A method for preparing ore samples and a method for studying flotation technology in process mineralogy research

Abstract

The present invention provides a method for preparing ore samples and a method for studying flotation processes in process mineralogy research, and relates to the fields of mineralogy and mineral processing technology. The present invention selects an aqueous resin similar to a flotation system to disperse the ore; by adding a flotation agent and aerating, a slurry system consistent with the flotation process is obtained, and suitable conditions are selected for solidification to obtain an ore sample containing flotation bubbles, flotation agents, and ore particles. Subsequently, the ore sample is cut, thinned, and polished to obtain an ore sample probe sheet in the "particle-bubble" phase interface sorting process, and the flotation process can be directly studied by an optical microscope, a scanning electron microscope, an electron probe, and the like. Based on the method for obtaining a probe sheet containing a "gas-solid" phase system proposed by the present invention, the effect of the agent can be directly and objectively evaluated, the factors affecting the flotation effect can be identified, and the flotation mechanism such as the mineral sorting process in the flotation process, the relationship between bubble characteristics and flotation effect, etc. can be studied.

Description

Technical Field

[0001] The present invention relates to the field of mineralogy and mineral processing technology, and in particular to a method for preparing an ore sample in process mineralogy research and a method for researching a flotation process. Background Art

[0002] Flotation is one of the most widely used mineral processing methods. Almost all ores, such as gold, silver, lead, zinc, copper, and rare earth ores, can be separated by flotation. The essence of flotation is the process of separating minerals at the solid-liquid-gas interface by exploiting differences in their surface properties. One of the core issues in current flotation research is the mechanism of interaction at the particle-bubble interface. With the rapid development of testing methods and characterization techniques, analytical tools such as high-speed photography, contact angle measurement, dynamic force measurement, and numerical simulation have been widely applied to flotation process mineralogy and flotation mechanism research. These techniques have significantly advanced understanding of the mechanisms of particle-bubble interaction during flotation. However, existing research methods rely on image processing and simulation, which prevents systematic process mineralogy analysis of the particle-bubble interface during flotation. This, in part, has limited in-depth research into flotation mechanisms. This is primarily due to the fact that flotation is a dynamic and rapid process, making it difficult to obtain ore samples in a flotation state using current methods.

[0003] To address this issue, the present invention provides a method for obtaining ore samples during the "particle-bubble" phase interface sorting process, which can help obtain "gas-solid" phase system samples during flotation, facilitate subsequent process mineralogy research, and deepen the understanding of the flotation mechanism. Summary of the Invention

[0004] The purpose of the present invention is to provide a method for preparing ore samples and a method for studying flotation processes in process mineralogy research. The present invention can obtain "gas-solid" phase system samples during flotation, laying the foundation for studying flotation mechanisms such as the mineral sorting process in the flotation process, the relationship between bubble characteristics and flotation effect, etc.

[0005] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0006] The present invention provides a method for preparing ore samples in process mineralogy research, comprising the following steps: crushing the ore to be sampled and grinding it to a fineness required for flotation to obtain ore particles;

[0007] Mixing a water-based epoxy resin, a water-based epoxy resin curing agent and water to obtain a water-based resin solution; the mass ratio of the water-based epoxy resin, the water-based epoxy resin curing agent and water is 1-1.5:1:1-5;

[0008] Mixing the aqueous resin solution and ore particles to obtain a slurry; the mass concentration of the slurry is 15 to 50%;

[0009] A flotation agent is added to the ore pulp to adjust the ore pulp system to be consistent with the flotation process conditions to be studied; the adjusted ore pulp is then stirred, and air is introduced into the ore pulp until the ore pulp becomes viscous. After the bubbles are evenly dispersed, the ore pulp is placed at 25-50° C. for more than 10 hours to allow the water-based epoxy resin to solidify, and air is continuously introduced during the placement process to obtain an ore sample.

[0010] Preferably, the method of introducing air includes: introducing air into the slurry through a glass tube with a diameter of 0.5 to 1 mm.

[0011] Preferably, the air introduction rate is 0.01 to 0.1 m 3 / h·L.

