A kind of iso-floatable separation process of mud-containing lepidolite

Abstract

The present invention discloses a kind of iso-floatable separation process of mud-containing lepidolite, which comprises: mixing raw ore with sodium hexametaphosphate and then finely grinding; adding collector JL-1 to the grinding product for flotation to obtain a foam product and a pulp product; the foam product is subjected to two-stage selection with sodium hexametaphosphate as a depressant to obtain lithium concentrate one, the selected tailings are scavenged with JL-1 as a collector and sodium hexametaphosphate as a depressant, and the scavenged foam product is returned to the first stage of selection; the pulp product is subjected to a one-coarse-two-fine-two-scavenging flotation process with JL-2 as a collector and sodium hexametaphosphate as a depressant to obtain lithium concentrate two. This application makes full use of the difference in the natural floatability of minerals, selects lepidolite collector JL-1 with strong selectivity to carry out iso-floatable separation on the raw ore, obtains easy-floating minerals and difficult-floating minerals, and then respectively carries out targeted recovery by lepidolite collector JL-1 and lepidolite collector JL-2 with strong collecting property to improve the grade of each section of lepidolite.

Description

Technical Field

[0001] The present invention relates to the field of lepidolite beneficiation, and in particular to an iso-floatable separation process for mud-containing lepidolite. Background Art

[0002] Lepidolite is one of the important minerals for lithium extraction. It is a silicate mineral belonging to the mica family. Its color is generally pink or purple, sometimes light to colorless. It usually exists in the form of fine scales or small flake aggregates and has a significant pearly luster. It is also called "lepidolite". Its chemical composition is K{Li 2-x Al 1+x [Al 2x Si 4-2x O 10 ](F,OH)2} (x = 0-0.5), and is often associated with various siliceous minerals such as quartz, feldspar, kaolin, montmorillonite, and serpentine. Currently, the primary recovery process for lepidolite is flotation. However, due to its unique flaky structure, lepidolite is difficult to grind. Prolonging the grinding time leads to an increase in secondary slime, which often covers the lepidolite particles, thereby reducing the yield and recovery rate of the lepidolite concentrate.

[0003] Because lepidolite deposits typically undergo severe weathering, the raw ore often contains a large amount of primary slime. The recycling of intermediate ore in actual production further leads to the continuous accumulation of slime during the beneficiation process, thereby deteriorating flotation conditions. Current lepidolite beneficiation processes generally use pre-flotation desliming to reduce the impact of slime on flotation, but this method in turn leads to lepidolite losses. To achieve more efficient recovery of lepidolite, the development of flotation processes and reagents suitable for high-mud lepidolite is a critical issue that urgently needs to be addressed. Summary of the Invention

[0004] The main purpose of the present invention is to provide a floatable separation process for mud-containing lepidolite, aiming to solve the above problems.

[0005] To achieve the above object, the present invention proposes a flotation separation process for mud-containing lepidolite, comprising:

[0006] S1, mixing the raw ore with sodium hexametaphosphate and then finely grinding it through a mill;

[0007] S2. Add collector JL-1 to the grinding product for flotation to obtain foam product and pulp product;

[0008] S3, the foam product in step S2 is subjected to two-stage selection with sodium hexametaphosphate as an inhibitor to obtain lithium concentrate 1, the selected tailings are scavenged with JL-1 as a collector and sodium hexametaphosphate as an inhibitor, the scavenged foam product is returned to the first stage of selection, and the remaining product forms the tailings;

[0009] S4. The pulp product in step S2 is subjected to a one-rough, two-fine, two-sweep flotation process using JL-2 as a collector and sodium hexametaphosphate as a depressant to obtain lithium concentrate and tailings. The tailings and the tailings in step S3 together form the final tailings, and the middlings at each level are returned to the previous flotation process.

[0010] In one embodiment, the raw ore is lepidolite, the grade of Li2O in the raw ore is between 0.2% and 1.2%, and the mass proportion of -325 mesh minerals in the raw ore is between 5% and 35%.

[0011] In one embodiment, the flotation collector JL-1 includes at least one of dodecylamine, sodium oleate, sodium dodecylsulfonate, dodecylamine polyoxyethylene ether, and tributyl phosphate.

[0012] In one embodiment, the JL-2 includes at least one of dodecylamine, sodium linoleate, sodium laurylsulfonate, octadecylamine polyoxyethylene ether, and polyethylene glycol.

[0013] In one embodiment, in steps S2, S3 and S4, the pH range of the slurry is controlled to be 6-8.

[0014] In one embodiment, in step S1, the amount of sodium hexametaphosphate used is 200 g / t-1000 g / t.

