Method of pulverizing molybdenum disulfide using dispersant and method of preparing high grade molybdenum disulfide from low grade molybdenite concentrate using the same

Abstract

The present invention provides a method for finely grinding molybdenum disulfide using tannic acid as a dispersant and wet grinding using an attrition mill, and a method for producing high-quality molybdenum disulfide products from molybdenum concentrate using the same.

Description

Technology Field

[0001] The present invention relates to a method for finely grinding molybdenum disulfide using a dispersant and a method for producing high-quality molybdenum disulfide products from molybdenum concentrate using the same. More specifically, the invention relates to a method for finely grinding molybdenum disulfide using tannic acid as a dispersant and wet grinding using an attrition mill, and a method for producing high-quality molybdenum disulfide products from molybdenum concentrate using the same. Background Technology

[0002] Molybdenum disulfide (MoS2) is utilized in various industrial fields, such as lubricants, energy storage materials, and catalysts, due to its excellent lubricating properties and electrical and chemical stability; for these applications, high-quality molybdenum disulfide in the form of fine powder with controlled particle size is required.

[0003] Currently, the fine grinding of molybdenum disulfide is primarily carried out through time-consuming processes using ball mills or complex multi-stage processes utilizing organic solvents. However, conventional grinding methods suffer from long grinding times, high energy consumption, and environmental burdens associated with the use of organic solvents. Furthermore, as molybdenum disulfide is a mineral with a highly hydrophobic layered structure, particle aggregation occurs easily during the fine grinding process, leading to a decrease in grinding efficiency.

[0004] Some prior art attempts to improve the dispersibility of molybdenum disulfide by using organic solvents as dispersion media or applying organic dispersants such as aniline oligomer derivatives, and mineral grinding techniques that induce inter-particle dispersion using inorganic dispersants such as sodium silicate are also known. However, these methods have problems such as complex processes, the need for expensive dispersants, or the inability to provide sufficient dispersion effects for layered minerals with strong hydrophobicity, such as molybdenum disulfide.

[0005] To improve the fine grinding efficiency of molybdenum disulfide, a hydrophobic mineral, it is important to enhance the dispersibility of mineral particles during the grinding process and effectively suppress particle aggregation. When dispersibility is improved, the probability of collision between the grinding medium and molybdenum disulfide particles increases, which can lead to improved grinding efficiency. However, conventional technologies face limitations, such as relying on organic solvents or expensive organic dispersants, or using inorganic dispersants that have limited dispersion effects on hydrophobic minerals.

[0006] Therefore, there is a need to develop a fine grinding technology for molybdenum disulfide that is simple in process and highly efficient by utilizing an environmentally friendly dispersant suitable for the surface characteristics of molybdenum disulfide having a hydrophobic layered structure. Prior art literature

[0007] Chinese Published Patent No. 001724594 Chinese Registered Patent Publication No. 107365259 The problem to be solved

[0008] The present invention aims to provide a method for finely grinding molybdenum disulfide using a dispersant that improves grinding efficiency and achieves particle size reduction by enabling additional grinding beyond the existing grinding limit during wet grinding using an attrition mill by introducing tannic acid, which is environmentally friendly and suitable for the surface characteristics of molybdenum disulfide, as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility, and a method for manufacturing high-quality molybdenum disulfide products from molybdenum concentrate using the same.

[0009] The problems that the present invention aims to solve are not limited to those mentioned above, and other unmentioned problems will be clearly understood by those skilled in the art from the description below. means of solving the problem

[0010] To achieve the above objective, according to one aspect of the present invention, a method for finely grinding molybdenum disulfide using a dispersant is,

[0011] (a-1) Step of preparing molybdenum concentrate containing MoS2;

[0012] (a-2) a step of adding the above-mentioned molybdenum concentrate containing MoS2 to water to form a slurry, and adding a dispersant to prepare a slurry; and

[0013] (a-3) A step of feeding the above slurry into a grinder and rotating an internal stirrer to wet grind it; is included.

[0014] In addition, the dispersant in step (a-2) above is characterized as being tannin acid.

[0015] In addition, the above step (a-2) is characterized by including the step of adding the dispersant at a rate of 250 g / ton or more and 500 g / ton or less, and mixing for a stirring time of 10 minutes.

[0016] In addition, in step (a-3) above, the grinder is an attrition mill, and

[0017] It is characterized by including the step of filling the above-mentioned attrition mill with steel balls.

[0018] In addition, the above step (a-3) is characterized by wet grinding by rotating the internal stirrer at 300 rpm or more.

[0019] In addition, after step (a-3) above, the particle size (D) of the molybdenum concentrate containing MoS2 50 ) is characterized by being 30 μm or less.

[0020] To achieve the above objective, according to another aspect of the present invention, a method for producing a high-grade molybdenum disulfide product from molybdenum concentrate is,

[0021] (b-1) A step of preparing molybdenum concentrate having a MoS2 content of 85 wt% or less;

[0022] (b-2) A step of forming a first slurry by adding the molybdenum concentrate having a MoS2 content of 85 wt% or less to water, and preparing a slurry by adding a dispersant;

[0023] (b-3) a step of feeding the above slurry into a grinder and rotating an internal stirrer to wet grind it; and

[0024] (b-4) A step of flotation separating the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less; is included.

