CN115215355B - Method for reducing fine sodium chloride in potassium chloride product and application thereof - Google Patents
Method for reducing fine sodium chloride in potassium chloride product and application thereof Download PDFInfo
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- CN115215355B CN115215355B CN202211002417.2A CN202211002417A CN115215355B CN 115215355 B CN115215355 B CN 115215355B CN 202211002417 A CN202211002417 A CN 202211002417A CN 115215355 B CN115215355 B CN 115215355B
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 134
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 80
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 37
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 37
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 37
- 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 94
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000243 solution Substances 0.000 claims abstract description 51
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 42
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 37
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 27
- 239000012452 mother liquor Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000010413 mother solution Substances 0.000 claims abstract description 7
- 238000007865 diluting Methods 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 235000002639 sodium chloride Nutrition 0.000 claims description 65
- 238000003756 stirring Methods 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 14
- 230000035484 reaction time Effects 0.000 claims description 10
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 8
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 8
- 229910001414 potassium ion Inorganic materials 0.000 claims description 8
- 229910001415 sodium ion Inorganic materials 0.000 claims description 8
- 238000011282 treatment Methods 0.000 claims description 6
- 239000012066 reaction slurry Substances 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 15
- 239000011591 potassium Substances 0.000 abstract description 15
- 229910052700 potassium Inorganic materials 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 239000003337 fertilizer Substances 0.000 description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 229940072033 potash Drugs 0.000 description 9
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 9
- 235000015320 potassium carbonate Nutrition 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 239000007790 solid phase Substances 0.000 description 7
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 6
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005188 flotation Methods 0.000 description 4
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 4
- 239000010442 halite Substances 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 230000003068 static effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 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 description 1
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000674 effect on sodium Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 210000004243 sweat Anatomy 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
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for reducing fine sodium chloride in a potassium chloride product and application thereof. The method comprises the following steps: (1) Hydrolyzing carnallite ore to obtain saturated mother liquor with three-phase balance of potassium chloride, sodium chloride and carnallite; (2) Mixing and diluting the saturated mother solution with water to obtain a decomposition solution; wherein the content of magnesium chloride in the decomposition solution is 0.25-2.42mol/kgH 2 O; (3) And adding carnallite ore into the decomposition solution in batches for reaction, and separating to obtain a potassium chloride product with low content of fine sodium chloride. The invention improves the potassium yield by reducing the content of fine sodium chloride in the production process; meanwhile, the method provided by the invention has the characteristics of simplicity and easiness in operation, compact flow, low water consumption and easiness in realization of large-scale production.
Description
Technical Field
The invention belongs to the technical field of salt lakes, and particularly relates to a method for reducing fine sodium chloride in a potassium chloride product and application thereof.
Background
Potassium salt is an important strategic mineral resource for guaranteeing national grain safety, and potash fertilizer is one of three basic fertilizers (nitrogen, phosphorus and potassium) for agriculture. By 2023, the global potash fertilizer demand is expected to increase to 7300 ten thousand tons, and the national demand will reach about 1700 ten thousand tons. The inlet amount of potash fertilizer in China is about 50% in recent years, and the supply pressure of the domestic potash fertilizer is increased year by year. At present, the potash fertilizer produced by taking salt lake brine as a raw material in China accounts for more than 90 percent, and the potash fertilizer has important significance for national production and plays a supporting role for guaranteeing national grain safety.
Carnallite ore is the most common production raw material for potash fertilizer production, and is solid carnallite ore obtained from salt field evaporation or sedimentary stratum, and the main mineral components of the carnallite ore are carnallite and halite, namely sodium chloride (NaCl), which have influence on the decomposition of the carnallite ore and the subsequent flotation of potassium chloride (KCl), and are mainly expressed in the following steps: (1) Sodium chloride (NaCl) affects the potassium yield of carnallite ore decomposition; (2) The recrystallization process of sodium chloride (NaCl) exists in the carnallite ore decomposition process, which is easy to cause crystallization precipitation of fine sodium chloride (NaCl); (3) Fine particulate sodium chloride (NaCl) has an effect on the potash fertilizer flotation process.
