CN116899741A - Method for reducing impurity content in carnallite ore - Google Patents
Method for reducing impurity content in carnallite ore Download PDFInfo
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- CN116899741A CN116899741A CN202310969307.1A CN202310969307A CN116899741A CN 116899741 A CN116899741 A CN 116899741A CN 202310969307 A CN202310969307 A CN 202310969307A CN 116899741 A CN116899741 A CN 116899741A
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- 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 158
- 238000000034 method Methods 0.000 title claims abstract description 96
- 239000012535 impurity Substances 0.000 title claims abstract description 73
- 238000005188 flotation Methods 0.000 claims abstract description 67
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000007873 sieving Methods 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims description 60
- 229910052791 calcium Inorganic materials 0.000 claims description 44
- 230000002000 scavenging effect Effects 0.000 claims description 19
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- -1 alkyl morpholine Chemical compound 0.000 claims description 16
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Natural products C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 13
- 239000004094 surface-active agent Substances 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 7
- 239000002002 slurry Substances 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 28
- 239000001103 potassium chloride Substances 0.000 abstract description 14
- 235000011164 potassium chloride Nutrition 0.000 abstract description 14
- 238000002425 crystallisation Methods 0.000 abstract description 13
- 230000008025 crystallization Effects 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 31
- 239000011734 sodium Substances 0.000 description 21
- 239000012141 concentrate Substances 0.000 description 19
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 16
- 235000002639 sodium chloride Nutrition 0.000 description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 229910001868 water Inorganic materials 0.000 description 14
- 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 12
- 229910052708 sodium Inorganic materials 0.000 description 12
- 239000000126 substance Substances 0.000 description 10
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000012267 brine Substances 0.000 description 3
- 239000001273 butane Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 239000008396 flotation agent Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 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
- JTJMJGYZQZDUJJ-UHFFFAOYSA-N phencyclidine Chemical class C1CCCCN1C1(C=2C=CC=CC=2)CCCCC1 JTJMJGYZQZDUJJ-UHFFFAOYSA-N 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000001612 separation test Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- VJXUJFAZXQOXMJ-UHFFFAOYSA-N D-1-O-Methyl-muco-inositol Natural products CC12C(OC)(C)OC(C)(C)C2CC(=O)C(C23OC2C(=O)O2)(C)C1CCC3(C)C2C=1C=COC=1 VJXUJFAZXQOXMJ-UHFFFAOYSA-N 0.000 description 1
- DSCFFEYYQKSRSV-KLJZZCKASA-N D-pinitol Chemical compound CO[C@@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@H]1O DSCFFEYYQKSRSV-KLJZZCKASA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 150000003841 chloride salts Chemical group 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010442 halite Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
- B03B9/00—General arrangement of separating plant, e.g. flow sheets
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application relates to the technical field of potassium chloride production, and particularly discloses a method for reducing impurity content in carnallite ore. The method comprises the steps of obtaining refined carnallite through pretreatment and reverse flotation; the pretreatment comprises the following steps: removing coarse fraction carnallite ore part in the raw ore pulp by a sieving mode; the removal granularity of the coarse fraction carnallite ore part is more than or equal to 1.5+/-1.0 mm; removing fine fraction carnallite ore in the raw ore pulp in a mechanical classification mode; the fine fraction carnallite ore part has a removal particle size to remove Ca in the reverse flotation carnallite ore ２＋ Is in an amount to satisfy the required Ca ２＋ Content requirement and K + The removal granularity with lower loss rate is a boundary value; only one reverse flotation collector is added in the reverse flotation. The application reduces the content of various impurities in carnallite ore through pretreatment and reverse flotation, and provides high-quality refined carnallite for the cold crystallization process so as to obtain high-quality KCl products in the later period.
Description
Technical Field
The application relates to the technical field of potassium chloride production, in particular to a method for reducing impurity content in carnallite ore.