[0025] In addition, in step (b-2) above, the concentration of the first slurry is 50 wt%, and

[0026] The above-mentioned dispersant is characterized as being tannin acid.

[0027] In addition, in step (b-3) above, the grinder is an attrition mill, and

[0028] It is characterized by including the step of filling the above-mentioned attrition mill with steel balls.

[0029] In addition, the particle size (D) of the wet-milled molybdenum concentrate having a MoS2 content of 85 wt% or less in step (b-4) above 50 ) is characterized by being 30 μm or less.

[0030] In addition, the above step (b-4) is characterized by including the step of forming a second slurry by adding the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less to water, and conditioning the second slurry by adding a flotation reagent.

[0031] In addition, the concentration of the second slurry is characterized as being 10 to 20 wt%.

[0032] In addition, the conditioning step is characterized by including a step of mixing 200 g / ton of coagulant (Kerosene) with a stirring time of 5 minutes.

[0033] In addition, the conditioning step is characterized by including a step of mixing 100 g / ton of foaming agent (AF65) with a stirring time of 5 minutes.

[0034] In addition, the above step (b-4) is characterized by being performed by setting the floating separation time to 5 minutes.

[0035] In addition, the molybdenum disulfide product obtained after step (b-4) above is characterized by having a grade of 98% or higher. Effects of the invention

[0036] According to the present invention, a method for finely grinding molybdenum disulfide using a dispersant is provided, in which an environmentally friendly tannic acid suitable for the surface characteristics of molybdenum disulfide is introduced as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility, thereby enabling additional grinding beyond the existing grinding limit during wet grinding using an attrition mill, and a method for manufacturing a high-quality molybdenum disulfide product from molybdenum concentrate using the same is provided.

[0037] The effects of the present invention are not limited to the effects described above, and should be understood to include all effects that can be inferred from the configuration of the invention described in the detailed description of the invention or the claims. Brief explanation of the drawing

[0038] FIG. 1 is a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention and a process diagram for producing a high-quality molybdenum disulfide product from molybdenum concentrate using the same. FIG. 2 is a schematic diagram of the interaction between tannic acid and MoS2 in a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention. Specific details for implementing the invention

[0039] Before describing the present invention in detail, it should be understood that the terms and words used in this specification should not be interpreted as being limited to their ordinary or dictionary meanings, and that the inventor of the present invention may appropriately define and use the concepts of various terms to best describe their invention, and furthermore, that these terms and words should be interpreted in a meaning and concept consistent with the technical spirit of the present invention.

[0040] In other words, it should be understood that the terms used in this specification are used merely to describe preferred embodiments of the present invention and are not intended to specifically limit the content of the present invention, and that these terms are defined in consideration of the various possibilities of the present invention.

[0041] In addition, it should be noted that in this specification, singular expressions may include plural expressions unless the context clearly indicates a different meaning, and that even if they are expressed in a similarly plural form, they may include the meaning of the singular.

[0042] Throughout this specification, where it is stated that a component "includes" another component, unless specifically stated otherwise, this may mean that it does not exclude any other component but may include any other component.

[0043] In addition, in the following description of the present invention, detailed descriptions of components that are deemed to unnecessarily obscure the essence of the present invention, such as known technologies including prior art, may be omitted.

[0045] The present invention will be described in detail below with reference to the drawings.

[0046] Method for finely grinding molybdenum disulfide using a dispersant

[0047] FIG. 1 is a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention and a process diagram for producing a high-quality molybdenum disulfide product from molybdenum concentrate using the same.

[0048] As illustrated in FIG. 1, a method for finely grinding molybdenum disulfide using a dispersant comprises: (a-1) a step of preparing a molybdenum concentrate containing MoS2; (a-2) a step of forming a slurry by adding the molybdenum concentrate containing MoS2 to water and preparing a slurry by adding a dispersant; and (a-3) a step of wet grinding by adding the slurry to a grinder and rotating an internal stirrer.

[0049] The present invention has the effect of improving grinding efficiency and achieving a reduction in particle size by introducing tannic acid, which is suitable for the surface characteristics of molybdenum disulfide and is environmentally friendly, as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility, thereby enabling additional grinding beyond the existing grinding limit when wet grinding using an attrition mill.

[0050] Step (a-1) is the step of preparing molybdenum concentrate containing MoS2.

[0051] The molybdenum concentrate containing MoS2 is not particularly limited in type, and is not limited to any molybdenum concentrate containing MoS2 to which the fine grinding method of molybdenum disulfide using the dispersant of the present invention can be applied, and a non-limiting example thereof may be a molybdenum concentrate having a MoS2 content of 85 wt% or less.

[0052] (a-2) Step is a step of forming a slurry by adding the molybdenum concentrate containing MoS2 to water and preparing a slurry by adding a dispersant.