The potassium fertilizer prepared from carnallite ore generally utilizes K + 、Na + 、Mg 2+ //Cl - -H 2 O quaternary water salt system phase diagram, through technological calculation, proper water adding amount is determined to make magnesium chloride (MgCl) 2 ) All dissolved into liquid phase, potassium chloride (KCl) crystallized. The carnallite ore comprises sodium chloride (NaCl), potassium chloride (KCl) and magnesium chloride (MgCl) 2 ) Wherein potassium chloride (KCl) and magnesium chloride (MgCl) 2 ) Constituting carnallite (KCl. MgCl) 2 ·6H 2 O), after addition of water, the following reaction takes place:
in the above process, potassium chloride (KCl) in carnallite is crystallized out and exists in the system as a solid phase, and sodium chloride (NaCl) is added in the initial magnesium chloride (MgCl) 2 ) The dissolution in solution is rapid, but as the decomposition proceeds, the magnesium chloride (MgCl) 2 ) The dissolution rate of sodium chloride (NaCl) is high, so that the saturation degree of sodium chloride (NaCl) is increased, the supersaturation phenomenon appears, the sodium chloride (NaCl) dissolved previously is recrystallized again and separated out, and the sodium chloride (NaCl) exists in the system in the form of fine fraction, and the newly formed sodium chlorideThe method has influence on the yield of decomposed potassium and the subsequent potassium salt flotation, and is a key for restricting the preparation of potash fertilizer by using carnallite ore.
Disclosure of Invention
The main purpose of the invention is to provide a method for reducing fine sodium chloride in potassium chloride products and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a method for reducing fine sodium chloride in a potassium chloride product, which comprises the following steps:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with three-phase balance of potassium chloride, sodium chloride and carnallite;
(2) Mixing and diluting the saturated mother solution with water to obtain a decomposition solution; wherein the content of magnesium chloride in the decomposition solution is 0.25-2.42mol/kgH 2 O；
(3) And adding carnallite ore into the decomposition solution in batches for reaction, and separating to obtain a potassium chloride product with low content of fine sodium chloride.
The embodiment of the invention also provides the application of the method in the preparation of potassium chloride by decomposing carnallite ore.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a method for decomposing carnallite ore containing sodium chloride by using a solution containing magnesium chloride as a decomposition solution, which reduces the content of fine sodium chloride in a decomposed product, improves the yield of decomposed potassium, reduces the adsorption effect of octadecylamine flotation agent on sodium chloride in a potassium salt flotation process, improves the yield of potassium, and ensures that the solution containing magnesium chloride is from saturated mother liquor balanced after the carnallite ore is decomposed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a process flow diagram of a method for reducing fine particulate sodium chloride in a potassium chloride product in an exemplary embodiment of the invention.
Detailed Description
In view of the drawbacks of the prior art, the inventors of the present invention have long studied and have made extensive efforts to propose a technical solution of the present invention, which is mainly a solution using a magnesium chloride (MgCl) 2 ) The solution of the components is a decomposition solution, which decomposes carnallite ore containing sodium chloride (NaCl), reduces the content of fine sodium chloride (NaCl) in the decomposed product, improves the yield of decomposed potassium, reduces the adsorption effect on sodium chloride (NaCl) in the potassium salt floatation process, improves the yield of potassium, and contains magnesium chloride (MgCl) 2 ) The solution of the components comes from the balanced saturated mother liquor after decomposing carnallite ore, and the method has the advantages of simplicity and easiness in operation, compact flow, low water consumption and easiness in realization of large-scale production.
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Specifically, as one aspect of the technical scheme of the invention, the method for reducing the fine sodium chloride in the potassium chloride product comprises the following steps:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with three-phase balance of potassium chloride, sodium chloride and carnallite;
(2) Mixing and diluting the saturated mother solution with water to obtain a decomposition solution; wherein the content of magnesium chloride in the decomposition solution is 0.25-2.42mol/kgH 2 O；
(3) And adding carnallite ore into the decomposition solution in batches for reaction, and separating to obtain a potassium chloride product with low content of fine sodium chloride.