Background
Potassium chloride is an important fertilizer and chemical raw material with strategic significance, and salt lake brine is mainly used as a raw material for potassium chloride production enterprises in China. Most of salt lake brine is chloride type potassium-containing brine, and is transported to a salt field, and then is subjected to beach sun-curing or forced evaporation to obtain carnallite type solid potassium salt mine. At present, various processing technologies of carnallite type solid potassium salt ores are formed, and mainly comprise a cold decomposition-positive flotation method, a cold decomposition-hot melting crystallization method, a reverse flotation-cold crystallization method, a brine-adding sodium-removing speed-control decomposition crystallization method, a salt field carnallite dissolution recrystallization method and the like. The potassium chloride product produced by the reverse flotation-cold crystallization process has high content, large grain diameter, low water content, low operation temperature, light corrosion to equipment and low construction investment cost, thereby becoming a relatively advanced and widely applied process route at present.
At present, the reverse flotation-cold crystallization process adopted by the production enterprises is to firstly float out impurity sodium chloride in carnallite ore by reverse flotation to obtain refined carnallite with sodium chloride content less than 6 percent, and then prepare potassium chloride products by crystallization. Since the impurities in carnallite ore are mainly stone salt (NaCl), gypsum (CaSO) 4 ·2H 2 O), water insoluble substances, etc., when the impurity content of gypsum and water insoluble substances is higher, the impurity content in the refined carnallite obtained by the reverse flotation process is also higher, and the cold crystallization process is directly affected, thus causing difficulty to the production of enterprises.
Therefore, there is a need for an effective de-doping method to reduce the content of various impurities in carnallite ore to solve the adverse effects of ore quality fluctuations.
In the related art, the method for removing impurities in the light halite mainly adopts alkyl morpholine surfactant as a collector to remove NaCl (simply called sodium removal) by reverse flotation, and the surfactant has good NaCl enrichment capacity, good selectivity and no need of being matched with other reagents, so that the method is widely applied to industrial production, but the surfactant cannot remove impurities such as calcium sulfate, water insoluble matters and the like. In the research of removing impurities such as calcium sulfate (decalcification for short), water insoluble substances and the like, flotation agents are adopted for removing impurities, and cyclones are also adopted for removing impurities.
Li Longgang et al (Li Longgang, zeng Ying, peng Shili, research on the removal of gypsum impurities from salt lake low-grade potassium carnallite ore by reverse flotation [ J ]]Chemical minerals and processing, 2016,45 (10): 11-13+28.) low grade potassium carnallite produced in a pergola salt lake is used as a raw material, GFR705 (550 g/t) flotation agent (combination of organic amine and sulfonate) is used to decalcify (gypsum) by reverse flotation to obtain Ca 2+ From 3.26% down to 0.62%, decalcified potassium carnallite was obtained. Decalcified potassium carnallite adopts octadecylamine hydrochloride to carry out positive flotation to obtain potassium chloride. The decalcification efficiency of the method reaches 87.72% by adopting reverse flotation, and the decalcification effect is good, but Ca is 2+ The content is still higher and is relative to Na + Poor impurity removal effect (Na + The content of the catalyst is reduced from 13.14% to 9.96%, and the catalyst is still high, so that the catalyst has a certain influence on subsequent production); the potassium chloride, K is floated by adopting a positive flotation process + The recovery rate is low, which is only 56.18%.
Wang Baocai et al (Wang Baocai, tang Hongxue, zhang Lin, xue Qin, yue Min. Preliminary investigation of flotation of calcium sulfate impurities from carnallite ore [ J)]The calcium sulfate in the light halate ore is subjected to flotation separation research by adopting a compound medicament (142 g/t) prepared from AN AN compound and a QHS-2 type flotation agent (2000 (08): 10-11+15). NaCl in the crude carnallite ore was reduced from 18.86% (Na + 7.43%) to 2.70% (Na) + About 1.06 percent), and the removal rate is more than 82 percent; caSO (Caso-like conductor) 4 From 1.38% (Ca) 2+ 0.406%) to 0.53% (Ca) 2+ About 0.156%) and the removal rate is about 69%. The removal effect of sodium is better, but the removal effect of calcium is general.
Li GoushengEt al (Liu Gousheng, song Jipin, zhang Xinlong, et al. Study of calcium sulfate cyclone separation test during reverse flotation-Cold crystalline Potassium chloride production [ J ]]Salt and chemical industry 2009,38 (03): 9-12+16.) separation of crude carnallite ore CaSO by hydrocyclone cyclone 4 . Two-stage series cyclone separation is studied, and the lower outlet material CaSO can be made 4 Reducing the recovery rate to 0.3 percent, and simultaneously improving the recovery rate of KCl through the reflux of materials. The method can reduce CaSO in carnallite ore 4 Content, but no control of the particle size limit is mentioned.
