CN115215355A - 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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- CN115215355A CN115215355A CN202211002417.2A CN202211002417A CN115215355A CN 115215355 A CN115215355 A CN 115215355A CN 202211002417 A CN202211002417 A CN 202211002417A CN 115215355 A CN115215355 A CN 115215355A
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- carnallite
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 title claims abstract description 132
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 title claims abstract description 85
- 239000011780 sodium chloride Substances 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000001103 potassium chloride Substances 0.000 title claims abstract description 40
- 235000011164 potassium chloride Nutrition 0.000 title claims abstract description 40
- 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 97
- 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 59
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 37
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 35
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 26
- 239000012452 mother liquor Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000007865 diluting Methods 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 11
- 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
- 238000005065 mining Methods 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
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000012216 screening Methods 0.000 claims description 6
- 239000012066 reaction slurry Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 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
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 235000002639 sodium chloride Nutrition 0.000 description 51
- 239000000243 solution Substances 0.000 description 41
- 239000003337 fertilizer Substances 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 229940072033 potash Drugs 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- 235000015320 potassium carbonate Nutrition 0.000 description 6
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 5
- 238000005188 flotation Methods 0.000 description 5
- 238000005191 phase separation Methods 0.000 description 5
- 239000007790 solid phase Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 230000002572 peristaltic effect Effects 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 carnallite halide Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 239000010442 halite Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000674 effect on sodium Effects 0.000 description 1
- 230000000694 effects 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
- 239000000463 material Substances 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
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 230000003068 static effect Effects 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
-
- 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
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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)
- 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 balanced three phases of potassium chloride, sodium chloride and carnallite; (2) Mixing and diluting the saturated mother liquor 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) Adding carnallite ore into the decomposition solution in batches for reaction, and then separating to obtain a potassium chloride product with low fine sodium chloride content. The invention improves the yield of potassium 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 a potassium fertilizer is one of three basic fertilizers (nitrogen, phosphorus and potassium) in agriculture. By 2023, the global potassium fertilizer demand is expected to increase to 7300 ten thousand tons, and the national demand reaches about 1700 ten thousand tons. The inlet amount of the potash fertilizer in China is about 50% in the past in recent years, and the supply pressure of the potash fertilizer in China is increased year by year. At present, the potash fertilizer produced by taking salt lake brine as a raw material in China accounts for over 90 percent, has important significance for national production, and plays a supporting role in guaranteeing national food safety.
Carnallite is the most common raw material for producing potash fertilizer, whether solid carnallite obtained by evaporation of salt pan or deposition stratum, and the main mineral components of the carnallite are carnallite and halite, wherein halite, namely sodium chloride (NaCl), has influence on the decomposition of the carnallite and the flotation of subsequent potassium chloride (KCl) and is mainly reflected in that: (1) Sodium chloride (NaCl) affects the potassium yield of carnallite decomposition; (2) Sodium chloride (NaCl) has a recrystallization process in the decomposition process of carnallite, which is easy to cause crystallization separation of fine sodium chloride (NaCl); (3) Fine sodium chloride (NaCl) particles have an influence on the potash fertilizer flotation process.
Preparation of potash fertilizer from carnallite ore generally utilizes K + 、Na + 、Mg 2+ //Cl - -H 2 Determining appropriate water addition amount by process calculation to obtain magnesium chloride (MgCl) 2 ) All dissolved in liquid phase, potassium chloride (KCl) crystallized. The main components of carnallite are sodium chloride (NaCl), potassium chloride (KCl) and magnesium chloride (MgCl) 2 ) Wherein potassium chloride (KCl) and magnesium chloride (MgCl) 2 ) Form carnallite (KCl MgCl) 2 ·6H 2 O), the following reaction takes place after the addition of water:
in this process, potassium chloride (KCl) in the carnallite is crystallized and exists in a solid phase in the system, and sodium chloride (NaCl) is initially low in magnesium chloride (MgCl) 2 ) Dissolve rapidly in solution, but with decompositionThe process proceeds due to magnesium chloride (MgCl) 2 ) The dissolution speed is fast, so that the saturation degree of sodium chloride (NaCl) is increased, the supersaturation phenomenon is generated, the previously dissolved sodium chloride (NaCl) is crystallized and separated again, the sodium chloride (NaCl) exists in a system in a fine-grained form, and the newly generated sodium chloride influences the yield of decomposed potassium and the subsequent potassium salt flotation, so that the method is a key for restricting the preparation of the potassium fertilizer by utilizing the carnallite.