In some preferred embodiments, a process flow diagram of the method of the present invention for reducing fine particulate sodium chloride in a potassium chloride product is shown in FIG. 1.
In some preferred embodiments, the carnallite ore is dry-mined salt pan carnallite ore obtained by evaporation of a karl sweat salt pan.
Further, 80wt% of the carnallite ore has a particle size of greater than 0.125mm.
Further, the carnallite ore comprises sodium chloride, wherein 83wt% of the sodium chloride has a particle size of less than 0.85mm.
In some preferred embodiments, the carnallite ore has a potassium ion content of 4.6 to 5.8wt%, a magnesium ion content of 4.3 to 5.5wt%, and a sodium ion content of 15.2 to 19.3wt%.
In some preferred embodiments, the saturated mother liquor has a magnesium chloride content of 3.64 to 4.22mol/kgH 2 O, potassium chloride content of 0.28-0.88mol/kgH 2 O, sodium chloride content of 0.44-0.46mol/kgH 2 O。
In some preferred embodiments, the magnesium chloride content of the decomposition solution is in the range of 0.20 to 2.02mol/kgH 2 O。
In some preferred embodiments, the decomposition solution is an equilibrium solution after dilution of the saturated mother liquor with water.
In some preferred embodiments, the amount of water used in step (2) is 50 to 80wt% of the decomposition solution.
In some preferred embodiments, step (3) comprises: placing the decomposition solution in a paddle stirring device, adding carnallite ore into the decomposition solution in batches for reaction, and adding water to obtain reaction slurry.
Further, the stirring speed of the paddle stirring device is 150-350rpm.
Further, the water is added in an amount of 20 to 50wt% of the reaction slurry.
Further, the mass ratio of the water added in the step (2) to the water added in the step (3) is 4-1:1-2.
In some preferred embodiments, the temperature of the reaction in step (3) is 20 to 30 ℃ for a period of 30 to 65 minutes.
In some preferred embodiments, the carnallite ore is added to the decomposition solution in step (3) three times.
Further, the mass ratio of the carnallite ore added for three times is 1.5-2: 1.3 to 2:2.2 to 4.
In some preferred embodiments, the rate of addition of the carnallite ore to the decomposition solution in step (3) is from 2 to 25g/min.
In some preferred embodiments, the separation treatment comprises a sieving treatment.
Further, the screening size used in the screening treatment is 100-140 meshes, preferably 100 meshes.
In some more specific embodiments, the method of reducing fine particulate sodium chloride in a potassium chloride product comprises:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with three-phase balance of potassium chloride, sodium chloride and carnallite;
(2) Diluting the saturated mother liquor with water to obtain a solution containing magnesium chloride (MgCl) 2 ) Solutions of the components, referred to as decomposition solutions;
(3) Placing the decomposition solution in a stirrer, slowly adding carnallite in batches, reacting for a period of time, and adding the water required by the residual system;
(4) The reaction slurry is separated by sieving, and the separated solid phase is potassium chloride (KCl) with low fine-particle sodium chloride (NaCl) content.
Further, in the step (1), the carnallite ore is dry-picked salt pan carnallite ore obtained by evaporation of a Conerspirants salt pan, wherein 80% of the carnallite ore has a grain size of more than 0.125mm, and 83% of sodium chloride has a grain size of less than 0.85mm; the content of potassium ions in the carnallite ore is 4.6-5.8%, the content of magnesium ions is 4.3-5.5%, and the content of sodium ions is 15.2-19.3%.
Further, in the step (1), the saturated mother liquor magnesium chloride (MgCl) 2 ) The component content is 3.64-4.22mol/kgH 2 O。
Further, in the step (2), the decomposition solution is an equilibrium solution after the saturated mother solution is diluted with water.