Disclosure of Invention
Based on the technical advantages of the reverse flotation-cold crystallization process and the defects of the method at the present stage, the application provides a method for reducing the impurity content in carnallite ore. The method reduces the content of various impurities in the carnallite ore through pretreatment and reverse flotation, and provides high-quality refined carnallite for the cold crystallization process so as to obtain high-quality KCl products in the later period.
The application provides a method for reducing impurity content in carnallite ore, which adopts the following technical scheme:
a method for reducing the impurity content in carnallite ore, which comprises the steps of obtaining refined carnallite through pretreatment and reverse flotation;
the pretreatment comprises the following steps:
removing coarse fraction carnallite ore part in the raw ore pulp by a sieving mode; the removal granularity of the coarse fraction carnallite ore part is more than or equal to 1.5+/-1.0 mm;
removing fine fraction carnallite ore in the raw ore pulp in a mechanical classification mode; the fine fraction carnallite ore part has a removal particle size to remove Ca in the reverse flotation carnallite ore 2+ Is in an amount to satisfy the required Ca 2+ Content requirement and K + The removal granularity with lower loss rate is a boundary value;
only one reverse flotation collector is added in the reverse flotation.
In the method provided by the application, the pretreatment comprises two parts, so that the content of various impurities in carnallite ore is effectively reduced, and a high-quality KCl product can be obtained in the later period. Wherein, a part is raw ore pulp sieving, coarse fraction carnallite ore is removed firstly by the raw ore pulp sieving mode, thus avoiding the influence of the coarse fraction carnallite ore on the later flotation index and the cold crystallization process due to the overlarge grain size of the coarse fraction carnallite ore. The removal granularity of the coarse fraction carnallite ore part is more than or equal to 1.5+/-1.0 mm. When the content of sodium and calcium impurities in the coarse fraction carnallite ore is high, the removal granularity limit value is biased to take a lower value, and conversely, is biased to take a higher value.
The other part is a fine fraction carnallite ore part in the separated raw ore pulp, the fine fraction carnallite ore part in the raw ore pulp is removed in a mechanical classification mode, and because calcium impurities and water insoluble substances are mostly enriched in the fine fraction carnallite ore part, the content of impurities can be effectively reduced by separating the fine fraction carnallite ore part in advance in a mechanical classification mode, so that the carnallite ore entering reverse flotation is reduced, and the use amount of reverse flotation agents is further reduced.
The removal of fine fraction carnallite ore fraction is mainly aimed at removing calcium impurities and water insoluble substances, and the removal granularity of fine fraction carnallite ore fraction is used for removing Ca in reverse flotation carnallite ore 2+ Is in an amount to satisfy the required Ca 2+ Content requirement and K + The removal granularity with lower loss rate is defined as a boundary value.
In addition, reverse flotation is mainly aimed at removing sodium impurities. Just because most of impurities in the pretreated raw ore pulp are removed, only one reagent needs to be added as an anti-flotation collector in the anti-flotation stage.
Preferably, the raw ore slurry is low-calcium carnallite ore or high-calcium carnallite ore.
Preferably, the reverse flotation collector is an alkyl morpholine surfactant.
Preferably, the coarse fraction carnallite ore is partly ground and the fraction smaller than the removal particle size is added to the raw pulp.
The coarse fraction carnallite ore removed by the raw ore pulp sieving method is ground, and the part smaller than the removal granularity (namely the part smaller than the limit value) is added into the raw ore pulp after grinding, so that the carnallite ore is utilized to the maximum extent, the waste of raw materials is avoided, and meanwhile, the high-quality KCl product can be obtained from the raw materials to the maximum extent.
Preferably, the mechanical classification means comprises a sieving or cyclone.
Preferably, the reverse flotation adopts a process flow of one roughing and N (N is more than or equal to 0) scavenging.