[0053] To improve the fine grinding efficiency of molybdenum disulfide (MoS2), a hydrophobic mineral, it is important to increase the dispersibility of mineral particles during the wet grinding process and effectively suppress aggregation between particles. When particle dispersibility is improved, the probability of collision between the grinding medium and molybdenum disulfide particles increases, allowing for efficient transfer of grinding energy and thereby improving grinding efficiency.

[0054] In step (a-2) above, the dispersant may be tannin acid.

[0055] In the prior art, the dispersibility of molybdenum disulfide was improved by using organic solvents as dispersion media or applying organic dispersants such as aniline oligomer derivatives, or inducing inter-particle dispersion using inorganic dispersants such as sodium silicate. However, these methods have problems in that the process is complex and they do not provide a sufficient dispersion effect for molybdenum disulfide, which is a layered mineral with a strong hydrophobic structure.

[0056] To solve these problems, according to the fine grinding method of molybdenum disulfide using a dispersant of the present invention, by using environmentally friendly tannic acid, which is suitable for the surface characteristics of molybdenum disulfide while suppressing particle aggregation during the grinding process and enhancing dispersibility, it is possible to achieve additional grinding beyond the existing grinding limits, thereby improving particle grinding efficiency and reducing particle size.

[0057] FIG. 2 is a schematic diagram of the interaction between tannic acid and MoS2 in a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention.

[0058] As shown in Fig. 2, tannin acid is a natural polymeric material derived from plants that contains multiple aromatic rings and phenolic hydroxyl groups (-OH). Due to these structural characteristics, it is adsorbed onto the basal plane of molybdenum disulfide through π-π interactions and van der Waals forces, and can form hydrogen bonds at defect sites. Tannin acid, which exhibits adsorption behavior suitable for the surface characteristics of molybdenum disulfide, inhibits inter-particle aggregation and restacking and improves dispersion stability by inducing steric hindrance due to its bulky molecular structure.

[0059] The above step (a-2) may include the step of adding the dispersant at a rate of 250 g / ton or more and 500 g / ton or less, and mixing for a stirring time of 10 minutes, and preferably, the dispersant may be added at a rate of 500 g / ton.

[0060] Here, when the above-mentioned dispersant is introduced within the above range, the hydrophobic surface of the molybdenum disulfide particles in the slurry is modified to be hydrophilic to improve dispersibility, thereby suppressing particle aggregation and restacking phenomena in the subsequent wet grinding step, and thus enabling additional grinding beyond the existing grinding limit, thereby significantly improving fine grinding efficiency and achieving particle size reduction.

[0061] If the above dispersant is added in an amount of 750 g / ton or more, the slurry viscosity increases due to the excessive addition and an intermolecular crosslinking effect occurs, which reduces the fine grinding efficiency during the subsequent wet grinding step.

[0062] (a-3) Step is the step of feeding the above slurry into a grinder and rotating an internal stirrer to wet grind it.

[0063] In step (a-3) above, the grinder is an attrition mill, and

[0064] The method may include a step of filling the above-mentioned attrition mill with steel balls.

[0065] An attrition mill is a wet grinding device that induces high-speed relative motion between the grinding medium and the material to be ground by the rotation of a stirring shaft or impeller inside a grinding tank filled with grinding medium, and finely grinds particles by shear force and friction force.

[0066] Unlike rotary ball mills, which primarily utilize impact force as the grinding medium falls with the rotation of the drum, attrition mills have a grinding mechanism in which shear stress acting along the particle surface is dominant as the grinding medium moves by rubbing against each other through stirring, and due to these characteristics, fine grinding and wet grinding processes are suitable.

[0067] Here, when wet grinding is performed using an attrition mill with the grinder, shear force and frictional force are mainly applied to the molybdenum disulfide particles, which is advantageous for inducing interlayer delamination along the layered structure of the molybdenum disulfide particles, and can suppress aggregation between fine particles that occurs during the fine grinding process. Additionally, the high frequency of contact between the grinding medium and the slurry allows for efficient transfer of grinding energy, and through the preceding step, tannic acid is adsorbed onto the surface of the molybdenum disulfide particles, thereby maintaining stable dispersibility. This enables additional grinding beyond the existing grinding limit, thereby improving grinding efficiency and achieving a reduction in particle size.

[0068] Meanwhile, since zirconia balls have low density and a chemically inert surface, the grinding efficiency may be limited when finely grinding molybdenum disulfide, a hydrophobic mineral. However, the steel balls used in the present invention have a higher density than zirconia balls, so the kinetic energy transferred per grinding medium is large, and in particular, the shear force and frictional force generated by the stirring motion of the attrition mill can be further amplified. In addition, the surface of the steel balls is rough and allows for hydrophilic interactions, which can further increase contact and friction with molybdenum disulfide particles.