Further, in the step (2), the water adding amount is 50-80% of the total system water required amount.
Further, in the step (2), magnesium chloride (MgCl) is decomposed 2 ) The concentration is 0.25-2.42mol/kgH 2 O。
Further, in the step (3), the stirrer is a paddle stirrer.
Further, in the step (3), the batch times are three times, and the weight ratio of the carnallite ore in the three batches is 1.5-2:1.3-2:2.2-4.
Further, in the step (3), the carnallite ore is added at a rate of 2-25g/min.
Further, in the step (3), the water required for adding the rest system is 20-50% of the total system water required.
Further, in the step (3), the stirring speed of the stirrer is 150-350rpm.
Further, in the step (3), the reaction time is 30-65min.
Further, in the step (4), the sieving size is 100 mesh, namely 0.15mm.
The invention improves the potassium yield by reducing the content of fine sodium chloride in the production process; meanwhile, the method provided by the invention has the characteristics of simplicity and easiness in operation, compact flow, low water consumption and easiness in realization of large-scale production.
Another aspect of an embodiment of the invention also provides the use of the foregoing method for the preparation of potassium chloride by carnallite ore decomposition. The technical scheme of the present invention is further described in detail below with reference to several preferred embodiments and the accompanying drawings, and the embodiments are implemented on the premise of the technical scheme of the present invention, and detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples described below, unless otherwise specified, were all commercially available from conventional biochemicals.
Example 1
(1) Raw ore carnallite is carnallite of dry-mining salt fieldThe average grain size is 0.20mm, the maximum grain size is 2.50mm, the potassium ion content is 9.05 percent, the magnesium ion content is 5.35 percent, the sodium ion content is 15.02 percent in raw ore carnallite, 500g of raw ore carnallite is taken, 164.21g of water is weighed, the raw ore carnallite is transferred into a 1000ml beaker according to the proportion to react, the stirring speed is 500rpm, the reaction time is 40-60min, the static balance is 12-24h, the solid-liquid separation is carried out, and saturated mother liquor is obtained, wherein the magnesium chloride content is 3.78mol/kgH 2 O；
(2) Saturated mother liquor is prepared according to water: the saturated mother liquor was mixed at a weight ratio of 2.18:1 to give a decomposition solution having a magnesium chloride content of 0.92mol/kg H 2 O, wherein the water amount is 52% of the total water amount of the system;
(3) Placing the decomposition solution in a 500ml beaker, wherein the stirrer is a paddle stirrer, raw ore carnallite is added in three batches, and the weight ratio of the three batches of carnallite is 1.6:1.5:2.3;
(4) The raw ore carnallite ore is fed at a speed of 15g/min, the stirring paddle is at a speed of 200rpm, and the reaction time is 5-20min;
(5) Adding the water required by the residual system into the reactor by a peristaltic pump, wherein the water is 48% of the total water of the system, and the water adding speed is 2.5g/min;
(6) After the water addition is completed, continuing to react for 5-20min, stirring at 150rpm and reacting at 22 ℃;
(7) After the reaction is completed, separating solid from liquid, wherein the mass of the solid-phase decomposed ore potassium chloride is 72.13g, the yield of the decomposed potassium is 84.01%, and the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of the fine-particle sodium chloride less than or equal to 100 meshes is 4.21%.