Preferably, the number of times of scavenging is selected to obtain Na in the refined carnallite + The content is the reference. When Na is + K is selected at a content of < 2.36% (i.e. NaCl < 6.0%) + The number of times of scavenging with higher recovery rate.
Preferably, the coarse fraction carnallite ore fraction has a removal particle size of 1.25mm.
Preferably, the fine fraction carnallite fraction has a removal particle size of 0.074mm.
In summary, the application has the following beneficial effects:
1. the method provided by the application can effectively reduce the content of sodium, calcium, water insoluble substances and other impurities in carnallite ores. The high-quality refined carnallite can be obtained for low-calcium carnallite ore, and the impurity removal effect is more remarkable for refractory high-calcium carnallite ore than for flotation reagent impurity removal, so that the refined carnallite meeting the production requirement can be obtained.
2. According to the method provided by the application, the ore quantity entering reverse flotation can be reduced by pretreatment, the influence of coarse fraction and ore slime on flotation is eliminated, and the dosage of flotation agents can be reduced. Meanwhile, large particles can be eliminated in advance, and the problem of potassium chloride quality degradation caused by incomplete decomposition of the large particles in a decomposition crystallizer is avoided.
3. The method provided by the application can be flexibly regulated and controlled according to the quality requirement of the product, and refined carnallite with different quality can be produced.
Drawings
Fig. 1 is a process flow diagram of a method for reducing the impurity content in carnallite ore provided by the application.
Fig. 2 is a process flow diagram of the method for reducing the impurity content in carnallite ore provided in example 1.
Fig. 3 is a process flow diagram of the method for reducing the impurity content in carnallite ore provided in example 2.
Fig. 4 is a process flow diagram of the method for reducing the impurity content in carnallite ore provided in example 3.
Detailed Description
The application provides a method for reducing impurity content in carnallite ore, which specifically comprises the following steps in combination with fig. 1:
(1) Pretreatment of
The raw ore pulp is screened (the mesh number of the screen determines the removal granularity), coarse-grain carnallite ore part is arranged on the screen, coarse-grain raw ore pulp is removed under the screen, and therefore the purpose of removing the coarse-grain carnallite ore part in the raw ore pulp is achieved. Further, coarse fraction carnallite ore on the screen is partly ground, and a fraction smaller than the removal particle size is added to the coarse-grained raw ore slurry under the screen. Wherein the removal granularity of the coarse fraction carnallite ore part is more than or equal to 1.5+/-1.0 mm. The raw ore pulp can be low-calcium carnallite ore or high-calcium carnallite ore.
And removing the fine fraction carnallite ore part in the coarse-grained raw ore pulp obtained by the mechanical classification mode to obtain the pretreated raw ore pulp. Mechanical classification means include sieving or cyclones. The fine fraction carnallite ore fraction is mainly calcium impurities and water insoluble. Removing granularity of fine fraction carnallite ore part, and then adding Ca into reverse flotation carnallite ore 2+ Is in an amount to satisfy the required Ca 2+ Content requirement and K + The removal granularity with lower loss rate is defined as a boundary value.
(2) Reverse flotation
And (3) performing reverse flotation on the pretreated raw ore pulp obtained by adopting a process flow of one-time roughing and N (N is more than or equal to 0) scavenging. The method comprises the following steps:
carrying out primary roughing on the pretreated raw ore pulp to obtain roughing concentrate and tailings to be cleaned;
scavenging the tailings to be scavenged for N (N is more than or equal to 0) times to obtain scavenged concentrate and tailings;
and combining the obtained scavenging concentrate and roughing concentrate to obtain the refined carnallite.
Only one reverse flotation collector is added in reverse flotation. The reverse flotation collector may be an alkyl morpholine surfactant. Number of sweeps to obtain Na in refined carnallite + The content is the reference. When Na is + K is selected at a content of < 2.36% (i.e. NaCl < 6.0%) + The number of times of scavenging with higher recovery rate.
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. All other embodiments, which can be made by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application.
The present application will be described in further detail with reference to examples, drawings, comparative examples and performance test results.
Examples and comparative examples
The following examples 1 and comparative examples 1-2 were run on mineral separation tests with low-calcium carnallite ore, which is mainly sodium impurity, other impurity content (Ca 2+ About 0.19%, about 0.22% of water insoluble material) and easy to sort. And the contents of various impurities after the treatment in each step in the above examples and comparative examples were examined, and the examination results are shown in table 1.