[0069] Here, when the above steel balls are filled, exfoliation is promoted along the layered structure of molybdenum disulfide, and the particle size reduction efficiency can be improved for the same grinding time. Additionally, by combining with an attrition mill, the fine grinding mechanism centered on shear and friction is reinforced, enabling additional grinding beyond the existing grinding limit, thereby improving grinding efficiency and achieving particle size reduction.

[0070] The above step (a-3) may involve wet grinding by rotating the internal stirrer at 300 rpm or more.

[0071] Here, when wet grinding is performed by rotating the internal stirrer within the rotational speed range, the tannic acid is adsorbed onto the surface of the molybdenum disulfide particles through the preceding step, and the dispersibility is stably maintained, thereby enabling additional grinding beyond the existing grinding limit, which improves grinding efficiency and achieves a reduction in particle size.

[0072] After step (a-3) above, the particle size (D) of the molybdenum concentrate containing MoS2 above 50 ) can be 30 μm or less.

[0073] Here, the particle size (D of the molybdenum concentrate containing MoS2) 50 The value of ) represents a 14.3% improvement in particle size reduction compared to the case where sodium silicate was used as a dispersant in conventional technology.

[0075] Method for manufacturing high-grade molybdenum disulfide products from molybdenum concentrate

[0076] FIG. 1 is a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention and a process diagram for producing a high-quality molybdenum disulfide product from molybdenum concentrate using the same.

[0077] As illustrated in FIG. 1, a method for manufacturing a high-grade molybdenum disulfide product from molybdenum concentrate comprises: (b-1) a step of preparing molybdenum concentrate having a MoS2 content of 85 wt% or less; (b-2) a step of adding the molybdenum concentrate having a MoS2 content of 85 wt% or less to water to form a first slurry and adding a dispersant to prepare a dispersion; (b-3) a step of adding the dispersion to a grinder and rotating an internal stirrer to wet grind; and (b-4) a step of floating the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less.

[0078] The present invention has the effect of improving grinding efficiency and achieving a reduction in particle size by introducing tannic acid, which is suitable for the surface characteristics of molybdenum disulfide and is environmentally friendly, as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility, thereby enabling additional grinding beyond the existing grinding limit when wet grinding using an attrition mill.

[0079] Step (b-1) is the step of preparing molybdenum concentrate with a MoS2 content of 85 wt% or less.

[0080] Molybdenum ore (MoS 20.4% or less) is crushed using a jaw crusher and a cone crusher in sequence. After crushing, a screening process is performed using a 48 to 100 mesh sieve to separate the obtained crushed material into coarse particles and fine particles.

[0081] In the above screen process, particles that do not fall within the above range (meaning particles that do not pass through the 48 to 100 mesh sieve) are fed back into the above cone crusher to perform repeated crushing.

[0082] After the above screen process, fine particles with a size of 150 to 350 μm are first ground using a ball mill, and then the ground material is rotated with water using a spiral classifier so that the coarse particles move to the bottom of the spiral classifier and the fine particles are obtained in a wet state.

[0083] Fine particles obtained by passing through a spiral classifier are secondarily ground using a ball mill, and then a slurry of the ground material mixed with water is fed into the inlet of a wet cyclone (hydrocyclone), and the fine particles are discharged through the upper outlet by centrifugal force.

[0084] Average particle size of fine particles obtained from the wet cyclone process (D 50 The particle size is 20 to 70 μm, and coarse particles having a particle size larger than the above average particle size range are fed back into the ball mill used for secondary grinding to perform repeated grinding.

[0085] The fine particles obtained from the above wet cyclone process are mixed with water to prepare a slurry, and then reagents are added to the slurry and a conditioning process is performed. At this time, each reagent, such as kerosene (a non-polar oil) as a coagulant to aggregate hydrophobic MoS2 particles, AF65 (Aerofroth 65) of the polypropylene system as a foaming agent, and sodium silicate (Na2SiO3) as a dispersant, is added in sequence to provide roughing flotation separation conditions for a certain period of time.

[0086] Here, the amount of kerosene added is 200 g / t to 250 g / t, the amount of AF65 added is 100 g / t to 150 g / t, and the amount of sodium silicate added is 1000 g / t to 1100 g / t.

[0087] Then, through the above-mentioned ship flotation separation, molybdenum concentrate particles are attached to bubbles to recover the concentrate product (floating matter), and the tailings product is subjected to scavenging flotation separation.

[0088] The concentrate product (float) obtained through the above cleaning flotation is subjected to further flotation. The tailings product (precipitate) obtained after the above cleaning flotation is completed has a MoS2 content of 0.01 wt% or less.

[0089] The concentrate obtained through the above ship flotation separation is subjected to cleaning flotation separation to further improve its grade. Through the above cleaning flotation separation, the concentrate (floating matter) is recovered, and the tailings (sediment) is subjected to ship flotation separation again.

[0090] After the above-mentioned flotation separation is completed, molybdenum concentrate is obtained, and the molybdenum concentrate obtained at this time has a MoS2 content of 85 wt% or less.

[0091] Through the process described above, molybdenum concentrate with a MoS2 content of 85 wt% or less is prepared.

