Application of PCE-11 as a modifier in the flotation separation of brucite and serpentine.
By using PCE-11 modifier in the flotation of brucite and serpentine, the difference in their flotation characteristics is altered, achieving effective separation of brucite and serpentine. This solves the problem of poor separation effect in existing technologies, improves the utilization rate of low-grade brucite resources, and reduces environmental pollution.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NORTHEASTERN UNIV CHINA
- Filing Date
- 2023-11-29
- Publication Date
- 2026-06-02
AI Technical Summary
Research on reagents for the flotation separation of brucite and serpentine is limited and the separation effect is poor, making it difficult to achieve effective separation and severely restricting the utilization of low-grade brucite resources.
By using PCE-11 as a modifier in a sodium oleate system, the adsorption characteristics of brucite and serpentine surfaces are affected, and the positive flotation method is used to achieve effective separation of brucite and serpentine. PCE-11 is a comb-shaped polymer graft copolymer.
It achieves effective separation of brucite and serpentine, improves the utilization rate of low-grade brucite resources, reduces the serpentine content in concentrate, and PCE-11 is green, environmentally friendly, and inexpensive, reducing environmental pollution.
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Figure CN117443584B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of brucite beneficiation and purification technology, specifically to the application of PCE-11 as a modifier in the flotation separation of brucite and serpentine. Background Technology
[0002] Magnesium is one of the most abundant elements on Earth, a lightweight and ductile silvery-white metal. With the continuous development of science and technology and the progress of industry, the utilization rate of magnesium resources has gradually increased. Some non-metallic minerals with lower utilization rates have also gradually attracted attention and research, with brucite being one of them. Brucite is the mineral with the highest magnesium content discovered to date. Because of this characteristic, it has advantages in producing high-purity magnesium oxide compared to raw materials such as seawater, brine, and magnesite, including lower cost and no pollution. Furthermore, because the products of the thermal decomposition of natural brucite are non-toxic and harmless, it can also be used as a high-grade flame retardant and refractory material. Brucite possesses unique physicochemical properties and plays an irreplaceable role in many industries such as papermaking, construction, military, metallurgy, and environmental protection. In recent years, people have gradually recognized the industrial value of brucite, leading to more in-depth research and development. However, due to the late start of brucite research in my country, the limited amount of related research, and the immature mineral processing technology, there has been a significant waste of brucite resources. Serpentine is a major associated gangue mineral in brucite ore. Both brucite and serpentine share similar physicochemical properties and interact during flotation, making effective separation difficult and severely limiting the utilization of low-grade brucite resources. Research on flotation reagents related to brucite and serpentine is limited, resulting in poor separation effects. Therefore, discovering a flotation modifier to alter the differences in flotation characteristics between brucite and serpentine, thereby achieving effective separation, is crucial for improving the utilization rate of low-grade brucite resources. Summary of the Invention
[0003] To address the shortcomings in the prior art regarding the limited research on reagents and poor separation effects in the flotation separation of brucite and serpentine, this invention provides the application of PCE-11 as a modifier in the flotation separation of brucite and serpentine. The purpose of this invention is to utilize the positive flotation method in a sodium oleate system, employing the modifier PCE-11 to amplify the difference in floatability between brucite and serpentine during the flotation process, thereby achieving effective separation of brucite and the gangue mineral serpentine.
[0004] The modifier PCE-11 is a high-molecular-weight graft copolymer, a comb-like polymer composed of a main chain and multiple side chains. Furthermore, modifier PCE-11 features good separation performance, non-toxicity, low price, and easy commercial availability.
[0005] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine involves adding PCE-11 to the prepared brucite ore pulp. The pH range of the pulp is 10.0–12.0. The dosage of PCE-11 added to the pulp is 400–700 mg / L.
[0006] The flotation separation process of brucite and serpentine specifically includes the following steps:
[0007] Step 1: Grinding
[0008] The raw brucite ore is crushed and ball-milled to obtain brucite ore powder; among which, the ore powder with a particle size of <74μm accounts for 70-90% of the total mass of brucite.