Example 1
The present embodiment provides a method for reducing the impurity content in carnallite ore.
The method specifically comprises the following steps:
(1) Pretreatment of
The raw ore pulp (low-calcium carnallite ore) is screened (the removal granularity is 1.25 mm), coarse-grain-grade carnallite ore part is arranged on the screen, and coarse-grain-removed raw ore pulp is arranged below the screen. Grinding coarse fraction carnallite ore on the sieve, and adding the fraction smaller than the removal granularity into coarse-grain-removed raw ore pulp under the sieve.
And removing fine fraction carnallite ore in the coarse-grained raw ore pulp obtained by the mechanical classification (screening) to obtain pretreated raw ore pulp, wherein the removal granularity is 0.074mm, so as to remove calcium impurities and water insoluble substances in the raw ore pulp.
(2) Reverse flotation
And (3) taking alkyl morpholine (21 g/t) as a collector, and performing reverse flotation on the pretreated raw ore pulp obtained by adopting a process flow of one-time roughing and one-time scavenging. The method comprises the following steps:
carrying out primary roughing on the pretreated raw ore pulp to obtain roughing concentrate and tailings to be cleaned;
scavenging the tailings to be scavenged for one time to obtain scavenged concentrate and tailings;
and combining the obtained scavenging concentrate and roughing concentrate to obtain refined carnallite, namely concentrate.
Comparative example
Comparative example 1
This comparative example provides a method for reducing the impurity content in carnallite ores. This comparative example differs from example 1 in that: the low-calcium carnallite ore is directly subjected to reverse flotation without pretreatment.
The method specifically comprises the following steps:
reverse flotation: the method is characterized in that alkyl morpholine (21 g/t) is used as a collector, and a reverse flotation process of primary roughing and primary scavenging is adopted to carry out reverse flotation on raw ore pulp (low-calcium carnallite ore), and the method comprises the following specific steps:
carrying out primary roughing on the raw ore pulp (low-calcium carnallite ore) to obtain roughing concentrate and roughing tailings to be cleaned;
scavenging the tailings to be scavenged for one time to obtain scavenged concentrate and tailings;
and combining the obtained scavenging concentrate and roughing concentrate to obtain the refined carnallite.
Comparative example 2
This comparative example provides a method for reducing the impurity content in carnallite ores. This comparative example differs from example 1 in that: the low-calcium carnallite ore is not pretreated and the collectors used in the reverse flotation step are different.
The method specifically comprises the following steps:
reverse flotation: alkyl morpholine (23 g/t, sodium removal) and a gemini surfactant butane, 1, 4-bis (hexadecyl morpholinyl ammonium bromide) (50 g/t, decalcification) are taken as collectors, and a two-time roughing reverse flotation process (one-time sodium removal and one-time decalcification) is adopted to carry out reverse flotation on raw ore slurry (low-calcium carnallite ore) to obtain refined carnallite and tailings.
TABLE 1 content of impurities in "Low-calcium carnallite ore" after treatment in each step of example 1 and comparative examples 1 to 2
As can be seen from the detection results in Table 1, the method of the application is used for separating low-calcium carnallite ore and Na in refined carnallite + 、Ca 2+ The impurity content is low, and Ca can be obtained 2+ High quality fine carnallite, K < 0.12% + 、Mg 2+ The recovery rate (the subsequent cold crystallization process can be recovered) is also higher, and the mineral separation index is better. From the above, the method provided by the application can effectively reduce the content of various impurities in the low-calcium carnallite ore, and provide high-quality refined carnallite for the cold crystallization process so as to obtain high-quality KCl products in the later period.
Examples 2 to 3 and comparative examples 3 to 6 below were subjected to beneficiation tests with high-calcium carnallite ore, which was contaminated with (Na + About 17%, ca 2+ About 1.5%, water insoluble about 5%) is higher and more difficult to sort. And the contents of various impurities after the treatment in each step in the above examples and comparative examples were examined, and the examination results are shown in table 2.
Example 2
The present embodiment provides a method for reducing the impurity content in carnallite ore.