[0012] Preferably, the stirring rate is 60-120 r / min.

[0013] The present invention provides a research method for a flotation process, comprising the following steps:

[0014] Prepare ore samples according to the preparation method described in the above scheme;

[0015] Slicing the ore sample to obtain a block sample;

[0016] The block sample is single-sided ground and polished, a binder is applied to the polished surface, and the block sample is affixed to a glass slide; the ore block on the glass slide is cut, and the cut slices are ground and polished until the thickness of the mineral slices is 0.03 to 0.1 mm, thereby obtaining a probe sheet containing flotation bubbles and mineral particles;

[0017] The probe sheet is placed under an optical microscope, an electron microscope or an electron probe for observation.

[0018] Preferably, the thickness of the block sample is 3 to 10 mm.

[0019] Preferably, the electron microscope includes a scanning electron microscope or a transmission electron microscope.

[0020] The invention provides a method for preparing ore samples in process mineralogy research. The method comprises the following steps: crushing ore to be sampled and grinding it to a fineness required for flotation to obtain ore particles; mixing a water-based epoxy resin, a water-based epoxy resin curing agent and water to obtain a water-based resin solution; the mass ratio of the water-based epoxy resin, the water-based epoxy resin curing agent and water is 1-1.5:1:1-5; mixing the water-based resin solution and the ore particles to obtain a pulp; the mass concentration of the pulp is 15-50%; adding a flotation agent to the pulp to adjust the pulp system to be consistent with the flotation process conditions to be studied; then stirring the adjusted pulp, and after the pulp becomes viscous, introducing air into the pulp, and after the bubbles are evenly dispersed, placing the pulp at 25-50°C for more than 10 hours to solidify the water-based epoxy resin, and continuously introducing air during the placing process to obtain the ore sample.

[0021] The present invention uses a water-based resin similar to the flotation system to disperse the ore; by adding flotation agents and aerating, a slurry system consistent with the flotation process is obtained, and suitable conditions are selected for solidification to obtain an ore sample containing flotation bubbles, flotation agents, and ore particles. The ore sample is subsequently cut, thinned, and polished to obtain a probe piece of the ore sample in the "particle-bubble" phase interface sorting process, and the flotation process can be directly studied using an optical microscope, a scanning electron microscope, an electron probe, etc. Based on the method proposed by the present invention for obtaining a probe piece containing a "gas-solid" phase system, it is possible to directly and objectively evaluate the effect of the agent, identify the factors affecting the flotation effect, and study the flotation mechanism such as the mineral sorting process in the flotation process, the relationship between bubble characteristics and flotation effect, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The process flow chart of the method for preparing ore samples in process mineralogy research of the present invention is as follows;

[0023] Figure 2 This is a photo of the ore sample of Example 1 under an optical microscope (left - reflected light; right - transmitted light). DETAILED DESCRIPTION

[0024] The present invention provides a method for preparing ore samples in process mineralogy research, comprising the following steps: crushing the ore to be sampled and grinding it to a fineness required for flotation to obtain ore particles;

[0025] Mixing a water-based epoxy resin, a water-based epoxy resin curing agent and water to obtain a water-based resin solution; the mass ratio of the water-based epoxy resin, the water-based epoxy resin curing agent and water is 1-1.5:1:1-5;

[0026] Mixing the aqueous resin solution and ore particles to obtain a slurry; the mass concentration of the slurry is 15 to 50%;

[0027] A flotation agent is added to the ore pulp to adjust the ore pulp system to be consistent with the flotation process conditions to be studied; the adjusted ore pulp is then stirred, and air is introduced into the ore pulp until the ore pulp becomes viscous. After the bubbles are evenly dispersed, the ore pulp is placed at 25-50° C. for more than 10 hours to allow the water-based epoxy resin to solidify, and air is continuously introduced during the placement process to obtain an ore sample.

[0028] The present invention crushes the ore to be sampled and grinds it to the fineness required for flotation to obtain ore particles. The present invention has no special requirements for the crushing and grinding process, and the crushing and grinding process well known in the art can be used.