[0092] (b-2) Step is a step of forming a first slurry by adding molybdenum concentrate having a MoS2 content of 85 wt% or less to water and preparing a slurry by adding a dispersant.

[0093] To improve the fine grinding efficiency of molybdenum disulfide (MoS2), a hydrophobic mineral, it is important to increase the dispersibility of mineral particles during the wet grinding process and effectively suppress aggregation between particles. When particle dispersibility is improved, the probability of collision between the grinding medium and molybdenum disulfide particles increases, allowing for efficient transfer of grinding energy and thereby improving grinding efficiency.

[0094] In step (b-2) above, the concentration of the first slurry may be 50 wt%, and

[0095] The above dispersant may be tannin acid.

[0096] In the prior art, the dispersibility of molybdenum disulfide was improved by using organic solvents as dispersion media or applying organic dispersants such as aniline oligomer derivatives, or inducing inter-particle dispersion using inorganic dispersants such as sodium silicate. However, these methods have problems in that the process is complex and they do not provide a sufficient dispersion effect for molybdenum disulfide, which is a layered mineral with a strong hydrophobic structure.

[0097] To solve these problems, according to the fine grinding method of molybdenum disulfide using a dispersant of the present invention, by using environmentally friendly tannic acid, which is suitable for the surface characteristics of molybdenum disulfide while suppressing particle aggregation during the grinding process and enhancing dispersibility, it is possible to achieve additional grinding beyond the existing grinding limits, thereby improving particle grinding efficiency and reducing particle size.

[0098] FIG. 2 is a schematic diagram of the interaction between tannic acid and MoS2 in a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention.

[0099] As shown in Fig. 2, tannin acid is a natural polymeric material derived from plants that contains multiple aromatic rings and phenolic hydroxyl groups (-OH). Due to these structural characteristics, it is adsorbed onto the basal plane of molybdenum disulfide through π-π interactions and van der Waals forces, and can form hydrogen bonds at defect sites. Tannin acid, which exhibits adsorption behavior suitable for the surface characteristics of molybdenum disulfide, inhibits inter-particle aggregation and restacking and improves dispersion stability by inducing steric hindrance due to its bulky molecular structure.

[0100] The above step (b-2) may include adding the dispersant at a rate of 250 g / ton or more and 500 g / ton or less, and mixing for a stirring time of 10 minutes, and preferably, 500 g / ton of dispersant may be added.

[0101] Here, when the above-mentioned dispersant is introduced within the above range, the hydrophobic surface of the molybdenum disulfide particles in the slurry is modified to be hydrophilic to improve dispersibility, thereby suppressing particle aggregation and restacking phenomena in the subsequent wet grinding step, and thus enabling additional grinding beyond the existing grinding limit, thereby significantly improving fine grinding efficiency and achieving particle size reduction.

[0102] If the above dispersant is added in an amount of 750 g / ton or more, the slurry viscosity increases due to the excessive addition and an intermolecular crosslinking effect occurs, which reduces the fine grinding efficiency during the subsequent wet grinding step.

[0103] (b-3) Step is the step of feeding the above slurry into a grinder and rotating an internal stirrer to wet grind it.

[0104] In step (b-3) above, the grinder is an attrition mill, and

[0105] The method may include a step of filling the above-mentioned attrition mill with steel balls.

[0106] An attrition mill is a wet grinding device that induces high-speed relative motion between the grinding medium and the material to be ground by the rotation of a stirring shaft or impeller inside a grinding tank filled with grinding medium, and finely grinds particles by shear force and friction force.

[0107] Unlike rotary ball mills, which primarily utilize impact force as the grinding medium falls with the rotation of the drum, attrition mills have a grinding mechanism in which shear stress acting along the particle surface is dominant as the grinding medium moves by rubbing against each other through stirring, and due to these characteristics, fine grinding and wet grinding processes are suitable.

[0108] Here, when wet grinding is performed using an attrition mill with the grinder, shear force and frictional force are mainly applied to the molybdenum disulfide particles, which is advantageous for inducing interlayer delamination along the layered structure of the molybdenum disulfide particles, and can suppress aggregation between fine particles that occurs during the fine grinding process. Additionally, the high frequency of contact between the grinding medium and the slurry allows for efficient transfer of grinding energy, and through the preceding step, tannic acid is adsorbed onto the surface of the molybdenum disulfide particles, thereby maintaining stable dispersibility. This enables additional grinding beyond the existing grinding limit, thereby improving grinding efficiency and achieving a reduction in particle size.

[0109] Meanwhile, since zirconia balls have low density and a chemically inert surface, the grinding efficiency may be limited when finely grinding molybdenum disulfide, a hydrophobic mineral. However, the steel balls used in the present invention have a higher density than zirconia balls, so the kinetic energy transferred per grinding medium is large, and in particular, the shear force and frictional force generated by the stirring motion of the attrition mill can be further amplified. In addition, the surface of the steel balls is rough and allows for hydrophilic interactions, which can further increase contact and friction with molybdenum disulfide particles.