The method specifically comprises the following steps:
(1) Pretreatment of
The raw ore pulp (high-calcium carnallite ore) is screened (the removal granularity is 1.25 mm), coarse-grain-grade carnallite ore part is arranged on the screen, and coarse-grain-removed raw ore pulp is arranged below the screen. Grinding coarse fraction carnallite ore on the sieve, and adding the fraction smaller than the removal granularity into coarse-grain-removed raw ore pulp under the sieve.
And removing fine fraction carnallite ore in the coarse-grained raw ore pulp obtained by the mechanical classification (screening) to obtain pretreated raw ore pulp, wherein the removal granularity is 0.074mm, so as to remove calcium impurities and water insoluble substances in the raw ore pulp.
(2) Reverse flotation
And (3) taking alkyl morpholine (165 g/t) as a collector, and performing reverse flotation on the pretreated raw ore pulp obtained by adopting a process flow of one-time roughing and two-time scavenging. The method comprises the following steps:
carrying out primary roughing on the pretreated raw ore pulp to obtain roughing concentrate and tailings to be cleaned;
scavenging the tailings to be scavenged twice to obtain scavenged concentrate and tailings;
combining the twice scavenging concentrate and the roughing concentrate to obtain refined carnallite, namely the concentrate.
Example 3
The present embodiment provides a method for reducing the impurity content in carnallite ore. This embodiment differs from embodiment 2 in that: the parameters of each step are different.
The differences are as follows:
pretreatment: removing fine fraction carnallite ore in the coarse-grained raw ore pulp obtained by the mechanical classification method, wherein the removal granularity is 0.088mm;
reverse flotation: the amount of collector added was 140g/t.
Comparative example 3
Comparative example 3 provides a method of reducing the impurity content in carnallite ore. This comparative example differs from example 2 in that: the high calcium carnallite ore is not pretreated and the reverse flotation step is different.
The method specifically comprises the following steps:
reverse flotation: the method comprises the following steps of (1) taking alkyl morpholine (184 g/t+74 g/t) as a collector, and adopting a two-time roughing reverse flotation process to carry out reverse flotation on raw ore pulp (high-calcium carnallite ore), wherein the specific steps are as follows:
and (3) carrying out rough concentration on the raw ore pulp (high-calcium carnallite ore) twice to obtain refined carnallite, tailings 1 and tailings 2.
Comparative example 4
Comparative example 4 provides a method of reducing the impurity content in carnallite ore. This comparative example differs from example 2 in that: the high calcium carnallite ore is not pretreated and the reverse flotation step is different.
The method specifically comprises the following steps:
reverse flotation: reverse flotation is carried out on raw ore pulp (high-calcium carnallite ore) by adopting a reverse flotation process (primary decalcification and primary sodium removal) of twice roughing (sectional addition of a collector), oleic acid (4.7 kg/t) and pinitol oil (100 g/t) are adopted as the collectors at one time, calcium impurities and water insoluble substances are removed, and alkyl morpholine (80 g/t) is adopted as the collector at one time, so that sodium impurities are removed. The method comprises the following steps:
and (3) carrying out rough concentration on the raw ore pulp (high-calcium carnallite ore) twice to obtain refined carnallite, tailings 1 and tailings 2.
Comparative example 5
Comparative example 5 provides a method of reducing the impurity content in carnallite ore. This comparative example differs from example 2 in that: the high calcium carnallite ore is not pretreated and the reverse flotation step is different.
The method specifically comprises the following steps:
reverse flotation: the method comprises the steps of taking alkyl morpholine (182 g/t, sodium removal) and gemini surfactant butane, 1, 4-bis (hexadecyl morpholinyl ammonium bromide) (81 g/t, decalcification) as collectors together, and carrying out reverse flotation on raw ore slurry (high-calcium carnallite ore) by adopting a reverse flotation process of primary roughing to obtain refined carnallite and tailings.
Comparative example 6
Comparative example 6 provides a method of reducing the impurity content in carnallite ore. This comparative example differs from example 2 in that: the high calcium carnallite ore is not pretreated and the reverse flotation step is different.