[0029] The present invention mixes a water-based epoxy resin, a water-based epoxy resin curing agent and water to obtain a water-based resin solution.

[0030] In the present invention, the mass ratio of the waterborne epoxy resin, waterborne epoxy resin curing agent and water is 1-1.5:1:1-5, preferably 1:1:2. The waterborne resin solution of the present invention is similar to the flotation system and can more realistically restore the flotation process.

[0031] After obtaining the ore particles and the aqueous resin solution, the present invention mixes the aqueous resin solution and the ore particles to obtain ore slurry.

[0032] In the present invention, the mass concentration of the ore pulp is preferably 15-50%, and more preferably consistent with the ore pulp concentration in the flotation process to be studied.

[0033] After obtaining the ore pulp, the present invention adds a flotation agent to the ore pulp and adjusts the ore pulp system to be consistent with the flotation process conditions to be studied; then the adjusted ore pulp is stirred, and air is introduced into the ore pulp after the ore pulp becomes viscous. After the bubbles are evenly dispersed, the ore pulp is placed at 25-50° C. for more than 10 hours to solidify the water-based epoxy resin, and air is continuously introduced during the placement process to obtain an ore sample.

[0034] In the present invention, the adjustment of the pulp system to be consistent with the flotation process conditions to be studied includes: maintaining the type and dosage of flotation reagents consistent, maintaining the pulp temperature consistent, and maintaining the pH value consistent.

[0035] In the present invention, the stirring rate is preferably 60 to 120 r / min, more preferably 80 to 100 r / min. In the present invention, the method of introducing air preferably includes: introducing air into the slurry through a glass tube with a diameter of 0.5 to 1 mm. In the present invention, the air introduction rate is preferably 0.01 to 0.1 m / min. 3 / h·L, more preferably 0.03 to 0.08m 3 / h·L. The present invention controls the air introduction rate to obtain micron-level and millimeter-level bubbles, at which time some mineral particles adhere to the bubbles.

[0036] Since the slurry is viscous and gas is continuously introduced, there will always be bubbles in the slurry. After the resin is solidified, the bubbles will be solidified inside the sample, thereby obtaining a "gas-solid" phase system sample during flotation, laying the foundation for studying the flotation mechanism such as the mineral sorting process in the flotation process, the relationship between bubble characteristics and flotation effect, etc.

[0037] The present invention provides a research method for a flotation process, comprising the following steps:

[0038] Prepare ore samples according to the preparation method described in the above scheme;

[0039] Slicing the ore sample to obtain a block sample;

[0040] The block sample is single-sided ground and polished, a binder is applied to the polished surface, and the block sample is affixed to a glass slide; the ore block on the glass slide is cut, and the cut slices are ground and polished until the thickness of the mineral slices is 0.03 to 0.1 mm, thereby obtaining a probe sheet containing flotation bubbles and mineral particles;

[0041] The probe sheet was placed under an electron microscope for observation.

[0042] The present invention will not elaborate on the preparation process of the ore sample.

[0043] After obtaining the ore sample, the present invention slices the ore sample to obtain a block sample.

[0044] In the present invention, the thickness of the block sample is preferably 3 to 10 mm. In the present invention, the block sample is preferably cut into block samples with two flat surfaces using a cutting machine.

[0045] After obtaining the block sample, the present invention performs single-side grinding and polishing on the block sample, applies an adhesive on the polished surface, and sticks the block sample onto a glass slide.

[0046] The present invention has no special requirements for the single-side grinding and polishing process, and a single-side grinding and polishing process well known in the art can be used. In the embodiment of the present invention, one side of the block is coarsely ground with a 200-mesh diamond grinding wheel to remove surface cuts, and then further finely ground with a 400-2000 mesh diamond grinding wheel to obtain a smoother surface. Then, an appropriate amount of diamond (3 μm) suspension is dripped onto a rotating polyurethane polishing pad to fully polish the ore surface.