Disclosure of Invention
The invention mainly aims to provide a method for reducing fine sodium chloride in a potassium chloride product and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, 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 balanced three phases of potassium chloride, sodium chloride and carnallite;
(2) Mixing and diluting the saturated mother liquor 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) Adding carnallite ore into the decomposition solution in batches for reaction, and then separating to obtain a potassium chloride product with low fine sodium chloride content.
The embodiment of the invention also provides application of the method in preparation of potassium chloride by decomposing carnallite.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a process flow which uses a solution containing a magnesium chloride component as a decomposition solution to decompose carnallite containing sodium chloride, reduces the content of fine sodium chloride in a decomposition product, improves the yield of decomposed potassium, reduces the adsorption effect of an octadecylamine flotation agent on sodium chloride in the potassium salt flotation process, and improves the yield of potassium.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the description of the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and it is also possible for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is a process flow diagram of a process for reducing fine sodium chloride in a potassium chloride product in accordance with an exemplary embodiment of the present invention.
Detailed Description
In view of the defects of the prior art, the inventors of the present invention have long studied and practiced in great numbers to provide a solution of the present invention, which mainly uses magnesium chloride (MgCl) 2 ) The solution of the components is a decomposition solution for decomposing carnallite ore containing sodium chloride (NaCl), reducing the content of fine sodium chloride (NaCl) in the decomposition product, improving the yield of decomposed potassium, reducing the adsorption effect on sodium chloride (NaCl) in the flotation process of sylvite, improving the yield of potassium, and containing magnesium chloride (MgCl) 2 ) The solution of the components comes from the balanced saturated mother liquor after decomposing the carnallite, and the method has the advantages of simple and easy operation, compact flow, low water consumption and easy realization of the process flow of large-scale production.
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Specifically, as one aspect of the technical scheme of the invention, the method for reducing fine sodium chloride in the potassium chloride product comprises the following steps:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with balanced three phases of potassium chloride, sodium chloride and carnallite;
(2) Mixing the saturated mother liquorMixing with water for dilution to obtain a decomposition solution; wherein the content of magnesium chloride in the decomposition solution is 0.25-2.42mol/kgH 2 O；
(3) Adding carnallite ore into the decomposition solution in batches for reaction, and separating to obtain a potassium chloride product with low fine sodium chloride content.
In some preferred embodiments, a process flow diagram of the process of the present invention for reducing fine sodium chloride in a potassium chloride product is shown in fig. 1.
In some preferred embodiments, the carnallite is dry-land carnallite evaporated from a sweat-salt pan of Carlo.
Further, 80wt% of the carnallite in the carnallite has a particle size of more than 0.125mm.
Further, the carnallite comprises sodium chloride, wherein 83wt% of the sodium chloride has a particle size of less than 0.85mm.
In some preferred embodiments, the carnallite 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 The content of O and potassium chloride is 0.28-0.88mol/kgH 2 The content of O and sodium chloride is 0.44-0.46mol/kgH 2 O。
In some preferred embodiments, the amount of magnesium chloride in the decomposition solution is from 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: and putting the decomposed solution into a paddle type stirring device, adding carnallite ore into the decomposed solution in batches for reaction, and then adding water to obtain reaction slurry.
Further, the stirring speed of the paddle type stirring device is 150-350rpm.
Further, the adding amount of the water is 20-50 wt% 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 ℃ and the time is 30 to 65min.
In some preferred embodiments, the number of batches of the carnallite ore added to the decomposing solution in step (3) is three.
Further, the weight ratio of the carnallite added for three times is 1.5-2: 1.3-2: 2.2 to 4.
In some preferred embodiments, the rate of addition of the carnallite ore to the decomposing solution in step (3) is 2 to 25g/min.
In some preferred embodiments, the separation treatment comprises a sieving treatment.
