Application of sodium dodecyl amino propionate in flotation separation of new magnetite and quartz
By using sodium dodecylaminopropionate as a collector, the flotation separation effect of new magnetite and quartz is improved, the problem of poor selectivity in the existing technology is solved, and the production of high-grade iron ore concentrate is achieved.
Patent Information
- Application Number
- CN202511189000.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-25
- Publication Date
- 2025-10-14
AI Technical Summary
Existing magnetite collectors have poor selectivity in separating newly formed magnetite from quartz, and are not suitable for newly formed magnetite, which results in quartz minerals being entrained and making it difficult to obtain high-grade iron concentrate.
Sodium dodecylaminopropionate is used as a collector to improve its low-temperature solubility and foaming performance, utilize the electron induction effect of amino and carboxyl groups, and improve the selectivity of the agent for flotation separation of new magnetite and quartz.
The flotation effect is improved, the selective separation ability of new magnetite and quartz is enhanced, the process is simplified, and it is easy to apply in industry.
Smart Images

Figure BDA0005563127350000011 
Figure BDA0005563127350000061
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of iron ore flotation separation, and particularly relates to application of sodium dodecylaminopropionate in flotation separation of newly formed magnetite and quartz. BACKGROUND
[0002] As a basic raw material for the steel industry, iron ore resources are crucial to the national economy. Among them, hematite, as the most important type of iron ore, is often associated with quartz. With the continuous development of mineral resources, iron ore presents the characteristics of "poor, fine and complex", and for the refractory hematite, research in recent years shows that it can be converted into magnetite by multi-stage suspension magnetization roasting, and then enriched and recovered by magnetic separation technology. However, due to the strong magnetic attraction between magnetite particles with strong magnetism in the magnetic separation process, and the sensitivity of fine particles to electrostatic force and van der Waals force, part of the quartz minerals are still wrapped and entrained into the magnetic separation concentrate. Therefore, in order to obtain high-grade iron concentrate products, the iron ore and quartz after magnetic separation must be further separated. At this link, flotation technology has been proven to be an effective means to achieve efficient separation of newly formed magnetite and quartz.
[0003] At present, the main magnetite flotation collectors are amine collectors and fatty acid collectors. The selectivity of amine collectors is poor because they are mainly adsorbed on minerals through electrostatic interaction or hydrogen bond interaction. The solubility of fatty acid collectors at low temperature is poor, and quartz is easily activated by unavoidable ions, thereby reducing the selectivity of flotation. In addition, there are great differences in the physical and chemical properties of newly formed magnetite generated after magnetization roasting of hematite and natural magnetite, and the existing magnetite collectors are not suitable for the newly formed magnetite system. Therefore, it is necessary to develop a collector suitable for the flotation separation of newly formed magnetite and quartz. SUMMARY
[0004] In view of the above technical problems, the application provides application of sodium dodecylaminopropionate in flotation separation of newly formed magnetite and quartz.
[0005] To achieve the above purpose, the application provides the following technical scheme:
[0006] One of the purposes of the application is to provide application of sodium dodecylaminopropionate in flotation separation of newly formed magnetite and quartz, and the sodium dodecylaminopropionate is used as a collector for flotation separation of newly formed magnetite and quartz. The structural formula of the sodium dodecylaminopropionate is:
[0007]
[0008] The application aims at the deficiencies of existing magnetite collectors and the technical blank of new-born magnetite flotation reagents, and proposes the application of sodium dodecylaminopropionate in the flotation separation of new-born magnetite and quartz, the amino structure of sodium dodecylaminopropionate can effectively improve the low-temperature solubility and foam performance of fatty acid reagents, the amino group at a specific position can produce electronic induction effect with carboxyl group, thereby effectively changing the chemical activity of carboxyl group and enhancing the selectivity of the reagent, and when the reagent is used for the flotation separation of new-born magnetite and quartz, the flotation effect can be effectively improved. In addition, the collector has the characteristics of wide raw material source, good foam performance, high low-temperature solubility and good selectivity, and can effectively improve the iron grade of the roasted hematite magnetic separation concentrate, which has important significance for producing high-quality iron concentrate.