[0047] The present invention has no special requirements for the specific type of the adhesive, and any adhesive well known in the art can be used, such as epoxy resin. The present invention preferably cleans the polished surface obtained in the previous step and fully dries it; then, apply an appropriate amount of adhesive evenly on the polished surface, press the polished surface onto a glass slide, expel the air, and let it stand at a temperature above 80°C for more than 2 hours to ensure that the glass slide is firmly adhered. The present invention adheres the block sample to the glass slide, which not only makes it easier to cut later, but also enhances the strength of the slice, making it less likely to break.

[0048] After the block sample is pasted onto a glass slide, the present invention cuts the ore block on the glass slide, and then grinds and polishes the cut slices until the thickness of the mineral slices is 0.03 to 0.1 mm to obtain probe slices containing flotation bubbles and mineral particles.

[0049] In the present invention, the cutting is preferably performed using a cutting machine. The thickness of the mineral film on the glass slide after cutting is preferably 0.5 mm. In the present invention, the grinding and polishing process is the same as the single-side grinding and polishing process described above, and will not be repeated here.

[0050] After obtaining a probe sheet containing flotation bubbles and mineral particles, the present invention places the probe sheet under an electron microscope for observation. In the present invention, the electron microscope preferably comprises a scanning electron microscope or a transmission electron microscope. The present invention uses an electron microscope to visually observe the flotation effect, directly and objectively evaluate the effectiveness of the reagent, identify factors affecting the flotation effect, and study flotation mechanisms such as the mineral separation process in the flotation process and the relationship between bubble characteristics and flotation effect.

[0051] The following is a detailed description of the method for preparing ore samples for process mineralogy research provided by the present invention in conjunction with the examples, but they should not be understood as limiting the scope of protection of the present invention.

[0052] Example 1

[0053] The Barzhe deposit (801 mine) in Inner Mongolia is a super-large deposit of rare earth, uranium, niobium, and zirconium polymetallic paragenesis. Its main useful minerals include niobium iron ore, khingyanite, zircon, fluorocarbon cerium, monazite, and zinc heliotropes, while its main gangue minerals are quartz, potassium feldspar, and sodium iron amphibole. The ore has a complex mineral composition, and during the flotation of niobium minerals, factors such as inter-mineral inclusions, inadequate mineral dissociation, and poor flotation agent selectivity can all affect the flotation efficiency.

[0054] In order to find out the factors that affect the flotation index of niobium minerals, 100g of ore was selected and Figure 1 Flotation test ore samples were prepared according to the process shown and simple mineralogical studies were performed.

[0055] The specific steps are as follows:

[0056] (1) Ore crushing and grinding: The ore to be sampled is crushed and finely ground to -0.043 mm, accounting for 95 wt%.

[0057] (2) Sample preparation:

[0058] a. A waterborne epoxy resin (purchased from Green Union (Jining) Chemical Technology Co., Ltd.), a waterborne epoxy resin curing agent, and water were mixed in a mass ratio of 1:1:2 to obtain a white viscous aqueous resin solution;

[0059] b 100g of ore and 150g of the aqueous resin solution obtained in step a was poured into a beaker to obtain an ore mass concentration of 40% slurry;

[0060] c were added to the slurry obtained in step b an appropriate amount of water glass adjustment agent 1000g / t, stirred for 2min, added a collector benzohydroxamic acid 600g / t, stirred for 3min, adjusted the slurry pH value to 8.5, the temperature 25 ℃;

[0061] d. Continue stirring for 50 minutes. When the slurry becomes viscous, introduce air into the slurry through a glass tube with a diameter of 0.5 mm. The aeration rate is controlled at 0.02 m 3 / h·L, stirring rate 90±20r / min, at this time some mineral particles adhere to the bubbles and are evenly dispersed in the slurry.

[0062] e. Place the beaker from the previous step on a hot plate, heat to 40°C, and maintain the constant temperature for 12 hours. The water-based resin in the beaker solidifies to obtain a blank containing ore and bubbles.

[0063] (3) Slicing: Use a cutting machine to process the blank into blocks with smooth surfaces and a thickness of about 5 mm.