[0015] In one embodiment, in step S2, the amount of JL-1 used is 300 g / t to 800 g / t.

[0016] In one embodiment, in step S3, the amount of sodium hexametaphosphate used is 200 g / t-500 g / t, and the amount of collector JL-1 used is 100 g / t-300 g / t.

[0017] In one embodiment, in step S4, the amount of sodium hexametaphosphate used in the roughing process is 100g / t-500g / t, and the amount of collector JL-2 used is 200g / t-600g / t; the amount of sodium hexametaphosphate used in the cleaning process is 200g / t-500g / t; the amount of sodium hexametaphosphate used in the scavenging process is 100g / t-300g / t, and the amount of collector JL-2 used is 100g / t-300g / t.

[0018] The beneficial effects of the present invention are as follows:

[0019] (1) Taking full advantage of the differences in the natural floatability of minerals, the highly selective lepidolite collector JL-1 was selected to perform equal floatation separation on the raw ore to obtain easy-floating minerals and difficult-floating minerals, which were then recovered separately through the lepidolite collector JL-1 and the highly selective lepidolite collector JL-2 to improve the grade of each section of lepidolite.

[0020] (2) Using the equal floatability separation process, a segmented flotation strategy is adopted based on the natural flotation of the minerals, avoiding the forced suppression of easily floatable minerals and adapting to the complex composition of the original ore. This method can effectively reduce the interference of fine mud on the flotation process, while reducing the amount of flotation reagents and the amount of foam generated. It not only ensures the high selectivity of the flotation process, but also facilitates control and stable operation, reducing the entrainment phenomenon caused by flotation foam and the difficulties in subsequent pipeline transportation.

[0021] (3) Lepidolite collector JL-1 and Lepidolite collector JL-2 have a certain synergistic effect, which can further improve the collection effect of difficult-to-float minerals. At the same time, the mineral processing wastewater generated during the flotation of easy-to-float minerals and difficult-to-float minerals can be recycled in the corresponding process to reduce treatment costs.

[0022] (4) The present invention creatively separates lepidolite according to its floatability and carries out targeted recovery of the two parts of minerals, thereby achieving full recovery of lepidolite of various particle sizes. It also has many advantages such as high concentrate quality, high sorting efficiency, low reagent dosage and wide applicability. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the structures shown in these drawings without paying any creative work.

[0024] Figure 1 The figure is a schematic flow chart of the iso-floatable separation process of mud-containing lepidolite according to an embodiment of the present invention.

[0025] The purpose, features and advantages of the present invention will be further described with reference to the accompanying drawings and in conjunction with the embodiments. DETAILED DESCRIPTION

[0026] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0027] Moreover, the technical solutions between the various embodiments of the present invention may be combined with each other, but this must be based on the fact that ordinary technicians in this field can implement them. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the present invention.

[0028] The invention provides an iso-floatable separation process for mud-containing lepidolite.

[0029] like Figure 1 As shown, the iso-floatable separation process of mud-containing lepidolite provided by the embodiment of the present invention includes:

[0030] S1, mixing the raw ore with sodium hexametaphosphate and then finely grinding it through a mill;

[0031] S2. Add collector JL-1 to the grinding product for flotation to obtain foam product and pulp product;

[0032] S3, the foam product in step S2 is subjected to two-stage selection with sodium hexametaphosphate as an inhibitor to obtain lithium concentrate 1, the selected tailings are scavenged with JL-1 as a collector and sodium hexametaphosphate as an inhibitor, the scavenged foam product is returned to the first stage of selection, and the remaining product forms the tailings;

[0033] S4. The pulp product in step S2 is subjected to a one-rough, two-fine, two-sweep flotation process using JL-2 as a collector and sodium hexametaphosphate as a depressant to obtain lithium concentrate and tailings. The tailings and the tailings in step S3 together form the final tailings, and the middlings at each level are returned to the previous flotation process.

[0034] Furthermore, the raw ore is lepidolite, the grade of Li2O in the raw ore is between 0.2% and 1.2%, and the mass proportion of -325 mesh minerals in the raw ore is between 5% and 35%.

[0035] Furthermore, the flotation collector JL-1 includes at least one of dodecylamine, sodium oleate, sodium dodecylsulfonate, dodecylamine polyoxyethylene ether and tributyl phosphate.

[0036] Furthermore, the JL-2 includes at least one of dodecylamine, sodium linoleate, sodium laurylsulfonate, octadecylamine polyoxyethylene ether and polyethylene glycol.

[0037] Furthermore, in steps S2, S3 and S4, the pH range of the slurry is controlled to be 6-8.