[0009] Further, the new-born magnetite is a magnetic separation concentrate obtained by magnetic separation of roasted hematite, and the specific steps are as follows: reducing roasting and magnetic separation of hematite to obtain the new-born magnetite.
[0010] Further, the Fe grade of the new-born magnetite is 50-65%, the SiO2 grade is less than 20%, and the component with a particle size of less than 0.074 mm accounts for 70-90% of the total mass.
[0011] The second object of the application is to provide a flotation separation method, which comprises the following steps:
[0012] The sodium dodecylaminopropionate is prepared into an aqueous solution to obtain a collector;
[0013] The new-born magnetite is mixed with water to obtain a slurry, the pH of the slurry is adjusted to 3-12, an activator is added, and finally the collector is added for flotation and bubble scraping.
[0014] Further, the mass concentration of the slurry is 20-35wt%; the mass concentration of the collector is 0.5-1wt%; and the activator is a CaCl2 solution with a mass concentration of 1-2wt%.
[0015] Further, the addition amount of the activator in the slurry is 200-300g / t, and the addition amount of the collector in the slurry is 800-1200g / t.
[0016] Further, the specific operation steps for adjusting the pH of the slurry to 3-12 are as follows: adding an HCl solution with a mass concentration of 0.2-3% or a NaOH solution with a mass concentration of 0.2-3% to the slurry to adjust the pH of the slurry to 3-12, and the slurry adjusting time is 2-3min.
[0017] Further, the addition time of the activator is 3-5min, the addition time of the collector is 3-5min, and the flotation and bubble scraping time is 3-5min.
[0018] Further, the flotation is carried out at 10-25 DEG C, and the flotation mode is positive flotation, and after the flotation, a froth product and a tank product are obtained.
[0019] Further, the flotation further comprises a post-treatment step of the froth product after the froth scraping, and the specific operation of the post-treatment is: drying the froth product to obtain an iron concentrate.
[0020] Compared with the prior art, the present application has the following advantages and technical effects:
[0021] (1) The newly generated magnetite after roasting of natural magnetite and hematite has differences in surface roughness, charging characteristics, contact angle and other properties, and the present application is specially aimed at the characteristics of the newly generated magnetite, and sodium dodecylaminopropionate is used as a collector for the flotation separation of the newly generated magnetite and quartz, which has high selectivity, and the flotation process is short and easy to be industrialized.
[0022] (2) The collector of the present application has the advantages of simple synthesis, good low-temperature resistance and strong selectivity compared with the current magnetite collector. DETAILED DESCRIPTION
[0023] The various exemplary embodiments of the present application will now be described in detail, which should not be considered as limiting the present application, but should be understood as a more detailed description of certain aspects, characteristics and embodiments of the present application.
[0024] It should be understood that the terms described in the present application are only for describing the specific embodiments, and are not used to limit the present application. In addition, for the numerical range in the present application, it should be understood that each intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Each smaller range between any stated value or stated range and any other stated value or intermediate value within the stated range is also included in the present application. The upper limit and the lower limit of these smaller ranges can be independently included or excluded from the range.
[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which the present application pertains. Although preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present application. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials in connection with which the documents are concerned. In the case of conflict, the content of this specification will control.
[0026] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from the description of the invention. The description and examples are intended to be illustrative only.
[0027] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.
[0028] An embodiment of the present invention provides an application of sodium dodecylaminopropionate in the flotation separation of newly formed magnetite and quartz. The sodium dodecylaminopropionate is used as a collector for the flotation separation of newly formed magnetite and quartz, and specifically comprises the following steps:
[0029] 1) preparing the sodium laurylaminopropionate into an aqueous solution to obtain a collector;
[0030] 2) Mixing the newly formed magnetite with water to obtain a pulp, adjusting the pH of the pulp to 3-12, adding an activator, and finally adding the collector to perform flotation and scraping.
[0031] In the following optional embodiments of the present invention, in step 1), the mass concentration of the collector is 0.5-1 wt %. As an example, in the following preferred embodiments of the present invention, the mass concentration of the collector is 0.5 wt % or 1 wt %.
