquid surface is (0.1-1): 10.
7. The method for improving the yield of potassium chloride from fine-grained high-sodium carnallite ore as claimed in claim 1, wherein the ratio of the diameter or side length of the sleeve to the diameter of the sleeve in the decomposing region of the crystallizer is (0.5-1.5): 10.
8. The method for improving the yield of potassium chloride from fine-grained high-sodium carnallite ore as claimed in claim 1, wherein the underflow is subjected to flotation, the slurry solid-to-liquid ratio during the flotation is 25% -30%, then the potassium chloride after the flotation is washed according to the solid-to-liquid ratio of 35% -50%, the washing time is 10-30min, and the potassium chloride product is prepared by drying the solid phase after the filtration.
9. The crystallizer is characterized by comprising a decomposition area, a crystallization growth area and an overflow area from inside to outside in sequence, wherein a stirring mechanism is arranged in the decomposition area, two sleeves are arranged in the decomposition area, the distance between the two sleeves on the horizontal plane is the maximum distance on the horizontal plane in the decomposition area, one sleeve is used for adding fine-grain high-sodium carnallite, and the other sleeve is used for adding decomposition liquid.
10. The crystallizer of claim 9, wherein the ratio of the length L of the jacket tube below the liquid level to the height H of the jacket tube below the liquid level in the decomposition zone in the crystallizer is (0.1-1): 10; the ratio of the diameter or the side length of the sleeve to the diameter of the sleeve in the decomposing area of the crystallizer is (0.5-1.5): 10.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073030A (en) * | 2013-02-01 | 2013-05-01 | 青海盐湖工业股份有限公司 | Crystallizer for hydrolyzing carnallite |
| CN107803047A (en) * | 2017-12-12 | 2018-03-16 | 天津大学 | A kind of continuous decomposition crystallizer for carnallite thermal decomposition preparing potassium chloride |
| CN109173327A (en) * | 2018-10-11 | 2019-01-11 | 北京恩泽佳立科技有限公司 | It is a kind of for hydrolyzing the crystallizer of carnallite preparing potassium chloride |
| CN113956079A (en) * | 2021-12-09 | 2022-01-21 | 中国科学院青海盐湖研究所 | Method for producing high-grade agricultural potassium chloride from fine-grain high-sodium carnallite |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073030A (en) * | 2013-02-01 | 2013-05-01 | 青海盐湖工业股份有限公司 | Crystallizer for hydrolyzing carnallite |
| CN107803047A (en) * | 2017-12-12 | 2018-03-16 | 天津大学 | A kind of continuous decomposition crystallizer for carnallite thermal decomposition preparing potassium chloride |
| CN109173327A (en) * | 2018-10-11 | 2019-01-11 | 北京恩泽佳立科技有限公司 | It is a kind of for hydrolyzing the crystallizer of carnallite preparing potassium chloride |
| CN113956079A (en) * | 2021-12-09 | 2022-01-21 | 中国科学院青海盐湖研究所 | Method for producing high-grade agricultural potassium chloride from fine-grain high-sodium carnallite |
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