[0038] Furthermore, in step S1, the amount of sodium hexametaphosphate used is 200 g / t-1000 g / t.

[0039] Furthermore, in step S2, the amount of JL-1 used is 300 g / t to 800 g / t.

[0040] Furthermore, in step S3, the amount of sodium hexametaphosphate used is 200 g / t-500 g / t, and the amount of collector JL-1 used is 100 g / t-300 g / t.

[0041] Furthermore, in step S4, the amount of sodium hexametaphosphate used in the roughing process is 100g / t-500g / t, and the amount of collector JL-2 used is 200g / t-600g / t; the amount of sodium hexametaphosphate used in the cleaning process is 200g / t-500g / t; the amount of sodium hexametaphosphate used in the scavenging process is 100g / t-300g / t, and the amount of collector JL-2 used is 100g / t-300g / t.

[0042] Furthermore, the mill in step S1 should be one of a ball mill, a rod mill, an autogenous mill or a semi-autogenous mill.

[0043] Furthermore, in steps S2, S3 and S4, the mixture must be stirred for 3-10 minutes after the addition of the reagent before proceeding to the next step.

[0044] Among them, g / t represents the ratio of the mass of collector to the mass of ore in the flotation process.

[0045] Compared with the prior art, the present invention has the following beneficial effects:

[0046] (1) Taking full advantage of the differences in the natural floatability of minerals, the highly selective lepidolite collector JL-1 was selected to perform equal floatation separation on the raw ore to obtain easy-floating minerals and difficult-floating minerals, which were then recovered separately through the lepidolite collector JL-1 and the highly selective lepidolite collector JL-2 to improve the grade of each section of lepidolite.

[0047] (2) Using the equal floatability separation process, a segmented flotation strategy is adopted based on the natural flotation of the minerals, avoiding the forced suppression of easily floatable minerals and adapting to the complex composition of the original ore. This method can effectively reduce the interference of fine mud on the flotation process, while reducing the amount of flotation reagents and the amount of foam generated. It not only ensures the high selectivity of the flotation process, but also facilitates control and stable operation, reducing the entrainment phenomenon caused by flotation foam and the difficulties in subsequent pipeline transportation.

[0048] (3) Lepidolite collector JL-1 and Lepidolite collector JL-2 have a certain synergistic effect, which can further improve the collection effect of difficult-to-float minerals. At the same time, the mineral processing wastewater generated during the flotation of easy-to-float minerals and difficult-to-float minerals can be recycled in the corresponding process to reduce treatment costs.

[0049] (4) The present invention creatively separates lepidolite according to its floatability and carries out targeted recovery of the two parts of minerals, thereby achieving full recovery of lepidolite of various particle sizes. It also has many advantages such as high concentrate quality, high sorting efficiency, low reagent dosage and wide applicability.

[0050] The technical solutions of the present invention are further illustrated below by specific examples. Those skilled in the art should understand that the examples are only provided to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0051] Example 1

[0052] The experimental object is a lepidolite mine in Jiangxi Province. The process mineralogy study shows that the ore belongs to the porcelain stone type lepidolite ore with a Li2O grade of 0.43%. The main valuable mineral is lepidolite. Lithium is mainly contained in lepidolite. The main gangue minerals are quartz and potassium-sodium feldspar. The associated mud minerals are feldspar, montmorillonite and other clay minerals. The on-site desludging amount is about 10%. The chemical analysis of the ore is shown in Table 1. The flotation system is as follows: Figure 1 shown.

[0053]

[0054] Table 1 Chemical analysis results of raw ore

[0055] The experimental steps are as follows:

[0056] (1) The raw ore was fed into a ball mill at a pulp concentration of 40%, 500 g / t of sodium hexametaphosphate was added, the grinding time was 5 min, and the ore was passed through a 40-mesh sieve to obtain flotation pulp.

[0057] (2) The slurry obtained in step (1) was added to a flotation machine, 450 g / t of collector JL-1 was added, and flotation was performed after stirring for 5 minutes.

[0058] (3) The foam product in step (2) was subjected to two-stage selection, wherein the amounts of sodium hexametaphosphate used in the two-stage selection were 350 g / t and 250 g / t, respectively; the selected tailings were combined and scavenged, wherein the amount of sodium hexametaphosphate used was 200 g / t, the amount of collector JL-1 used was 150 g / t, and the stirring time after adding the drugs was 3 min, thereby finally obtaining lithium concentrate 1.