[0032] In the following optional embodiments of the present invention, in step 2), the mass concentration of the slurry is 20-35 wt %. As an example, in the following preferred embodiments of the present invention, the mass concentration of the slurry is 25 wt % or 35 wt %.
[0033] In the following optional embodiments of the present invention, in step 2), the activator is a CaCl2 solution having a mass concentration of 1-2wt%. As an example, in the following preferred embodiments of the present invention, the mass concentration of the CaCl2 solution is 1wt% or 2wt%.
[0034] In the following optional embodiment of the present invention, in step 2), the newly formed magnetite is a magnetic concentrate obtained by magnetic separation of roasted hematite, and the specific steps are: reducing roasting and magnetic separation of hematite to obtain the newly formed magnetite. The newly formed magnetite has an Fe grade of 50-65% (e.g., 56wt% or 60wt%), an SiO2 grade of less than 20% (e.g., 10.4wt% or 12.02wt%), and components with a particle size of less than 0.074mm account for 70-90% (e.g., 85%) of the total mass.
[0035] In the following optional embodiment of the present application, the amount of the activator added in the slurry in step 2) is 200-300 g / t. As an example, in the following preferred embodiment of the present application, the amount of the activator added in the slurry is 200 g / t or 250 g / t.
[0036] In the following optional embodiment of the present application, the amount of the activator added in the slurry in step 2) is 200-300 g / t. As an example, in the following preferred embodiment of the present application, the amount of the activator added in the slurry is 200 g / t or 250 g / t.
[0037] In the following optional embodiment of the present application, the specific operation step of adjusting the pH of the slurry to 3-12 in step 2) is adding HCl solution with a mass concentration of 0.2-3% (such as 1%) or NaOH solution with a mass concentration of 0.2-3% (such as 1%) to the slurry to adjust the pH of the slurry to 3-12 (such as 10 or 11), and the slurry adjusting time is 2-3 min (such as 2 min or 3 min).
[0038] In the following optional embodiment of the present application, the addition time of the activator in step 2) is 3-5 min. As an example, in the following preferred embodiment of the present application, the addition time of the activator is 3 min or 4 min.
[0039] In the following optional embodiment of the present application, the addition time of the activator in step 2) is 3-5 min. As an example, in the following preferred embodiment of the present application, the addition time of the activator is 3 min or 4 min.
[0040] In the following optional embodiment of the present application, the scraping time of the flotation in step 2) is 3-5 min. As an example, in the following preferred embodiment of the present application, the scraping time of the flotation is 4 min or 5 min.
[0041] In the following optional embodiment of the present application, the flotation in step 2) is carried out at 10-25℃ (such as 15℃ or 20℃), and the flotation mode is positive flotation, and the foam product and the in-tank product are obtained after the flotation.
[0042] In the following optional embodiment of the present application, the flotation in step 2) is carried out at 10-25℃ (such as 15℃ or 20℃), and the flotation mode is positive flotation, and the foam product and the in-tank product are obtained after the flotation.
[0043] In the present application, "room temperature" refers to 20-25℃ unless otherwise specified.
[0044] In the present application, all raw materials are purchased from the market.
[0045] The technical solutions of the present application are further described below through examples.
[0046] Example 1
[0047] A flotation separation method, the steps are as follows:
[0048] (1) Preparation of new magnetite: hematite is reduced roasting in hydrogen at 500℃ for 30 min, and magnetic separation is carried out under a magnetic field intensity of 1000OE, and the chemical composition of the obtained new magnetite is: Fe content is 56wt%, SiO2 content is 12.02wt%, Al2O3 content is 3.15wt%, CaO content is 0.40wt%, MgO content is 0.76wt%, and the component with particle size less than 0.074mm in the new magnetite accounts for 85% by mass;
[0049] (2) Preparation of activator: analytical pure CaCl2 is mixed with water at a mass ratio of 1:100 at room temperature, stirred at a speed of 800r / min for 5min, and a 1wt% activator is obtained;
[0050] (3) Preparation of collector: sodium dodecylaminopropionate is mixed with water at a mass ratio of 1:100 at room temperature, stirred at a speed of 800r / min for 5min, and a 1wt% collector is obtained;
[0051] (4) Slurry preparation and flotation: the new magnetite obtained in step (1) is mixed with water to prepare a slurry with a mass concentration of 30wt%, then 1wt% HCl solution is added to adjust the pH of the slurry to 3, the slurry preparation time is 2min, then the activator of step (2) and the collector of step (3) are added to the slurry in turn, the addition amount is 250g / t and 1000g / t respectively, and the dosing time is 3min, then the aeration is started, and the flotation is carried out at 20℃ for 5min to obtain the flotation foam product and the product in the tank (quartz and other gangue minerals in the tank);
[0052] (5) Post-treatment of foam product: the foam product obtained in step (4) is dried to obtain an iron concentrate with Fe grade of 61% and SiO2 grade of 1.2%, and the recovery rate of the iron concentrate is 90%.