[0110] Here, when the above steel balls are filled, exfoliation is promoted along the layered structure of molybdenum disulfide, and the particle size reduction efficiency can be improved for the same grinding time. Additionally, by combining with an attrition mill, the fine grinding mechanism centered on shear and friction is reinforced, enabling additional grinding beyond the existing grinding limit, thereby improving grinding efficiency and achieving particle size reduction.

[0111] The above step (b-3) may involve wet grinding by rotating the internal stirrer at 300 rpm or more.

[0112] Here, when wet grinding is performed by rotating the internal stirrer within the rotational speed range, the tannic acid is adsorbed onto the surface of the molybdenum disulfide particles through the preceding step, and the dispersibility is stably maintained, thereby enabling additional grinding beyond the existing grinding limit, which improves grinding efficiency and achieves a reduction in particle size.

[0113] (b-4) Step is a step of flotation separation of the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less.

[0114] In step (b-4) above, the particle size (D) of the wet-milled molybdenum concentrate having a MoS2 content of 85 wt% or less 50 ) is characterized by being 30 μm or less.

[0115] The average particle size of mineral particles is an important factor in determining liberation, and this is a significant factor affecting the flotation results.

[0116] Here, the particle size (D) of the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less. 50 When ) is within the above range, the physical bonding of molybdenum disulfide particles with gangue minerals is resolved, thereby improving the degree of separation of the particles, and during the subsequent flotation separation step, the molybdenum disulfide particles are easily selectively attached to bubbles, thereby improving the quality and recovery rate of the molybdenum disulfide product.

[0117] The above step (b-4) includes the step of forming a second slurry by adding the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less to water, and conditioning the second slurry by adding a flotation reagent.

[0118] The conditioning step is a process of adapting the crushed molybdenum concentrate present in the slurry before flotation separation so that it can react well with the reagent.

[0119] The concentration of the second slurry may be 10 to 20 wt%.

[0120] The concentration of the slurry is an important factor affecting the flotation separation results.

[0121] Here, if the concentration of the slurry exceeds 20%, the viscosity of the slurry increases, which may hinder air dispersion and the formation of excellent bubbles, and may reduce the recovery rate of high-quality molybdenum disulfide products.

[0122] The above conditioning step includes a step of mixing 200 g / ton of coagulant (Kerosene) with a stirring time of 5 minutes.

[0123] Coagulants are chemical substances used to form bridges between mineral particles and to gather small particles into one large mass for separation. Kerosene, a non-polar oil and one type of coagulant, increases the interaction of hydrophobic minerals, namely MoS2 particles, allowing them to aggregate more easily. Since aggregation is strengthened with only a small amount of addition, it helps improve flotation separation efficiency and is advantageous for manufacturing high-quality molybdenum disulfide products.

[0124] In addition, if the amount of the above-mentioned coagulant added is less than 200 g / ton, the aggregation of MoS2 particles is reduced, which may decrease the flotation separation efficiency and reduce the recovery rate of high-quality molybdenum disulfide products.

[0125] The above conditioning step includes a step of mixing 100 g / ton of foaming agent (AF65) with a stirring time of 5 minutes.

[0126] Foaming agents are surfactants that adsorb to the liquid-gas interface to lower the surface tension of the liquid, facilitating the generation and dispersion of small bubbles and stably forming foam.

[0127] If the amount of the foaming agent added exceeds 100 g / ton, only the amount of reagent used increases, and the recovery rate of high-quality molybdenum disulfide products may not increase significantly.

[0128] In addition, if the amount of the foaming agent added is less than 100 g / ton, the surfactant action, which lowers the surface tension of the slurry, is not properly performed, so MoS2 particles cannot rise, which may reduce the flotation separation efficiency and may not improve the recovery rate of high-quality molybdenum disulfide products.

[0129] The above step (b-4) can be performed by setting the floating separation time to 5 minutes.

[0130] The molybdenum disulfide product obtained after step (b-4) above is characterized by having a grade of 98% or higher.

[0131] As described above, the fine grinding method of molybdenum disulfide using a dispersant according to one embodiment of the present invention has the effect of improving grinding efficiency and achieving a reduction in particle size by enabling additional grinding beyond the existing grinding limit during wet grinding using an attrition mill by introducing tannic acid, which is suitable for the surface characteristics of molybdenum disulfide and is environmentally friendly, as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility.

[0132] In addition, the method for producing a high-quality molybdenum disulfide product from molybdenum concentrate according to one embodiment of the present invention has the effect of producing a high-quality molybdenum disulfide product with a MoS2 content of 98 wt% or more from molybdenum concentrate with a MoS2 content of 85 wt% or less by using a fine grinding method of molybdenum disulfide using the dispersant of the present invention.

[0133] Hereinafter, a method for finely grinding molybdenum disulfide using a dispersant according to one embodiment of the present invention will be described with reference to the following experimental examples.