Example 2
(1) The raw ore carnallite is dry-picked salt field carnallite, the average grain size is 0.20mm, the maximum grain size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05%, the magnesium ion content is 5.35%, the sodium ion content is 15.02%, 500g of raw ore carnallite is taken, 164.21g of water is weighed according to the proportion and transferred into a 1000ml beaker for reaction, the stirring speed is 500rpm, the reaction time is 40-60min, the static balance is 12-24h, the solid-liquid separation is carried out, and saturated mother liquor is obtained, wherein the magnesium chloride content is 3.78mol/kgH 2 O；
(2) Saturated mother liquor is prepared according to water: the saturated mother liquor is 1: a weight mix of 1.69 a and,as the decomposition solution, the magnesium chloride content of the decomposition solution was 2.01mol/kgH 2 O, wherein the water quantity is 65% of the total water quantity of the system;
(3) Placing the decomposition solution in a 500ml beaker, wherein the stirrer is a paddle stirrer, raw ore carnallite is added in three batches, and the weight ratio of the three batches of carnallite is 1.5:2:3;
(4) The raw ore carnallite ore is fed at a speed of 15g/min, the stirring paddle is at a speed of 200rpm, and the reaction time is 5-20min;
(5) Adding water required by the residual system into the reactor by a peristaltic pump, wherein the water is 35% of the total water of the system, and the water adding speed is 2.5g/min;
(6) After the water addition is completed, continuing to react for 5-20min, stirring at a rotation speed of 150rpm and a reaction temperature of 23 ℃;
(7) After the reaction is completed, separating solid from liquid, wherein the mass of the solid-phase decomposed ore potassium chloride is 71.81g, the yield of the decomposed potassium is 84.26%, and the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of the fine-particle sodium chloride less than or equal to 100 meshes is 3.01%.
Example 3
(1) The raw ore carnallite is dry-picked salt field carnallite, the average grain size is 0.20mm, the maximum grain size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05%, the magnesium ion content is 5.35%, the sodium ion content is 15.02%, 500g of raw ore carnallite is taken, 164.21g of water is weighed according to the proportion and transferred into a 1000ml beaker for reaction, the stirring speed is 500rpm, the reaction time is 40-60min, the static balance is 12-24h, the solid-liquid separation is carried out, and saturated mother liquor is obtained, wherein the magnesium chloride content is 3.78mol/kgH 2 O；
(2) Saturated mother liquor is prepared according to water: the saturated mother liquor was mixed at a weight ratio of 1:0.89 as a decomposition solution having a magnesium chloride content of 1.45mol/kg H 2 O, wherein the water amount is 75% of the total water amount of the system;
(3) Placing the decomposition solution in a 500ml beaker, wherein the stirrer is a paddle stirrer, raw ore carnallite is added in three batches, and the weight ratio of the three batches of carnallite is 1.8:1.8:1.9;
(4) The raw ore carnallite ore is fed at a speed of 15g/min, the stirring paddle is at a speed of 200rpm, and the reaction time is 5-20min;
(5) Adding the water required by the residual system into the reactor by a peristaltic pump, wherein the water is 25% of the total water of the system, and the water adding speed is 2.5g/min;
(6) After the water addition is completed, continuing to react for 5-20min, stirring at a rotation speed of 150rpm and a reaction temperature of 23 ℃;
(7) After the reaction is completed, solid-liquid phase separation is carried out, the mass of the solid-phase decomposed ore potassium chloride is 72.82g, the yield of the decomposed potassium is 84.31%, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of the fine-particle sodium chloride less than or equal to 100 meshes is 3.82%.
Comparative example 1
The process is the same as in example 1, except that the magnesium chloride content in the decomposition solution in this comparative example is not within the scope of the claims of the present application; and provides corresponding result data.
(1) The raw ore carnallite is dry-picked salt field carnallite, the average grain size is 0.20mm, the maximum grain size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05%, the magnesium ion content is 5.35%, and the sodium ion content is 15.02%.
(2) 164.21g of water is weighed and placed in a 1000ml beaker, and the stirrer is a paddle stirrer;
(3) 500g of carnallite raw ore is weighed, the raw ore carnallite is added in three batches, and the weight ratio of the three batches of carnallite ore is 1.7:2:2.5;
(4) The raw ore carnallite ore feeding speed is 25g/min, and the stirring paddle speed is 300rpm
(5) After carnallite and halite are added, the reaction time is continued for 30-45min, the stirring speed is 200rpm, and the reaction temperature is 25 ℃;
(6) After the reaction is completed, separating solid from liquid, wherein the mass of the solid-phase decomposed ore potassium chloride is 71.81g, the yield of the decomposed potassium is 83.36%, and the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of the fine-particle sodium chloride less than or equal to 100 meshes is 5.38%.