[0053] Example 2
[0054] A flotation separation method, the steps are as follows:
[0055] (1) Preparation of the new-born magnetite: hematite was reduced at 500℃ in hydrogen for 30 min, and then was subjected to magnetic separation at a magnetic field intensity of 1000 Oe, to obtain a new-born magnetite with a chemical composition of Fe content of 60wt%, SiO2 content of 10.4wt%, Al2O3 content of 2.11wt%, CaO content of 0.7wt%, and MgO content of 0.2wt%, and the component with particle size less than 0.074 mm accounted for 85% by mass;
[0056] (2) Preparation of the activator: analytical pure CaCl2 was mixed with water at a mass ratio of 2:100 at room temperature, and was stirred at a rotation speed of 1000 r / min for 5 min, to obtain an activator with a mass concentration of 2wt%;
[0057] (3) Preparation of the collector: sodium dodecylaminopropionate was mixed with water at a mass ratio of 0.5:100 at room temperature, and was stirred at a rotation speed of 1000 r / min for 5 min, to obtain a collector with a mass concentration of 0.5wt%;
[0058] (4) Slurry preparation and flotation: the new-born magnetite obtained in step (1) was mixed with water to prepare a slurry with a mass concentration of 25wt%, then NaOH solution with a mass concentration of 1wt% was added to the slurry to adjust the pH of the slurry to 10, and the slurry preparation time was 3 min, then the activator of step (2) and the collector of step (3) were added to the slurry in sequence, and the addition amounts were 200 g / t and 800 g / t respectively, and the dosing time was 4 min, then the aeration was started, and the flotation was carried out at 15℃ for 4 min to obtain the flotation froth product and the tank product;
[0059] (5) Post-treatment of the froth product: the froth product obtained in step (4) was dried to obtain an iron concentrate with Fe grade of 67% and SiO2 grade of 0.5%, and the recovery rate of the iron concentrate was 85%.
[0060] Comparative Example 1
[0061] The same as Example 2, except that the sodium dodecylaminopropionate of step (3) was replaced by an amino and carboxyl containing fatty acid type collector α-n-hexylaminododecanoic acid with the following structure:
[0062]
[0063] The comparative example obtained an iron concentrate with Fe grade of 60% and SiO2 grade of 9.82%, and the recovery rate of the iron concentrate was 92%. It can be found that the collector used in the comparative example has strong collecting ability for quartz as well, and cannot realize the separation of the new-born magnetite and quartz.
[0064] Comparative Example 2
[0065] A flotation separation method, the steps are as follows:
[0066] (1) Preparation of new magnetite: hematite monomineral is reduced roasting in hydrogen at 500℃ for 30min, and the obtained new magnetite monomineral has Fe3O4 content of more than 90%;
[0067] (2) Preparation of collector: sodium oleate is configured into a sodium oleate solution with a concentration of 4×10 -2 mol / L;
[0068] (3) Slurry preparation and flotation: the new magnetite obtained in step (1) is mixed with water to prepare a slurry with a mass concentration of 5wt%, then 1wt% NaOH solution is added to the slurry to adjust the pH of the slurry to 9, the slurry preparation time is 3min, then the collector of step (3) is added to the slurry, the amount of addition is 0.5mL (the concentration of sodium oleate is about 5×10 -4 mol / L), and the addition time is 3min, and the flotation is carried out at 15℃ for 3min to obtain a flotation froth product and a tank product;
[0069] (4) Post-treatment of froth product: the froth product obtained in step (3) is dried.