[0135] Example 1: Method for finely grinding molybdenum disulfide using a dispersant

[0136] First, molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 250 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0137] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0139] Example 2: Method for finely grinding molybdenum disulfide using a dispersant

[0140] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 250 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0141] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0143] Example 3: Method for finely grinding molybdenum disulfide using a dispersant

[0144] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 500 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0145] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0147] Example 4: Method for finely grinding molybdenum disulfide using a dispersant

[0148] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 500 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0149] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0151] Comparative Example 1

[0152] First, molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 750 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0153] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0155] Comparative Example 2

[0156] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 750 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0157] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0159] Comparative Example 3

[0160] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 1000 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0161] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0163] Comparative Example 4

[0164] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 1000 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0165] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0167] Comparative Example 5

[0168] First, molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, and a slurry was prepared without adding a dispersant.

[0169] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0171] Comparative Example 6

[0172] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, and a slurry was prepared without adding a dispersant.

[0173] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0175] Comparative Example 7

[0176] First, molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 500 g / ton of sodium silicate was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0177] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 16 minutes.

[0179] Comparative Example 8

[0180] Molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a slurry with a concentration of 50 wt%, 500 g / ton of sodium silicate was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0181] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0183] Example 5: Method for manufacturing high-grade molybdenum disulfide products from molybdenum concentrateFirst, molybdenum concentrate with a MoS2 content of 85 wt% or less was prepared by crushing, classifying, and flotation separation of molybdenum ore (MoS2 0.4% or less) as described above. The prepared molybdenum concentrate with a MoS2 content of 85 wt% or less was added to water to form a first slurry with a concentration of 50 wt%, 500 g / ton of tannic acid was added, and the mixture was stirred for 10 minutes to prepare a slurry.

[0184] The slurry was fed into an attrition mill and filled with steel balls to 50% of the internal effective area (media filling rate). Then, the internal stirrer was wet-ground at 300 rpm for 32 minutes.

[0185] Particle size of molybdenum disulfide powder obtained after grinding (D 50 ) was 23.736 μm.

[0186] The crushed material was added to water to prepare a second slurry with a concentration of 20 wt%. Then, 200 g / ton of coagulant (Kerosene) was added and stirred for 5 minutes. Subsequently, 100 g / ton of foaming agent (AF65) was added and stirred for 5 minutes. The final prepared slurry was loaded into a laboratory-scale Denver Sub-A flotation device and flotation was performed for 5 minutes to produce a high-quality molybdenum disulfide product with a MoS2 content of 98 wt% or more.

[0188] Experimental Example 1: Fine grinding results according to dispersant - Particle size (D 50 ) analyze

[0189] The pulverized materials obtained after wet grinding in Examples 1 to 4 and Comparative Examples 1 to 8 were subjected to particle size analysis using a laser diffraction-based particle size analyzer. The analysis results are as shown in [Table 1] below.

[0190] hour Dispersant injection X Sodium Silicate dosage Tannin acid input amount 500 g / ton 250 g / ton 500 g / ton 750 g / ton 1000 g / ton Particle size (D 50 ) : Unit μm 1 min 60.726 57.01 59.63 60.23 60.211 58.593 2 min 42.722 39.384 42.199 46.951 42.889 42.829 4 min 27.966 40.585 38.878 45.33 35.009 36.345 8 min 34.201 37.944 31.136 40.13 28.344 33.816 16 min 30.85 (Comparative Example 5) 35.491 (Comparative Example 7) 25.658 (Example 1) 28.002 (Example 3) 26.020 (Comparative Example 1) 29.072 (Comparative Example 3) 32 min 29.7 (Comparative Example 6) 27.698 (Comparative Example 8) 28.572 (Example 2) 23.736 (Example 4) 24.022 (Comparative Example 2) 26.020 (Comparative Example 4)

[0192] Referring to [Table 2] above, as a result of comparing the fine grinding efficiency according to the amount of tannic acid added, in Example 4 above, after adding 500 g / ton of tannic acid and grinding for 32 minutes, the particle size (D) of the ground material 50 ) was 23.736 μm, which represented the minimum value.

[0193] On the other hand, in Comparative Example 6, in which a dispersant was not used, the particle size (D) of the ground material 50 The particle size was 29.7 μm, and Example 4 showed a result of a 20.1% improvement in particle size reduction compared to Comparative Example 6.

[0194] In addition, in Comparative Example 8 using sodium silicate as a dispersant, the particle size (D) of the ground material 50 The value was 27.698 μm, and Example 4 showed a result of a 14.3% improvement in particle size reduction compared to Comparative Example 8.

[0195] In Comparative Example 5, which did not use a dispersant, the grinding efficiency decreased rapidly after 16 minutes of grinding time and the particle size tended to stagnate, whereas in Example 3, which used tannic acid, it was confirmed that continuous fine grinding was possible even after 16 minutes of grinding time.