[0059] (4) The slurry product in step (2) was subjected to a one-roughing, two-fine, two-scavenging beneficiation process, with the roughing sodium hexametaphosphate dosage being 350 g / t and the collector JL-2 dosage being 400 g / t; the two-stage fine concentration sodium hexametaphosphate dosages being 300 g / t and 200 g / t, respectively; the two-stage scavenging sodium hexametaphosphate dosages being 250 g / t and 200 g / t, and the collector JL-2 dosages being 200 g / t and 150 g / t, respectively. The stirring time after adding the drugs was 3 min, and lithium concentrate 2 was finally obtained.

[0060] Comparative Example 1-1

[0061] The difference between Comparative Example 1-1 and Example 1 is that: in Comparative Example 1, the collector is only JL-1, the flotation system is one coarse, two fine and one scavenging, the middlings are returned to the previous flotation process, and the reagent system is as follows: the roughing amount of sodium hexametaphosphate is 1200g / t, the collector amount is 600g / t, and the two-stage concentrating amounts of sodium hexametaphosphate are 600g / t and 400g / t respectively; the scavenging amount of sodium hexametaphosphate is 400g / t, the collector amount is 250g / t, and the stirring time is 3min.

[0062] Comparative Example 1-2

[0063] The difference between Comparative Example 1-2 and Example 1 is that: in Comparative Example 1, the collector is only JL-2, the flotation system is one coarse, two fine and one sweep, the middlings are returned to the previous flotation process, and the reagent system is as follows: the roughing sodium hexametaphosphate dosage is 800g / t, the collector dosage is 650g / t, and the two-stage cleaning sodium hexametaphosphate dosages are 600g / t and 400g / t, respectively; the scavenging sodium hexametaphosphate dosage is 400g / t, the collector dosage is 300g / t, and the stirring time is 3min.

[0064]

[0065] Table 2 Flotation data of porcelain stone type lepidolite

[0066] Example 2

[0067] The experimental object is a lepidolite mine in Jiangxi Province. The process mineralogy study shows that the ore belongs to the porcelain clay type lepidolite ore with a Li2O grade of 0.55%. The main valuable mineral is lepidolite. Lithium is mainly contained in lepidolite. The main gangue minerals are quartz and potassium-sodium feldspar. The argillaceous minerals include feldspar, montmorillonite, kaolin and other clay minerals. The on-site desludging amount is about 20%. The chemical analysis of the ore is shown in Table 3. The flotation system is as follows: Figure 1 shown.

[0068] Table 3 Chemical analysis results of raw ore

[0069]

[0070] The experimental steps are as follows:

[0071] (1) The raw ore was fed into a ball mill at a pulp concentration of 40%, 800 g / t of sodium hexametaphosphate was added, the grinding time was 3 min, and the ore was passed through a 40-mesh sieve to obtain flotation pulp.

[0072] (2) The slurry obtained in step (1) was added to a flotation machine, 500 g / t of collector JL-1 was added, and flotation was performed after stirring for 10 min.

[0073] (3) The foam product in step (2) was subjected to two-stage selection, wherein the amounts of sodium hexametaphosphate used in the two stages were 400 g / t and 300 g / t, respectively; the selected tailings were combined and scavenged, wherein the amount of sodium hexametaphosphate used was 200 g / t, the amount of collector JL-1 used was 200 g / t, and the stirring time after adding the drugs was 5 min to obtain lithium concentrate 1.

[0074] (4) The slurry product in step (2) was subjected to a one-roughing, two-fine, two-scavenging beneficiation process, with the roughing sodium hexametaphosphate dosage of 500 g / t and the collector JL-2 dosage of 400 g / t; the two-stage fine concentration sodium hexametaphosphate dosages were 300 g / t and 200 g / t, respectively; the two-stage scavenging sodium hexametaphosphate dosages were 250 g / t and 200 g / t, and the collector JL-2 dosages were 200 g / t and 150 g / t, respectively. The stirring time after adding the drugs was 5 min to obtain lithium concentrate 2.

[0075] Comparative Example 2-1

[0076] The difference between Comparative Example 1-1 and Example 1 is that: in Comparative Example 1, the collector is only JL-1, the flotation system is one coarse, two fine and one scavenging, the middlings are returned to the previous flotation process, and the reagent system is as follows: the roughing amount of sodium hexametaphosphate is 1500g / t, the collector amount is 700g / t, and the two-stage cleaning amounts of sodium hexametaphosphate are 650g / t and 450g / t respectively; the scavenging amount of sodium hexametaphosphate is 500g / t, the collector amount is 350g / t, and the stirring time is 5min.