[0070] Comparative Example 3
[0071] A flotation separation method, the steps are as follows:
[0072] (1) Natural magnetite: Fe3O4 content of more than 90%;
[0073] (2) Preparation of collector: sodium oleate is configured into a sodium oleate solution with a concentration of 4×10 -2 mol / L;
[0074] (3) Slurry preparation and flotation: the natural magnetite of step (1) is mixed with water to prepare a slurry with a mass concentration of 5wt%, then 1wt% NaOH solution is added to the slurry to adjust the pH of the slurry to 9, the slurry preparation time is 3min, then the collector of step (3) is added to the slurry, the amount of addition is 0.5mL (the concentration of sodium oleate is about 5×10 -4 mol / L), and the addition time is 3min, and the flotation is carried out at 15℃ for 3min to obtain a flotation froth product and a tank product;
[0075] (4) Post-treatment of froth product: the froth product obtained in step (3) is dried.
[0076] Comparative Example 2 and Comparative Example 3 are compared, the concentration of sodium oleate is 5×10 -4When the concentration of the butyl xanthate is 0.5 mol / L, the recovery rate of the natural magnetite in Comparative Example 3 can reach 95%, while the roasted newly-born magnetite in Comparative Example 2 is hardly floated, which indicates that the physical and chemical properties of the natural magnetite and the roasted newly-born magnetite have great difference, and the indexes of the natural magnetite and the roasted newly-born magnetite are greatly different when floated by the same flotation reagent.
[0077] The above merely provides the preferred embodiments of the present application, but the protection scope of the present application is not limited thereto, and any person skilled in the art can easily think of the changes or replacements within the technical scope disclosed by the present application, which should be covered within the protection scope of the present application. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.
Claims
1. Application of sodium laurylaminopropionate in flotation separation of newborn magnetite and quartz, characterized in that: The sodium dodecylaminopropionate is used as a collector for flotation separation of newborn magnetite and quartz.
2. The use according to claim 1, characterized in that The new magnetite is a magnetic concentrate obtained by magnetic separation of roasted hematite.
3. The use according to claim 1, characterized in that The Fe grade of the newly formed magnetite is 50-65%, the SiO2 grade is less than 20%, and the components with a particle size less than 0.074 mm account for 70-90% of the total mass.
4. A flotation separation method, characterized in that: The following steps are involved: Sodium laurylaminopropionate is prepared into an aqueous solution to obtain a collector; The newly formed magnetite is mixed with water to obtain slurry, the pH of the slurry is adjusted to 3-12, an activator is added, and finally the collector is added to perform flotation and foam scraping.
5. The flotation separation method according to claim 4, characterized in that: The mass concentration of the slurry is 20-35wt%; and / or, The mass concentration of the collector is 0.5-1wt%; and / or, The activator is a CaCl2 solution with a mass concentration of 1-2wt%.
6. The flotation separation method according to claim 4, characterized in that: The amount of the activator added to the slurry is 200-300 g / t; and / or, The amount of the collector added to the ore pulp is 800-1200 g / t.
7. The flotation separation method according to claim 4, characterized in that: The specific operation steps of adjusting the pH of the ore pulp to 3-12 are: adding HCl solution with a mass concentration of 0.2-3% or NaOH solution with a mass concentration of 0.2-3% to the ore pulp to adjust the pH of the ore pulp to 3-12, and the slurry adjustment time is 2-3 minutes.
8. The flotation separation method according to claim 4, characterized in that: The activator is added for 3-5 minutes; and / or, The collector is added for 3-5 minutes; and / or The flotation scraping time is 3-5 minutes.
9. The flotation separation method according to claim 4, characterized in that: The flotation is carried out at 10-25° C., and the flotation method is positive flotation. After flotation, a foam product and an in-tank product are obtained.
10. The flotation separation method according to claim 4, characterized in that: The flotation process also includes a post-processing step for the foam product after foam scraping, and the specific operation is: drying the foam product to obtain iron concentrate.