[0064] (4) Single-sided grinding and polishing:

[0065] a. Grind one side of the block with a 200-mesh diamond grinding wheel to remove the surface cuts;

[0066] b. Use 1000 mesh diamond grinding wheel to further grind to obtain a smooth surface;

[0067] c. Add an appropriate amount of diamond (3μm) suspension onto the rotating polyurethane polishing pad to fully polish the ore surface.

[0068] (5) Paste the slide

[0069] a. Clean and dry the polished surface obtained in the previous step;

[0070] b. Apply an appropriate amount of epoxy resin evenly on the polished surface, press the polished surface tightly onto the glass slide and expel the air;

[0071] c. Place at 85°C for 3 hours to ensure that the slide is firmly adhered.

[0072] (6) Thin slice cutting: The sample is further cut. The ore block on the glass slide is carefully cut to a thickness of about 0.5 mm using a diamond wire saw.

[0073] (7) Using the method in step (4), the surface of the thin slice is polished to a thickness of 0.03 mm to obtain a probe sheet containing flotation bubbles and mineral particles, which is then cleaned and dried.

[0074] (8) Take the probe sheet obtained in step (7) and study the behavior of the target mineral (niobite) during the flotation process under an optical microscope.

[0075] Example 1 Test results are shown in Figure 2 (Left - reflected light; right - transmitted light). Figure 2 As can be seen, the flotation reagent has relatively good selectivity, and the collector has a strong ability to capture niobium ore. During the flotation process, a large amount of the target mineral, niobium ore, accumulated on the bubbles, along with a very small amount of ilmenite. Minerals such as zircon and natrium-iron amphibole showed little adsorption on the flotation bubbles, and no mechanical inclusions were observed during the flotation process. The flotation process conditions are considered appropriate. The left image shows some niobium ore intergrowth with natrium-iron amphibole, indicating that increasing the grinding time, for example, should be used to improve the degree of monomer dissociation of the minerals.

[0076] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A method for preparing ore samples in process mineralogy research, characterized in that: The following steps are involved: Crushing the ore to be sampled and grinding it to the fineness required for flotation to obtain ore particles; Mixing a water-based epoxy resin, a water-based epoxy resin curing agent, and water to obtain a water-based resin solution; the mass ratio of the water-based epoxy resin, the water-based epoxy resin curing agent, and water is 1-1.5:1:1-5; Mixing the aqueous resin solution and ore particles to obtain a slurry; the mass concentration of the slurry is 15-50%; A flotation agent is added to the slurry to adjust the slurry system to be consistent with the flotation process conditions to be studied; the adjusted slurry is then stirred, and air is introduced into the slurry until the slurry becomes viscous. After the bubbles are evenly dispersed, the slurry is placed at 25-50° C. for more than 10 hours to allow the water-based epoxy resin to cure, with air being continuously introduced during the placement process, to obtain an ore sample.

2. The preparation method according to claim 1, characterized in that The method of introducing air includes: introducing air into the slurry through a glass tube with a diameter of 0.5-1 mm.

3. The preparation method according to claim 1 or 2, characterized in that The air introduction rate is 0.01~0.1m 3 / h·L.

4. The preparation method according to claim 1, characterized in that The stirring rate is 60-120 r / min.

5. A research method for flotation process, characterized in that: The following steps are involved: preparing an ore sample according to the preparation method according to any one of claims 1 to 4; Slicing the ore sample to obtain a block sample; The block sample is single-sided ground and polished, a binder is applied to the polished surface, and the block sample is affixed to a glass slide; the ore block on the glass slide is cut, and the cut slices are ground and polished until the thickness of the mineral slices is 0.03 to 0.1 mm, thereby obtaining a probe sheet containing flotation bubbles and mineral particles; The probe sheet is placed under an optical microscope, an electron microscope or an electron probe for observation.

6. The research method according to claim 5, characterized in that The thickness of the block sample is 3-10 mm.

7. The research method according to claim 5, characterized in that The electron microscope includes a scanning electron microscope or a transmission electron microscope.

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