[0077] Comparative Example 2-2

[0078] The difference between Comparative Example 1-2 and Example 1 is that: in Comparative Example 1, the collector is only JL-2, the flotation system is one coarse, two fine and one scavenging, the middlings are returned to the previous flotation process, and the reagent system is as follows: the roughing amount of sodium hexametaphosphate is 1000g / t, the collector amount is 700g / t, and the amounts of sodium hexametaphosphate in the two stages of fine selection are 650g / t and 450g / t, respectively; the scavenging amount of sodium hexametaphosphate is 500g / t, the collector amount is 400g / t, and the stirring time is 5min.

[0079]

[0080] Table 4 Flotation data of china clay type lepidolite

[0081] As can be seen from Table 2 and Table 4, compared with the conventional one-rough two-fine one-sweep flotation process, the process of the present invention has a better product quality. For low-grade (Li2O wt.% <0.5%) or high-mud (demuding amount ≈ 20%) lithium mica ores, a recovery rate of more than 85% can be achieved, and the enrichment ratio exceeds 6.5. Comparing the recovery of lithium concentrates 1 and 2 in the table with Examples 1 and 2, it can be seen that the grade of the concentrate product of lithium concentrate 1 is close to that of the corresponding comparative example 1, but the grade of lithium concentrate 2 is higher than that of comparative example 2, and the total yield is higher than the yield of a single reagent, showing the synergistic effect between the reagents, indicating that the present method can effectively improve the recovery of lithium mica.

[0082] In summary, the desludging step can be omitted when flotation of lepidolite using the method of the present invention, and no pH adjuster needs to be added during flotation. For low-grade, high-mud lepidolite ore, the total recovery rate of Li2O in the flotation concentrate exceeds 85%. This effectively avoids the challenges of Li2O loss that may result from traditional flotation processes, safety and environmental issues in strongly acidic environments, as well as complex reagent systems, high costs, and difficult tailings treatment. The method is green and environmentally friendly, achieves efficient recovery of lepidolite from neutral flotation pulp, and demonstrates its value and potential in practical applications.

[0083] The above description is only a preferred embodiment of the present invention and does not limit the patent scope of the present invention. All equivalent structural transformations made by using the contents of the present invention description and drawings under the concept of the present invention, or direct / indirect application in other related technical fields are included in the patent protection scope of the present invention.

Claims

1. A floatable separation process for mud-containing lepidolite, characterized in that: The iso-floatable separation process of mud-containing lepidolite comprises: S1, mixing the raw ore with sodium hexametaphosphate and then finely grinding it through a mill; S2. Add collector JL-1 to the grinding product for isoflotation to obtain foam product and pulp product; S3, the foam product in step S2 is subjected to two-stage selection with sodium hexametaphosphate as an inhibitor to obtain lithium concentrate 1, the selected tailings are scavenged with JL-1 as a collector and sodium hexametaphosphate as an inhibitor, the scavenged foam product is returned to the first stage of selection, and the remaining product forms the tailings; S4, the pulp product in step S2 is subjected to a one-coarse two-fine two-sweep flotation process using JL-2 as a collector and sodium hexametaphosphate as a depressant to obtain lithium concentrate and tailings. The tailings and the tailings from step S3 together form the final tailings, and the middlings at all levels are returned to the previous flotation process; The JL-1 comprises dodecylamine, sodium oleate, sodium laurylsulfonate, dodecylamine polyoxyethylene ether and tributyl phosphate; The JL-2 comprises dodecylamine, sodium linoleate, sodium laurylsulfonate, octadecylamine polyoxyethylene ether and polyethylene glycol.

2. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: The raw ore is lepidolite, the grade of Li2O in the raw ore is between 0.2% and 1.2%, and the mass proportion of -325 mesh minerals in the raw ore is between 5% and 35%.

3. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: In steps S2, S3 and S4, the pH range of the slurry is controlled to be 6-8.

4. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: In step S1, the amount of sodium hexametaphosphate used is 200 g / t-1000 g / t.

5. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: In step S2, the amount of JL-1 used is 300 g / t to 800 g / t.

6. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: In step S3, the amount of sodium hexametaphosphate used is 200g / t-500g / t, and the amount of collector JL-1 used is 100g / t-300g / t.

7. The iso-floatable separation process of muddy lepidolite according to claim 1, characterized in that: In step S4, the amount of sodium hexametaphosphate used in the roughing process is 100g / t-500g / t, and the amount of collector JL-2 used is 200g / t-600g / t; the amount of sodium hexametaphosphate used in the cleaning process is 200g / t-500g / t; The dosage of sodium hexametaphosphate in the scavenging process is 100g / t-300g / t, and the dosage of collector JL-2 is 100g / t-300g / t.

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