A method for the separation of spodumene from gangue minerals by reverse flotation

Abstract

This invention discloses a reverse flotation method for separating spodumene from gangue minerals. The method includes the following steps: grinding spodumene-containing minerals in a ball mill until the particle size is -0.074 mm and the content is 85%; adjusting the slurry mass percentage concentration to 45%; introducing the slurry into a stirred tank for conditioning; adding 300g of spodumene inhibitor YLI per ton of slurry at the inlet of the stirred tank, followed by adding 700g of collector BGU per ton of slurry to obtain the conditioned slurry. The conditioned slurry is then subjected to rapid flotation separation using an aerated flotation machine. The selected froth product consists of gangue minerals such as feldspar and quartz, while the product at the bottom of the flotation tank is spodumene. This invention achieves effective flotation separation of spodumene and gangue minerals, reducing the gangue content in spodumene.

Description

Technical Field

[0001] This invention relates to the field of mineral separation and beneficiation technology, and in particular to a method for separating spodumene and gangue minerals by reverse flotation. Background Technology

[0002] With the booming development of the new energy industry, the efficient recovery technology of lithium oxide from lithium-bearing ores has become a key focus. Spodumene is the most important industrial source of lithium, and its applications in ceramics, metallurgy, porcelain making, special glass, and chemicals are rapidly developing and expanding. Flotation is the most effective method for obtaining high-quality spodumene concentrate. Industrial applications of spodumene existed abroad as early as the 1930s, while research on spodumene flotation in my country began in the 1950s. Currently, industrial spodumene flotation processes include both direct flotation and reverse flotation, depending on the ore properties. Reverse flotation typically uses starch, dextrin, etc., to suppress spodumene, while cationic collectors float silicate gangue minerals such as quartz, feldspar, and mica under alkaline conditions, enriching spodumene in the flotation cell to obtain spodumene concentrate. However, these conventional depressants not only suppress spodumene but also have a certain inhibitory effect on gangue minerals during flotation. For this type of difficult-to-process ore, it is necessary to continuously optimize the beneficiation reagents and processes to improve the beneficiation indicators and ensure the maximum utilization rate of lithium oxide ore resources. Summary of the Invention

[0003] To address the technical problems existing in the background art, this invention proposes a reverse flotation method for separating spodumene from gangue minerals.

[0004] The present invention proposes a method for separating spodumene and gangue minerals by reverse flotation, characterized by comprising the following steps:

[0005] Lithium-containing spodumene minerals are ground in a ball mill to obtain a slurry;

[0006] The slurry is introduced into a mixing tank and then treated with chemicals to adjust the slurry.

[0007] Sodium tripolyphosphate was added at the inlet of the mixing tank as a slurry conditioner, and 300 g / t of YLI inhibitor was prepared by using acetic acid in combination with pregelatinized starch and cyclomaltheptaose.

[0008] Polyoxyethyleneamine, cycloalkanamine and maleate were used to prepare the collector BGU 700g / t;

[0009] Adding the collector BGU to the YLI inhibitor yields a slurry.

[0010] The prepared slurry is fed into a flotation machine for rapid flotation separation. The flotation foam product is gangue minerals such as feldspar and quartz, while the product at the bottom of the flotation tank is spodumene.

[0011] Preferably, the preparation method of YLI inhibitor is as follows: acetic acid solution with a mass fraction of 8% is prepared by mixing acetic acid and water; sodium tripolyphosphate is then added to the acetic acid solution to obtain a first solution, wherein the concentration of sodium tripolyphosphate in the acetic acid solution in the first solution is 30-70 g / L; pregelatinized starch and cyclomaltheptaose in a mass ratio of 1:1 are then weighed and added to the first solution and stirred evenly to obtain a viscous substance, wherein the content of sodium tripolyphosphate in the pregelatinized starch and cyclomaltheptaose in the viscous substance is 30-70 mg / g; the evenly stirred viscous substance is placed in a constant temperature drying oven for drying, and after grinding, spodumene YLI inhibitor is obtained.

[0012] Preferably, the temperature of the constant temperature drying oven is set to 60°C.

[0013] Preferably, the preparation method of collector BGU is as follows: weigh 100g of raw material polyoxyethylene amine, add 100mL of water, mix and heat to 80℃, stir for 1 hour, this is component a. Under the condition of 50℃~60℃, add 50g each of cycloalkanamine and maleate to 100mL of water, stir for 2 hours, this is component b. After mixing component a and component b, add 10g of water glass and stir. After stirring evenly, BGU flotation collector is obtained.