Further, the screening size selected in the screening treatment is 100-140 meshes, and preferably 100 meshes.
In some more specific embodiments, the method of reducing fine particulate sodium chloride in a potassium chloride product comprises:
(1) Adding water into carnallite ore to decompose to obtain saturated mother liquor with balanced three phases of potassium chloride, sodium chloride and carnallite;
(2) Diluting the saturated mother liquor with water to obtain a magnesium chloride (MgCl) 2 ) Solutions of the components, referred to as decomposition solutions;
(3) Placing the decomposition solution in a stirrer, slowly adding carnallite into the stirrer in batches, and adding water required by the residual system after reacting for a period of time;
(4) And (3) screening and separating the reaction slurry, wherein the solid phase after separation is potassium chloride (KCl) with low fine-grain sodium chloride (NaCl) content.
Further, in the step (1), the carnallite is carnallite in a dry-mining salt field obtained by evaporation in a Carlo salt field, the grain size of 80% of the carnallite is larger than 0.125mm, and the grain size of 83% of sodium chloride is smaller 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), 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 obtained by diluting the saturated mother liquor with water.
Further, in the step (2), the water adding amount is 50-80% of the water amount required by the total system.
Further, in the step (2), the solution of 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.
Furthermore, 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 adding speed of the carnallite ore is 2-25g/min.
Further, in the step (3), the amount of water required by adding the residual system is 20-50% of the amount of water required by the total system.
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 sieve size is 100 meshes, namely 0.15mm.
The invention improves the yield of potassium 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.
In another aspect of an embodiment of the present invention there is also provided the use of the aforementioned process for the decomposition of carnallite ore to produce potassium chloride. The technical solutions of the present invention are further described in detail below with reference to several preferred embodiments and the accompanying drawings, which are implemented on the premise of the technical solutions of the present invention, and a detailed implementation manner and a specific operation process are provided, but the scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples used below were all available from conventional biochemical reagents companies, unless otherwise specified.
Example 1
(1) The raw ore carnallite is carnallite in dry-mining salt field, the average size fraction is 0.20mm, the maximum particle 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%, 500g of raw ore carnallite is taken, 164.21g of water is weighed again, the raw ore carnallite is transferred into a 1000ml beaker according to the proportion for reaction, the stirring rotation speed is 500rpm, the reaction time is 40-60min, the static balance is 12-24h, solid-liquid separation is carried out, saturated mother liquor is obtained, wherein the magnesium chloride content is 3.78mol/kgH 2 O；
(2) The saturated mother liquor is mixed according to the following ratio of 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/kgH 2 O, wherein the water amount is 52 percent of the total water amount of the system;
(3) Placing the decomposed solution into a 500ml beaker, wherein a paddle stirrer is used as the stirrer, and adding the raw ore carnallite into the beaker in three batches, wherein the weight ratio of the carnallite in the three batches is 1.6:1.5:2.3;
(4) The raw ore carnallite ore feeding speed is 15g/min, the stirring paddle speed is 200rpm, and the reaction time is 5-20min;
(5) Adding water required by the residual system into the reactor by using a peristaltic pump, wherein the water amount is 48% of the total water amount of the system, and the water adding speed is 2.5g/min;
(6) After the water is added, continuously reacting for 5-20min at the stirring speed of 150rpm and the reaction temperature of 22 ℃;
(7) After the reaction is finished, solid-liquid phase separation is carried out, the mass of potassium chloride of solid-phase decomposed ore is 72.13g, the yield of the potassium chloride is 84.01%, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of fine sodium chloride with the grain size of less than or equal to 100 meshes is 4.21%.