[0009] Step 2: Prepare the paste
[0010] Mix the raw magnesia ore powder with deionized water and put it into the flotation equipment. The solid-liquid ratio of the slurry is 1:(8-10). Stir the mixture to ensure that the ore sample is fully mixed. Add a pH adjuster to adjust the pH of the slurry to 10-12 until the pH of the slurry is stable, and the raw ore slurry is obtained.
[0011] Step 3: Direct flotation separation of brucite and serpentine
[0012] Add PCE-11 solution to the slurry with a pH of 10-12 and stir. After the PCE-11 is fully dispersed and reacted, add sodium oleate collector and continue stirring until the reaction is complete. Start flotation froth removal to obtain the final flotation froth concentrate and tailings in the tank.
[0013] Step 4: Processing the flotation product
[0014] The final flotation froth product is dried to obtain the final product, brucite concentrate.
[0015] In step 1, the main component of the brucite ore is brucite, and its gangue mineral is mainly serpentine. The ore contains 50-60% MgO and 5-15% SiO2 by weight percentage.
[0016] In step 2, the flotation equipment is a hanging tank flotation machine with an impeller speed of 1800 rpm to 2100 rpm.
[0017] In step 2, the slurry preparation is carried out at room temperature, which is 20℃~26℃.
[0018] In step 2, the pH adjuster is a NaOH solution, preferably a NaOH aqueous solution with a mass fraction of 1-5%.
[0019] In step 3, the stirring speed is 1800 rpm to 2100 rpm.
[0020] In step 3, the mass concentration of the modifier PCE-11 is 10.0–15.0 g / L; the addition amount is 400–700 mg / L.
[0021] In step 3, the mass concentration of the collector sodium oleate is 3.0-5.0 g / L, and the amount added is 200-400 mg / L. The preparation method is as follows: weigh an appropriate amount of sodium oleate solid powder and add it to an appropriate amount of deionized water, stir at 50-70°C until the sodium oleate solid powder is completely dissolved to obtain an aqueous solution of the collector sodium oleate.
[0022] In step 3, the foam scraping time is 3 to 5 minutes, and the foam is scraped once every 10 seconds.
[0023] In step 4, the drying method is to place the item in a vacuum drying oven for drying.
[0024] In the above method, the main components of the brucite concentrate are MgO > 64.0% and SiO2 < 1.5% by mass percentage.
[0025] In the above method, the MgO recovery rate in brucite concentrate is 70.0% to 85.0% by mass percentage.
[0026] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine, compared with the prior art, has the following advantages:
[0027] 1. The modifier developed in this invention, in a sodium oleate system, affects the adsorption of sodium oleate on the surfaces of brucite and serpentine, thereby creating a difference in the hydrophobicity of the brucite and serpentine surfaces. This enhances the hydrophilicity of the gangue mineral serpentine surface, while brucite retains good floatability after reacting with PCE-11, effectively reducing the serpentine content in the concentrate and achieving the separation of brucite and serpentine. The modifier provided by this invention exhibits significant separation and purification effects, achieving good separation indicators.
[0028] 2. This invention develops the application of PCE-11 as a modifier. The modifier of this invention is mainly used as a water-reducing agent in the silicate concrete industry. Therefore, it is used as a modifier for the separation of brucite and serpentine. The modifier PCE-11 has different effects on the flotation of brucite and serpentine. At present, there is very little research on related reagents for effectively separating brucite and serpentine. This invention provides a new flotation separation reagent for the separation of brucite and gangue mineral serpentine.
[0029] 3. The modifier PCE-11 provided by this invention, compared with traditional separation agents for brucite and serpentine (inorganic agents such as water glass), is green, environmentally friendly, and biodegradable, which can reduce the pollution caused by the agents to the environment. At the same time, the agent PCE-11 provided by this invention is also inexpensive and readily available. Attached Figure Description
[0030] Figure 1 This is a schematic diagram of the process of using PCE-11 as a modifier in the flotation separation of brucite and serpentine in an embodiment of the present invention. Detailed Implementation
[0031] The present invention will be further described in detail below with reference to the embodiments.
[0032] The following embodiments are intended to enable those skilled in the art to more fully understand the present invention, but do not limit the invention in any way.
[0033] Unless otherwise specified, the experimental methods described in the following examples are conventional methods; the reagents and materials described are commercially available unless otherwise specified.