[0014] Preferably, sodium carbonate is used to adjust the pH of the pulp to 8 during flotation.

[0015] Preferably, the grinding process requires a particle size of -0.074 mm to account for 85%, and the slurry mass percentage concentration to be adjusted to 45%.

[0016] Preferably, the ball mill is model XMQΦ240*90.

[0017] Preferably, the flotation machine is an XFG type aerated flotation machine.

[0018] The present invention proposes a method for separating spodumene and gangue minerals via reverse flotation, which has the following advantages:

[0019] 1. The prepared YLI inhibitor is stable in nature. When combined with grinding, pulping and dosing, and aeration flotation processes, it can effectively separate spodumene from gangue minerals during reverse flotation of spodumene.

[0020] 2. The amount of YLI inhibitor used in the process is small, and it has almost no inhibitory effect on gangue minerals, which can effectively improve the grade of spodumene.

[0021] 3. The prepared collector BGU is stable and, when combined with grinding, pulping, reagent addition, and aeration flotation processes, can effectively selectively float feldspar and quartz.

[0022] 4. The amount of collector BGU used in the process is small, and the use of YLI inhibitor will not have a significant collecting effect on spodumene. It can effectively separate spodumene from gangue minerals in the reverse flotation of spodumene.

[0023] Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. Detailed Implementation

[0024] The embodiments of the present invention are described in detail below:

[0025] Example 1

[0026] An example of a reverse flotation method for separating spodumene and gangue minerals according to the present invention includes the following steps: Spodumene-containing minerals are ground in a ball mill until the particle size is -0.074 mm and the content is 85%. The mass percentage concentration of the slurry is adjusted to 45%. The slurry is then introduced into a stirred tank for reagent preparation. At the inlet of the stirred tank, 300g of spodumene inhibitor YLI is added per ton of slurry, followed by 700g of collector BGU per ton of slurry, to obtain the prepared slurry. The prepared slurry is then introduced into an aerated flotation machine for rapid flotation separation. The preparation method of YLI inhibitor is as follows: acetic acid solution with a mass fraction of 8% is prepared by mixing acetic acid and water. Sodium tripolyphosphate is then added to the acetic acid solution to obtain a first solution with a sodium tripolyphosphate concentration of 30 g / L. Pregelatinized starch and cyclomaltheptaose in a mass ratio of 1:1 are then weighed and added to the first solution and stirred evenly to obtain a viscous substance. The sodium tripolyphosphate content in the viscous substance is 30 mg / g in the pregelatinized starch and cyclomaltheptaose. The evenly stirred viscous substance is placed in a constant temperature drying oven set at 60℃ and dried. After grinding, the spodumene YLI inhibitor is obtained. The preparation method of collector BGU is as follows: Weigh 100g of raw material polyoxyethylene amine, add 100mL of water, mix and heat to 80℃, stir for 1 hour, this is component a. Under the condition of 50℃~60℃, add 50g each of cycloalkanamine and maleate to 100mL of water, stir for 2 hours, this is component b. After mixing components a and b, add 10g of water glass and stir. After stirring evenly, BGU flotation collector is obtained.

[0027] Example 2

[0028] This embodiment is an application example of embodiment 1.

[0029] 1. Mineral Raw Materials: The mineral raw materials used are ore containing spodumene and gangue minerals. The raw ore has a Li₂O grade of 0.42%, which is the main target mineral to be recovered. It mainly exists as an independent mineral in spodumene, with a small amount occurring as isomorphous inclusions in feldspar, biotite, chlorite, and muscovite. Other minerals are present as fine-grained inclusions. SiO₂ is the main gangue mineral, accounting for 66.15%, mainly existing in the form of quartz. The remaining gangue minerals are plagioclase, potassium feldspar, muscovite, etc.

[0030] 2. Reagent formulation and operating conditions: The pH of the pulp was adjusted to 8 using sodium carbonate. The dosage of YLI inhibitor prepared in Example 1 was 300 g / t, and the dosage of collector BGU was 700 g / t. The results showed that the above reagent conditions could effectively inhibit spodumene and separate it from gangue minerals by flotation. After one roughing, three cleaning and two scavenging processes (the dosage of reagents was halved in each cleaning process), and the middlings were returned step by step, a flotation concentrate with a lithium oxide grade of 3.51% and a recovery rate of 72.55% was obtained.