Example 2
(1) The raw ore carnallite is carnallite in dry-land salt-mining fields, the average size fraction is 0.20mm, the maximum particle size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05 percent, the magnesium ion content is 5.35 percent, the sodium ion content is 15.02 percent, 500g of the raw ore carnallite is taken, 164.21g of water is further weighed, and the weight percentage is calculated according to the weightTransferring the mixture into a 1000ml beaker for reaction, stirring at the rotating speed of 500rpm for 40-60min, standing for balancing for 12-24h, and carrying out solid-liquid separation to obtain saturated mother liquor, wherein the content of magnesium chloride is 3.78mol/kgH 2 O；
(2) The saturated mother liquor is treated according to the following steps of: the saturated mother liquor is 1:1.69 as a decomposing solution, the decomposing solution had a magnesium chloride content of 2.01mol/kgH 2 O, wherein the water amount is 65 percent of the total water amount of the system;
(3) Placing the decomposed solution into a 500ml beaker, wherein a paddle stirrer is used, and adding the raw ore carnallite into the beaker in three batches, wherein the weight ratio of the carnallite in the three batches is 1.5: 2: 3;
(4) The raw ore carnallite ore feeding speed is 15g/min, the stirring paddle speed is 200rpm, and the reaction time is 5-20min;
(5) Adding water required by the residual system into the reactor by using a peristaltic pump, wherein the water amount is 35% of the total water amount of the system, and the water adding speed is 2.5g/min;
(6) After the water is added, the reaction is continued for 5-20min, the stirring speed is 150rpm, and the reaction temperature is 23 ℃;
(7) After the reaction is finished, solid-liquid phase separation is carried out, the mass of potassium chloride of solid decomposed ore is 71.81g, the yield of the potassium decomposed ore is 84.26%, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of fine sodium chloride with the grain size of less than or equal to 100 meshes is 3.01%.
Example 3
(1) The raw ore carnallite is carnallite in a dry-land salt-mining salt field, the average size fraction is 0.20mm, the maximum particle size is 2.50mm, the potassium ion content in the raw ore carnallite is 9.05 percent, the magnesium ion content is 5.35 percent, the sodium ion content is 15.02 percent, 500g of raw ore carnallite is taken, 164.21g of water is weighed, the raw ore carnallite and the water are transferred into a 1000ml beaker according to the proportion for reaction, the stirring speed is 500rpm, the reaction time is 40-60min, the raw ore carnallite is statically balanced for 12-24h, solid-liquid separation is carried out, saturated mother liquor is obtained, wherein the magnesium chloride content is 3.78mol/kgH 2 O；
(2) The saturated mother liquor is treated according to the following steps of: the saturated mother liquor was mixed at a weight ratio of 1: 0.89 to give a decomposition solution having a magnesium chloride content of 1.45mol/kgH 2 O, wherein the water amount is 75 percent of the total water amount of the system;
(3) Placing the decomposed solution into a 500ml beaker, wherein a paddle stirrer is used as the stirrer, and adding the raw ore carnallite into the beaker in three batches, wherein the weight ratio of the carnallite in the three batches is 1.8:1.8:1.9;
(4) The raw ore carnallite ore feeding speed is 15g/min, the stirring paddle speed is 200rpm, and the reaction time is 5-20min;
(5) Adding water required by the residual system into the reactor by using a peristaltic pump, wherein the water amount is 25% of the total water amount of the system, and the water adding speed is 2.5g/min;
(6) After the water is added, continuously reacting for 5-20min at the stirring speed of 150rpm and the reaction temperature of 23 ℃;
(7) After the reaction is finished, solid-liquid phase separation is carried out, the mass of potassium chloride of solid-phase decomposed ore is 72.82g, the yield of the potassium chloride is 84.31%, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of fine sodium chloride with the grain size of less than or equal to 100 meshes is 3.82%.
Comparative example 1
The process was the same as example 1 except that the magnesium chloride content in the decomposition solution in this comparative example was out of the range claimed in the present application; and provides corresponding result data.
(1) The raw ore carnallite is carnallite in a dry-land salt-mining field, the average size fraction is 0.20mm, the maximum particle size is 2.50mm, and the raw ore carnallite contains 9.05 percent of potassium ions, 5.35 percent of magnesium ions and 15.02 percent of sodium ions.
(2) Weighing 164.21g of water, and placing the water in a 1000ml beaker, wherein a stirrer is a paddle stirrer;
(3) Weighing 500g of carnallite raw ore, adding the raw ore carnallite into the raw ore in three batches, wherein the weight ratio of the carnallite in the three batches 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 the carnallite halide ore is added, continuing to react for 30-45min, wherein the stirring speed is 200rpm, and the reaction temperature is 25 ℃;
(6) After the reaction is finished, solid-liquid phase separation is carried out, the mass of potassium chloride of solid decomposed ore is 71.81g, the yield of the potassium decomposed ore is 83.36%, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of fine sodium chloride with the particle size of less than or equal to 100 meshes is 5.38%.