Comparative example 2
The method was the same as in example 1, except that the carnallite ore was added 1 or more times in this comparative example,
(1) The raw ore carnallite is dry-picked salt field carnallite, the average grain size is 0.20mm, the maximum grain size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05%, the magnesium ion content is 5.35%, and the sodium ion content is 15.02%.
(2) 164.21g of water is weighed and placed in a 1000ml beaker, and the stirrer is a paddle stirrer;
(3) Weighing 500g of carnallite raw ore, and adding the raw ore carnallite into the raw ore at one time;
(4) The raw ore carnallite ore has a charging speed of 20g/min and a stirring paddle speed of 300rpm
(5) After carnallite and halite are added, the reaction time is continued for 30-45min, the stirring speed is 150rpm, and the reaction temperature is 25 ℃;
(6) After the reaction is completed, separating solid from liquid, wherein the mass of the solid-phase decomposed ore potassium chloride is 70.29g, the yield of the decomposed potassium is 82.07%, and the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of the fine-particle sodium chloride less than or equal to 100 meshes is 6.33%.
In addition, the inventors have conducted experiments with other materials, process operations, and process conditions as described in this specification with reference to the foregoing examples, and have all obtained desirable results.
It should be understood that the technical solution of the present invention is not limited to the above specific embodiments, and all technical modifications made according to the technical solution of the present invention without departing from the spirit of the present invention and the scope of the claims are within the scope of the present invention.
Claims (7)
1. A method for reducing fine particulate sodium chloride in a potassium chloride product comprising:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with three-phase balance of potassium chloride, sodium chloride and carnallite; the content of magnesium chloride in the saturated mother solution is 3.64-4.22mol/kgH 2 O, potassium chloride content of 0.28-0.88mol/kgH 2 O, sodium chloride content of 0.44-0.46mol/kgH 2 O；
(2) Mixing and diluting the saturated mother solution with water to obtain a decomposition solution; wherein the content of magnesium chloride in the decomposition solution is 0.25-2.42mol/kgH 2 O；
(3) Placing the decomposition solution in a paddle stirring device, adding carnallite ore into the decomposition solution for three times to react, adding water to obtain reaction slurry, and separating to obtain a potassium chloride product with low fine sodium chloride content; the stirring speed of the paddle stirring device is 150-350 rpm; the addition amount of the water is 20-50wt% of the reaction slurry; the mass ratio of the carnallite ore added for three times is 1.5-2:1.3-2:2.2-4; the rate of adding the carnallite into the decomposition solution is 2-25 g/min;
wherein the carnallite ore is dry-picked salt pan carnallite ore obtained by evaporation of a Nalge salt pan; 80wt% of the carnallite ore has a particle size greater than 0.125mm; the carnallite ore comprises sodium chloride, wherein 83wt% of the sodium chloride has a particle size of less than 0.85mm; the content of potassium ions in the carnallite ore is 4.6-5.8wt%, the content of magnesium ions is 4.3-5.5wt%, and the content of sodium ions is 15.2-19.3wt%.
2. The method according to claim 1, characterized in that: the decomposition solution is an equilibrium solution obtained by diluting saturated mother solution with water.
3. The method according to claim 1, characterized in that: the water in the step (2) accounts for 50-80 wt% of the decomposition solution.
4. The method according to claim 1, characterized in that: the mass ratio of water added in the step (2) to the step (3) is 4-1:1-2.
5. The method according to claim 1, characterized in that: the reaction temperature in the step (3) is 20-30 ℃ and the reaction time is 30-65min.
6. The method according to claim 1, characterized in that: the separation treatment is selected from screening treatments; the screening size adopted in the screening treatment is 100-140 meshes.
7. Use of the method of any one of claims 1-6 for the preparation of potassium chloride by carnallite ore decomposition.
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