[0031] Example 3

[0032] An example of the reverse flotation method for separating spodumene and gangue minerals according to the present invention includes the following steps:

[0033] The spodumene-containing minerals were ground in a ball mill until the particle size was -0.074 mm and the content was 85%. The mass percentage concentration of the slurry was adjusted to 45%. The slurry was then introduced into a stirred tank for reagent preparation. At the inlet of the stirred tank, 300 g of spodumene inhibitor YLI and 700 g of collector BGU were added per ton of slurry, respectively, to obtain the prepared slurry. The prepared slurry was then introduced into an aerated flotation machine for rapid flotation separation. The preparation method of the FLI inhibitor is as follows: acetic acid solution with a mass fraction of 8% is prepared by mixing acetic acid and water. Sodium tripolyphosphate is then added to the acetic acid solution to obtain a first solution with a sodium tripolyphosphate concentration of 50 g / L in the acetic acid solution. Pregelatinized starch and cyclomaltheptaose in a mass ratio of 1:1 are then weighed and added to the first solution and stirred evenly to obtain a viscous substance. The content of sodium tripolyphosphate in the pregelatinized starch and cyclomaltheptaose in the viscous substance is 50 mg / g. The evenly stirred viscous substance is placed in a constant temperature drying oven set at 60℃ and dried. After grinding, the spodumene YLI inhibitor is obtained. The preparation method of collector BGU is as follows: Weigh 100g of raw material polyoxyethylene amine, add 100mL of water, mix and heat to 80℃, stir for 1 hour, this is component a. Under the condition of 50℃~60℃, add 50g each of cycloalkanamine and maleate to 100mL of water, stir for 2 hours, this is component b. After mixing components a and b, add 10g of water glass and stir. After stirring evenly, BGU flotation collector is obtained.

[0034] Example 4

[0035] This embodiment is an application example of embodiment 3.

[0036] 1. Mineral Raw Materials: The mineral raw materials used are ore containing spodumene and gangue minerals. The raw ore has a Li₂O grade of 0.42%, which is the main target mineral to be recovered. It mainly exists as an independent mineral in spodumene, with a small amount occurring as isomorphous inclusions in feldspar, biotite, chlorite, and muscovite. Other minerals are present as fine-grained inclusions. SiO₂ is the main gangue mineral, accounting for 66.15%, mainly existing in the form of quartz. The remaining gangue minerals are plagioclase, potassium feldspar, muscovite, etc.

[0037] 2. Reagent formulation and operating conditions: The pH of the pulp was adjusted to 8 using sodium carbonate. The dosage of YLI inhibitor prepared in Example 3 was 300 g / t, and the dosage of collector BGU was 700 g / t. The results showed that the above reagent conditions could effectively inhibit spodumene and separate it from gangue minerals by flotation. After one roughing, three cleaning, and two scavenging processes (the reagent dosage was halved in each cleaning process), and the middlings were returned step by step, a flotation concentrate with a lithium oxide grade of 3.63% and a recovery rate of 73.85% was obtained.

[0038] Example 5

[0039] An example of the reverse flotation method for separating spodumene and gangue minerals according to the present invention includes the following steps:

[0040] The spodumene-containing minerals were ground in a ball mill until the particle size was -0.074 mm and the content was 85%. The mass percentage concentration of the slurry was adjusted to 45%. The slurry was then introduced into a stirred tank for reagent preparation. At the inlet of the stirred tank, 300 g of spodumene inhibitor YLI and 700 g of collector BGU were added per ton of slurry, respectively, to obtain the prepared slurry. The prepared slurry was then introduced into an aerated flotation machine for rapid flotation separation. The preparation method of YLI inhibitor is as follows: acetic acid solution with a mass fraction of 8% is prepared by mixing acetic acid and water. Sodium tripolyphosphate is then added to the acetic acid solution to obtain a first solution with a sodium tripolyphosphate concentration of 70 g / L in the acetic acid solution. Pregelatinized starch and cyclomaltheptaose in a mass ratio of 1:1 are then weighed and added to the first solution and stirred evenly to obtain a viscous substance. The content of sodium tripolyphosphate in the pregelatinized starch and cyclomaltheptaose in the viscous substance is 70 mg / g. The evenly stirred viscous substance is placed in a constant temperature drying oven set at 60℃ and dried. After grinding, the spodumene YLI inhibitor is obtained. The preparation method of collector BGU is as follows: Weigh 100g of raw material polyoxyethylene amine, add 100mL of water, mix and heat to 80℃, stir for 1 hour, this is component a. Under the condition of 50℃~60℃, add 50g each of cycloalkanamine and maleate to 100mL of water, stir for 2 hours, this is component b. After mixing components a and b, add 10g of water glass and stir. After stirring evenly, BGU flotation collector is obtained.