[0034] In the following examples, the main components of the brucite ore were brucite and gangue mineral serpentine, containing 50-60% MgO and 5-15% SiO2 by weight. The PCE-11 pH adjuster and sodium oleate collector were chemically pure, and the hydrochloric acid and sodium hydroxide pH adjusters were analytically pure. All reagents were prepared into aqueous solutions of the appropriate concentrations using deionized water.
[0035] Example 1
[0036] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine is described in the following process flow diagram. Figure 1 This includes the following steps:
[0037] Step 1: Grinding
[0038] The raw brucite ore is crushed and ball-milled to obtain brucite powder; of which, the powder with a particle size of <74μm accounts for 80% of the total mass of brucite.
[0039] Step 2: Prepare the paste
[0040] At 26℃, brucite ore powder was placed in a hanging trough flotation machine, and deionized water was added. The ore powder and deionized water were thoroughly mixed at a mass ratio of 1:9. The mixture was stirred for 2 minutes at a flotation machine speed of 2000 rpm to obtain brucite ore slurry. Then, the pH of the slurry was measured, and a 3% NaOH aqueous solution was added to adjust the pH value to 11.0. The mixture was then stirred for another 3 minutes to stabilize the pH value, resulting in a brucite ore slurry with a pH value of 11.0.
[0041] Step 3: Direct flotation separation of brucite and serpentine
[0042] Add PCE-11 solution to the slurry with a pH of 11.0. The amount of PCE-11 in the slurry with a pH of 11.0 is 500 mg / L. Stir for 3 min to allow PCE-11 to be fully dispersed in the slurry. Then add sodium oleate collector. The amount of sodium oleate in the slurry with a pH of 11 is 300 mg / L. Continue stirring. After 3 min, start flotation froth removal for 3 min to obtain the final flotation froth product and the product in the tank.
[0043] Step 4: Processing the flotation product
[0044] The final flotation foam product and the remaining product in the tank are dried to obtain brucite concentrate and tailings after flotation separation and purification. The composition is analyzed and the product indicators are calculated.
[0045] In this embodiment, the main components of the final brucite concentrate product, by mass ratio, are: MgO 68.34% and SiO2 0.83%. The MgO recovery rate in the brucite concentrate is 75.67% by mass percentage.
[0046] Example 2
[0047] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine is described in the following process flow diagram. Figure 1 This includes the following steps:
[0048] Step 1: Grinding
[0049] The raw brucite ore is crushed and ball-milled to obtain brucite powder; of which, the powder with a particle size of <74μm accounts for 80% of the total mass of brucite.
[0050] Step 2: Prepare the paste
[0051] At 26℃, brucite ore powder was placed in a hanging trough flotation machine, and deionized water was added. The ore powder and deionized water were thoroughly mixed at a mass ratio of 1:9. The mixture was stirred for 2 minutes at a flotation machine speed of 1800 rpm to obtain brucite ore slurry. Then, the pH of the slurry was measured, and a 2.5% NaOH aqueous solution was added to the slurry to adjust the pH value to 10.5. The mixture was then stirred for 3 minutes to stabilize the pH value, resulting in a brucite ore slurry with a pH value of 10.5.
[0052] Step 3: Direct flotation separation of brucite and serpentine
[0053] Add PCE-11 solution to the slurry with a pH of 10.5. The amount of PCE-11 in the slurry with a pH of 10.5 is 440 mg / L. Stir for 3 min to allow PCE-11 to be fully dispersed in the slurry. Then add sodium oleate collector. The amount of sodium oleate in the slurry with a pH of 11 is 340 mg / L. Continue stirring. After 3 min, start flotation froth removal for 3 min to obtain the final flotation froth product and the product in the tank.
[0054] Step 3: Processing the flotation product
[0055] The final flotation foam product and the remaining product in the tank are dried to obtain brucite concentrate and tailings after flotation separation and purification. The composition is analyzed and the product indicators are calculated.
[0056] In this embodiment, the main components of the final brucite concentrate product, by mass ratio, are: MgO 67.21% and SiO2 0.98%. The MgO recovery rate in the brucite concentrate is 80.44% by mass.