The method specifically comprises the following steps:
reverse flotation: the method comprises the steps of taking a gemini surfactant butane and 1, 4-bis (hexadecyl morpholinyl ammonium bromide) (500 g/t, decalcification) as collectors, and adopting a primary roughing reverse flotation process to carry out reverse flotation on raw ore pulp (high-calcium carnallite ore) to obtain refined carnallite and tailings.
TABLE 2 content of impurities in "high calcium carnallite ore" after treatment in each step of examples 2 to 3 and comparative examples 3 to 6
As is clear from the results of comparative example 3, alkyl morpholine was able to effectively remove sodium but not calcium, and Ca in the resulting refined carnallite 2+ Higher levels will have an impact on the production at the next stage.
As is clear from the detection result of comparative example 4, the primary roughing in reverse flotation has a certain effect on decalcification, but is still not ideal, the consumption of the collector is large, and meanwhile, the decalcification agent affects the sodium-removed alkyl morpholine agent, so that the sodium-removal effect is poor.
As is clear from the detection result of comparative example 5, the two collectors do not produce a good synergistic effect, and Na in the obtained refined carnallite + 、Ca 2+ The impurity content is high.
From the results of comparative example 6, it was found that the gemini surfactant was able to remove 75.92% of calcium impurities, but the resulting refined carnallite had Ca 2+ The impurity content is still higher and the collector consumption is also higher.
Example 2 and example 3 are both Na in the refined carnallite obtained by the process of the application + 、Ca 2+ The impurity content was low, especially Na in the refined carnallite obtained by the method of example 3 + 、Ca 2+ The refined carnallite K obtained in example 2 has a lower impurity content + 、Mg 2+ The recovery rate is higher. The detection result shows that the method provided by the application can effectively reduce the content of various impurities in the high-calcium carnallite ore, and can control the impurity content according to concentrate requirements.
According to the method, refractory high-calcium carnallite ore is selected, the impurity content in the obtained refined carnallite can be effectively reduced, the ore which is difficult to normally produce can be effectively utilized, and the method has the advantages of low medicament consumption and good ore dressing index.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and are not limiting; although the application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present application.
Claims (9)
1. A method for reducing the impurity content in carnallite ore, which is characterized in that the method comprises the steps of pretreatment and reverse flotation to obtain refined carnallite;
the pretreatment comprises the following steps:
removing coarse fraction carnallite ore part in the raw ore pulp by a sieving mode; the removal granularity of the coarse fraction carnallite ore part is more than or equal to 1.5+/-1.0 mm;
removing fine fraction carnallite ore in the raw ore pulp in a mechanical classification mode; the fine fraction carnallite ore part has a removal particle size to remove Ca in the reverse flotation carnallite ore ２＋ Is in an amount to satisfy the required Ca ２＋ Content requirement and K + The removal granularity with lower loss rate is a boundary value;
only one reverse flotation collector is added in the reverse flotation.
2. The method of reducing the impurity level in carnallite ore according to claim 1, wherein the raw ore slurry is low-calcium carnallite ore or high-calcium carnallite ore.
3. The method of reducing the impurity level in carnallite ore according to claim 1, wherein the reverse flotation collector is an alkyl morpholine surfactant.
4. The method of reducing the impurity level in carnallite ore according to claim 1, wherein the coarse fraction of carnallite ore is ground and the fraction smaller than the removal particle size is added to the raw ore slurry.
5. The method of reducing the impurity level in carnallite ore according to claim 1, wherein the mechanical classification means comprises sieving or cyclone.
6. The method for reducing the impurity content in carnallite ore according to claim 1, wherein the reverse flotation adopts a process flow of one roughing and N (N is not less than 0) scavenging.
7. The method for reducing the impurity content in carnallite ore according to claim 1, wherein the number of times of scavenging is such that Na in the obtained refined carnallite + The content is the reference. When Na is + K is selected at a content of < 2.36% (i.e. NaCl < 6.0%) + The number of times of scavenging with higher recovery rate.
8. The method of reducing the impurity level in carnallite ore according to claim 1, wherein the coarse fraction carnallite ore fraction has a removal particle size of 1.25mm.
9. The method of reducing the impurity level in carnallite ore according to claim 1, wherein preferably the fine fraction carnallite ore fraction has a removal particle size of 0.074mm.
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