[0041] Example 6

[0042] This embodiment is an application example of embodiment 5.

[0043] 1. Mineral Raw Materials: The mineral raw materials used are ore containing spodumene and gangue minerals. The raw ore has a Li₂O grade of 0.42%, which is the main target mineral to be recovered. It mainly exists as an independent mineral in spodumene, with a small amount occurring as isomorphous inclusions in feldspar, biotite, chlorite, and muscovite. Other minerals are present as fine-grained inclusions. SiO₂ is the main gangue mineral, accounting for 66.15%, mainly existing in the form of quartz. The remaining gangue minerals are plagioclase, potassium feldspar, muscovite, etc.

[0044] 2. Reagent formulation and operating conditions: The pH of the pulp was adjusted to 8 using sodium carbonate. The dosage of YLI inhibitor prepared in Example 5 was 300 g / t, and the dosage of collector BGU was 700 g / t. The results showed that the above reagent conditions could effectively inhibit spodumene and separate it from gangue minerals by flotation. After one roughing, three cleaning, and two scavenging processes (the reagent dosage was halved in each cleaning process), and the middlings were returned step by step, a flotation concentrate with a lithium oxide grade of 3.69% and a recovery rate of 73.32% was obtained.

[0045] It should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" are used only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention.

[0046] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this invention, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0047] In this invention, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection, an electrical connection, or a connection that allows communication between them; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0048] In this invention, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "over," and "on top" of the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0049] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A method for the separation of spodumene from gangue minerals by reverse flotation, characterized in that, Includes the following steps: Lithium-containing spodumene minerals are ground in a ball mill to obtain a slurry; The slurry is introduced into a mixing tank and then treated with chemicals to adjust the slurry. Sodium tripolyphosphate was added at the inlet of the mixing tank as a slurry conditioner, and 300 g / t of YLI inhibitor was prepared by using acetic acid in combination with pregelatinized starch and cyclomaltheptaose. A collector BGU 700g / t was prepared by mixing polyoxyethyleneamine, cycloalkanamine and maleate. Adding the collector BGU to the YLI inhibitor yields a slurry. The prepared slurry is fed into a flotation machine for rapid flotation separation. The flotation foam product is feldspar and quartz vein minerals, while the product at the bottom of the flotation tank is spodumene.

2. A method of reverse flotation separation of spodumene from gangue minerals according to claim 1, characterised in that, The preparation method of YLI inhibitor is as follows: An 8% acetic acid solution is prepared by mixing acetic acid and water. Sodium tripolyphosphate is then added to the acetic acid solution to obtain a first solution, in which the concentration of sodium tripolyphosphate in the acetic acid solution is 30-70 g / L. Pregelatinized starch and cyclomaltheptaose in a 1:1 mass ratio are then weighed and added to the first solution, and stirred until homogeneous to obtain a viscous substance. The content of sodium tripolyphosphate in the pregelatinized starch and cyclomaltheptaose in the viscous substance is 30-70 mg / g. The homogeneous viscous substance is placed in a constant temperature drying oven for drying, and after grinding, the spodumene YLI inhibitor is obtained.

3. A method of reverse flotation separation of spodumene from gangue minerals according to claim 2, characterised in that: The temperature of the constant temperature drying oven is set to 60°C.

4. The method for separating spodumene and gangue minerals by reverse flotation according to claim 1, characterized in that, The preparation method of collector BGU is as follows: Weigh 100g of raw material polyoxyethylene amine, add 100mL of water, mix and heat to 80℃, stir for 1 hour, this is component a. Under the condition of 50℃~60℃, add 50g each of cycloalkanamine and maleate to 100mL of water, stir for 2 hours, this is component b. After mixing components a and b, add 10g of water glass and stir. After stirring evenly, BGU flotation collector is obtained.

5. The method for separating spodumene and gangue minerals by reverse flotation according to claim 1, characterized in that, Sodium carbonate is used to adjust the pH of the pulp to 8 during flotation.

6. The method for separating spodumene and gangue minerals by reverse flotation according to claim 1, characterized in that, The grinding process requires a particle size of -0.074mm and a content of 85%, with the slurry concentration adjusted to 45% by mass percentage.

7. The method for separating spodumene and gangue minerals by reverse flotation according to claim 1, characterized in that, The ball mill model is XMQΦ240*90.

8. The method for separating spodumene and gangue minerals by reverse flotation according to claim 1, characterized in that, The flotation machine is an XFG type aerated flotation machine.