[0057] Example 3
[0058] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine is described in the following process flow diagram. Figure 1 This includes the following steps:
[0059] Step 1: Grinding
[0060] The raw brucite ore is crushed and ball-milled to obtain brucite powder; among which, the powder with a particle size of <74μm accounts for 90% of the total mass of brucite.
[0061] Step 2: Prepare the paste
[0062] At 26℃, brucite ore powder was placed in a hanging trough flotation machine, and deionized water was added. The ore powder and deionized water were thoroughly mixed at a mass ratio of 1:8. The mixture was stirred for 2 minutes at a flotation machine speed of 2100 rpm to obtain brucite ore slurry. Then, the pH of the slurry was measured, and a 4% NaOH aqueous solution was added to adjust the pH value to 11.5. The mixture was then stirred for 3 minutes to stabilize the pH value, resulting in brucite ore slurry with a pH value of 11.5.
[0063] Step 3: Direct flotation separation of brucite and serpentine
[0064] Add PCE-11 solution to the slurry with a pH of 11.5. The amount of PCE-11 in the slurry with a pH of 11.5 is 540 mg / L. Stir for 3 minutes to allow PCE-11 to be fully dispersed in the slurry. Then add sodium oleate collector. The amount of sodium oleate in the slurry with a pH of 11 is 260 mg / L. Continue stirring. After 3 minutes, start flotation froth removal for 4 minutes to obtain the final flotation froth product and the product in the tank.
[0065] Step 4: Processing the flotation product
[0066] The final flotation foam product and the remaining product in the tank are dried to obtain brucite concentrate and tailings after flotation separation and purification. The composition is analyzed and the product indicators are calculated.
[0067] In this embodiment, the main components of the final brucite concentrate product, by mass ratio, are: MgO 68.01% and SiO2 0.75%. The MgO recovery rate in the brucite concentrate is 72.08% by mass.
[0068] Example 4
[0069] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine is described in the following process flow diagram. Figure 1 This includes the following steps:
[0070] Step 1: Grinding
[0071] The raw brucite ore is crushed and ball-milled to obtain brucite powder; of which, the powder with a particle size of <74μm accounts for 70% of the total mass of brucite.
[0072] Step 2: Prepare the paste
[0073] At 20℃, brucite ore powder was placed in a hanging trough flotation machine, and deionized water was added. The ore powder and deionized water were thoroughly mixed at a mass ratio of 1:10. The mixture was stirred for 2 minutes at a flotation machine speed of 1950 rpm to obtain brucite ore slurry. Then, the pH of the slurry was measured, and a 3% NaOH aqueous solution was added to the slurry to adjust the pH value to 10. The mixture was then stirred for another 3 minutes to stabilize the pH value, resulting in a brucite ore slurry with a pH value of 10.
[0074] Step 3: Direct flotation separation of brucite and serpentine
[0075] Add PCE-11 solution to the slurry with a pH of 10. The amount of PCE-11 in the slurry with a pH of 10 is 600 mg / L. Stir for 3 min to allow PCE-11 to be fully dispersed in the slurry. Then add sodium oleate collector. The amount of sodium oleate in the slurry with a pH of 10 is 380 mg / L. Continue stirring. After 3 min, start flotation froth removal for 5 min to obtain the final flotation froth product and the product in the tank.
[0076] Step 4: Processing the flotation product
[0077] The final flotation foam product and the remaining product in the tank are dried to obtain brucite concentrate and tailings after flotation separation and purification. The composition is analyzed and the product indicators are calculated.
[0078] In this embodiment, the main components of the final brucite concentrate product, by mass ratio, are: MgO 65.67% and SiO2 1.26%. The MgO recovery rate in the brucite concentrate is 72.81% by mass.
[0079] Example 5
[0080] The application of PCE-11 as a modifier in the flotation separation of brucite and serpentine is described in the following process flow diagram. Figure 1 This includes the following steps:
[0081] Step 1: Grinding
[0082] The raw brucite ore is crushed and ball-milled to obtain brucite powder; among which, the powder with a particle size of <74μm accounts for 90% of the total mass of brucite.