Comparative example 2
The process was the same as example 1 except that the number of times the carnallite ore was added in this comparative example was 1 or more,
(1) The raw ore carnallite is carnallite in dry-mining salt fields, the average size fraction is 0.20mm, the maximum particle 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) Weighing 164.21g of water, and putting the water in a 1000ml beaker, wherein a 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 feeding speed is 20g/min, and the stirring paddle speed is 300rpm
(5) After the carnallite halide ore is added, continuing to react for 30-45min at the stirring speed of 150rpm and the reaction temperature of 25 ℃;
(6) After the reaction is finished, solid-liquid phase separation is carried out, the mass of potassium chloride of solid-phase decomposed ore is 70.29g, the yield of the decomposed potassium is 82.07 percent, the decomposed ore is sieved by a 100-mesh Taylor sieve, and the content of fine sodium chloride with the mesh size of less than or equal to 100 is 6.33 percent.
In addition, the inventors of the present invention have also made experiments with other raw materials, process operations, and process conditions described in the present specification with reference to the above examples, and have obtained preferable results.
It should be understood that the technical solution of the present invention is not limited to the above-mentioned specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention without departing from the spirit of the present invention and the protection scope of the claims.
Claims (10)
1. A process for reducing fine sodium chloride in a potassium chloride product, comprising:
(1) Hydrolyzing carnallite ore to obtain saturated mother liquor with balanced three phases of potassium chloride, sodium chloride and carnallite;
(2) Mixing and diluting the saturated mother liquor 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) Adding carnallite ore into the decomposition solution in batches for reaction, and then separating to obtain a potassium chloride product with low fine sodium chloride content.
2. The method of claim 1, wherein: the carnallite is carnallite of dry-land salt-mining field obtained by evaporation of Carlsberg salt-mining field; preferably, 80wt% of the carnallite present in the carnallite has a particle size of greater than 0.125mm; preferably, the carnallite ore comprises sodium chloride, wherein 83wt% of the sodium chloride has a particle size of less than 0.85mm;
and/or, the content of potassium ions in the carnallite 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%.
3. The method of claim 1, wherein: the content of magnesium chloride in the saturated mother liquor is 3.64-4.22mol/kgH 2 The content of O and potassium chloride is 0.28-0.88mol/kgH 2 The content of O and sodium chloride is 0.44-0.46mol/kgH 2 O。
4. The method of claim 1, wherein: the content of magnesium chloride in the decomposition solution is 0.20-2.02mol/kgH 2 O；
And/or the decomposition solution is an equilibrium solution obtained by diluting saturated mother liquor with water;
and/or, the water in the step (2) is used in 50-80 wt% of the decomposition solution.
5. The method of claim 1, wherein step (3) comprises: putting the decomposed solution into a paddle type stirring device, adding carnallite ore into the decomposed solution in batches for reaction, and adding water to obtain reaction slurry; preferably, the stirring speed of the paddle type stirring device is 150-350 rpm; preferably, the water is added in an amount of 20 to 50wt% of the reaction slurry.
6. The method of claim 5, wherein: the mass ratio of the water added in the step (2) to the water added in the step (3) is 4-1: 1-2.
7. The method of claim 1, wherein: the reaction temperature in the step (3) is 20-30 ℃, and the reaction time is 30-65min.
8. The method of claim 1, wherein: the batch number of the carnallite ore added into the decomposition solution in the step (3) is three times; preferably, the mass ratio of the carnallite ore added for three times is 1.5-2: 1.3-2: 2.2-4;
and/or the rate of adding the carnallite ore into the decomposition solution in the step (3) is 2-25g/min.
9. The method of claim 1, wherein: the separation treatment comprises a screening treatment; preferably, the screening size of the screening treatment is 100-140 meshes.
10. Use of the process of any one of claims 1 to 9 for the decomposition of carnallite ore to produce potassium chloride.
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