[0196] As a result of analyzing the dispersion effect according to the amount of tannic acid added, in Examples 1 to 4, dispersion performance improved with increasing tannic acid addition in the range of 250 to 500 g / ton; however, in Comparative Examples 2 and 4, dispersion performance tended to decrease when 750 g / ton or more was added. In particular, when 1000 g / ton was added, the particle size (D of the ground material) 50 The viscosity increased to 26.020 μm, which is attributed to the increase in slurry viscosity and intermolecular cross-linking effects caused by the addition of an excessive amount of tannic acid. Therefore, when the slurry concentration (solid content concentration) is 50 wt% and the steel ball filling rate (media filling rate) relative to the effective internal area of ​​the grinder is 50%, the optimal amount of tannic acid added was determined to be 500 g / ton.

[0197] According to the present invention, by introducing tannic acid, which is suitable for the surface characteristics of molybdenum disulfide and is environmentally friendly, as a dispersant to suppress aggregation between particles during the grinding process and enhance dispersibility, it was confirmed that additional grinding beyond the existing grinding limit is possible during wet grinding using an attrition mill, thereby improving grinding efficiency and achieving a reduction in particle size.

[0199] Although various preferred embodiments of the present invention have been described above with some examples, the descriptions of various embodiments described in the "Specific details for carrying out the invention" section are merely illustrative, and those skilled in the art to which the present invention pertains will understand that the present invention can be carried out with various modifications or equivalent embodiments from the above description.

[0200] Furthermore, since the present invention can be implemented in various other forms, the present invention is not limited by the description above. The above description is provided merely to make the disclosure of the present invention complete and to fully inform those skilled in the art of the scope of the present invention, and it should be understood that the present invention is defined only by each claim of the claims.

Claims

Claim 1 (a-1) a step of preparing a molybdenum concentrate containing MoS2; (a-2) a step of forming a slurry by adding the molybdenum concentrate containing MoS2 to water and preparing a slurry by adding a dispersant, tannin acid, at a rate of 250 g / ton or more and 500 g / ton or less; and (a-3) a step of wet grinding by adding the slurry to an attrition mill, which is a grinder, and rotating an internal stirrer at 300 rpm or more for 16 to 32 minutes; comprising a method for fine grinding molybdenum disulfide using a dispersant. Claim 2 delete Claim 3 A method for finely grinding molybdenum disulfide using a dispersant, wherein, in claim 1, the above step (a-2) includes a step of mixing for a stirring time of 10 minutes after adding the dispersant. Claim 4 A method for finely grinding molybdenum disulfide using a dispersant, characterized in that, in step (a-3) of claim 1, the step of filling the attrition mill with steel balls is included. Claim 5 delete Claim 6 In claim 1, the particle size (D of the molybdenum concentrate containing MoS2) after step (a-3) above. 50 A method for finely grinding molybdenum disulfide using a dispersant, characterized in that ) is 30 μm or less. Claim 7 (b-1) a step of preparing a molybdenum concentrate having a MoS2 content of 85 wt% or less; (b-2) a step of forming a first slurry by adding the molybdenum concentrate having a MoS2 content of 85 wt% or less to water, and preparing a slurry by adding a dispersant, tannin acid, at a rate of 250 g / ton or more and 500 g / ton or less; (b-3) a step of wet grinding by adding the slurry to an attrition mill having a grinder and rotating an internal stirrer at 300 rpm or more for 16 to 32 minutes; and (b-4) a step of flotation separating the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less; comprising a method for producing a high-quality molybdenum disulfide product from molybdenum concentrate. Claim 8 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate, characterized in that, in step (b-2) of claim 7, the concentration of the first slurry is 50 wt%. Claim 9 A method for producing a high-grade molybdenum disulfide product from molybdenum concentrate, characterized in that, in step (b-3) of claim 7, the step of filling the attrition mill with steel balls is included. Claim 10 In claim 7, the particle size (D) of the wet-milled molybdenum concentrate having a MoS2 content of 85 wt% or less in step (b-4) above. 50 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate, characterized in that ) is 30 μm or less. Claim 11 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate according to claim 7, wherein step (b-4) comprises the step of adding the wet-ground molybdenum concentrate having a MoS2 content of 85 wt% or less to water to form a second slurry, and adding a flotation reagent to the second slurry to condition it. Claim 12 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate, characterized in that, in claim 11, the concentration of the second slurry is 10 to 20 wt%. Claim 13 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate, wherein, in claim 11, the conditioning step comprises a step of mixing with 200 g / ton of coagulant (Kerosene) and a stirring time of 5 minutes. Claim 14 A method for producing a high-quality molybdenum disulfide product from molybdenum concentrate, wherein, in claim 11, the conditioning step comprises a step of mixing with 100 g / ton of foaming agent (AF65) and a stirring time of 5 minutes. Claim 15 A method for producing a high-grade molybdenum disulfide product from molybdenum concentrate, wherein, in claim 7, the above step (b-4) is performed by setting the flotation separation time to 5 minutes. Claim 16 A method for producing a high-grade molybdenum disulfide product from molybdenum concentrate, characterized in that, in claim 7, the grade of the molybdenum disulfide product obtained after step (b-4) is 98% or higher.

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