[0083] Step 2: Prepare the paste
[0084] At 20℃, brucite ore powder was placed in a hanging trough flotation machine, and deionized water was added. The ore powder and deionized water were thoroughly mixed at a mass ratio of 1:9. The mixture was stirred for 2 minutes at a flotation machine speed of 1900 rpm to obtain brucite ore slurry. Then, the pH of the slurry was measured, and a 5% NaOH aqueous solution was added to the slurry to adjust the pH value to 12. The mixture was then stirred for 3 minutes to stabilize the pH value, resulting in brucite ore slurry with a pH value of 12.
[0085] Step 3: Direct flotation separation of brucite and serpentine
[0086] Add PCE-11 solution to the slurry with a pH of 12. The amount of PCE-11 in the slurry with a pH of 12 is 650 mg / L. Stir for 3 minutes to allow PCE-11 to be fully dispersed in the slurry. Then add sodium oleate collector. The amount of sodium oleate in the slurry with a pH of 12 is 400 mg / L. Continue stirring. After 3 minutes, start flotation froth removal for 5 minutes to obtain the final flotation froth product and the product in the tank.
[0087] Step 4: Processing the flotation product
[0088] The final flotation foam product and the remaining product in the tank are dried to obtain brucite concentrate and tailings after flotation separation and purification. The composition is analyzed and the product indicators are calculated.
[0089] In this embodiment, the main components of the final brucite concentrate product, by mass ratio, are: MgO 66.77% and SiO2 1.29%. The MgO recovery rate in the brucite concentrate is 82.01% by mass.
Claims
1. Use of PCE-11 as a regulator in the flotation separation of brucite from serpentine, characterized in that, The flotation separation of brucite and serpentine includes the following steps: Step 1: Grinding: The raw brucite ore is crushed and ball-milled to obtain brucite ore powder. Step 2: Prepare the paste: Mix the raw magnesia ore powder with deionized water and put it into the flotation equipment. The solid-liquid ratio of the slurry is 1:(8-10). Stir the mixture to make the ore sample fully mixed. Add a pH adjuster to adjust the pH value of the slurry to a stable value to obtain the raw ore slurry. Step 3: Direct flotation separation of brucite and serpentine: Add PCE-11 modifier to the raw ore slurry obtained in step 2 and stir. After the PCE-11 modifier is fully dispersed and reacted, add sodium oleate collector and continue stirring until the reaction is complete. Start flotation froth removal to obtain the final flotation froth concentrate and tailings in the tank. Step 4: Processing the flotation product: The final flotation foam product is dried to obtain the final product, brucite concentrate.
2. Use of PCE-11 as a regulator in the flotation separation of brucite from serpentine according to claim 1, characterized in that, In step 1, the mass of brucite ore powder with a particle size of <74μm accounts for 70-90% of the total mass of brucite.
3. Use of PCE-11 as claimed in claim 1 as a regulator in the flotation separation of brucite from serpentine, characterized in that, The flotation equipment in step 2 is a hanging tank flotation machine with an impeller speed of 1800 rpm to 2100 rpm.
4. Use of PCE-11 as claimed in claim 1 as a regulator in the flotation separation of brucite from serpentine, characterized in that, The pH adjustment process in step 2 is carried out at room temperature, and the pH value is adjusted to 10-12; the pH adjuster is a NaOH solution with a mass fraction of 1%-5%.
5. Use of PCE-11 as claimed in claim 1 as a regulator in the flotation separation of brucite from serpentine, characterized in that, In step 3, the modifier PCE-11 is added in the form of a PCE-11 solution; the mass concentration of the PCE-11 solution is 10.0 to 15.0 g / L, and the amount of PCE-11 added is 400 to 700 mg / L.
6. Use of PCE-11 as claimed in claim 1 as a regulator in the flotation separation of brucite from serpentine, characterized in that, In step 3, the collector sodium oleate is added in the form of a sodium oleate solution with a mass concentration of 3.0–5.0 g / L and an addition amount of 400–700 mg / L.
7. Use of PCE-11 as claimed in claim 6 as a regulator in the flotation separation of brucite from serpentine, characterized in that, The sodium oleate solution is prepared by weighing sodium oleate solid powder and adding it to deionized water, stirring at 50-70°C until the sodium oleate solid powder is completely dissolved to obtain an aqueous solution of sodium oleate.