Collecting agent, flotation reagent and method for flotation of ilmenite

Abstract

The invention belongs to the field of flotation, and particularly relates to a collecting agent for flotation of ilmenite, which comprises a collecting agent a with a formula 1 # imgabs 0 # structure and / or a collecting agent b with a formula 2 # imgabs 1 # structure, r1 is alkyl of C1 to C10, and R2 is alkyl of H and C1 to C10; r < 3 > is an alkyl group of C < 1 > to C < 10 >; ma and Mb are independently H, Na, K or NH4. The collecting agent a and / or the collecting agent b are / is adopted as the collecting agent of the ilmenite, excellent collecting selectivity is achieved, titanium in the ilmenite can be targeted efficiently and highly selectively, and then the collecting capacity and selectivity of the ilmenite are improved. Moreover, the collecting agent can accidentally meet the flotation requirements of the micro-fine-particle ilmenite, and excellent titanium collecting capacity and selectivity can still be obtained in the flotation process of the micro-fine-particle ilmenite.

Description

Technical Field

[0001] The invention belongs to the flotation reagent technology in the field of mineral processing, and in particular relates to the flotation field of ilmenite. Background Art

[0002] With the increasing depletion of high-grade ilmenite resources, the currently available ilmenite ore tends to be "poor, fine, and mixed", and the difficulty of development is gradually increasing. Therefore, the mineral separation process relies more on fine grinding to achieve sufficient monomer dissociation of the mineral. However, as the mineral particles become finer, the floatability of fine-grained ilmenite (mineral particles of -38μm particle size) also deteriorates, resulting in a weakening of the effect of commonly used flotation collectors and a decrease in metal recovery rate. This not only leads to a large amount of resource waste, but also causes fine-grained ilmenite to enter the external environment with the tailings, which has an adverse impact on ecological protection. Therefore, improving the metal recovery rate of fine-grained ilmenite has become a problem that needs to be solved urgently.

[0003] In order to improve the metal recovery rate of fine-grained ilmenite, the key is to improve the collection effect of flotation collector on fine-grained ilmenite. Therefore, developing new and efficient flotation collectors to reduce production costs and improve economic benefits is an important direction for improving the metal recovery rate of fine-grained ilmenite. Fatty acid collectors are commonly used flotation collectors for ilmenite, such as oleic acid and its salt compounds. In recent years, a large number of studies on hydroxamic acid and alkylphosphonic acid collectors have also been carried out. For example, the Chinese patent document with publication number CN117732601A discloses a flotation agent combination of a short-chain fatty acid, phosphoric acid, and hydroxamic acid. The Chinese patent document with publication number CN117463510A discloses a scheme for flotation of fine-grained ilmenite using fatty acids. However, the collection ability of the above-mentioned agents for fine-grained ilmenite is still unsatisfactory, and there is a lack of exclusive collectors for fine-grained refractory ilmenite.

[0004] In summary, there is a lack of efficient and highly selective collectors in the current flotation process of "poor, fine and mixed" ilmenite. If conventional fatty acid collectors continue to be used, it will lead to problems such as low utilization of ilmenite metal resources and poor environmental protection. Summary of the invention

[0005] In view of the problem that the existing collectors have insufficient collection capacity for ilmenite, especially fine-grained ilmenite, and it is difficult to achieve a high flotation recovery rate, the present invention provides a collector for flotation ilmenite, aiming to improve the collection and selectivity of ilmenite and make it suitable for the recovery rate requirements of ilmenite, especially fine-grained ilmenite flotation.

[0006] The second object of the present invention is to provide a flotation reagent comprising the collector for flotation of ilmenite.

[0007] The third object of the present invention is to provide a method for flotation of ilmenite using the collector and a flotation reagent containing the collector.

[0008] High-grade ilmenite is easy to achieve efficient and selective flotation recovery, but because the surface of fine ilmenite has fewer adsorption sites that can effectively interact with reagents, the capture effect is greatly reduced, and the fine ilmenite and gangue minerals present a complex intergrowth structure, which ultimately leads to a significant increase in the difficulty of flotation. In response to this problem, the present invention proposes the following solutions:

[0009] A collector for flotation of ilmenite, comprising a collector a having a structure of Formula 1, and / or a collector b having a structure of Formula 2;

[0010]

[0011] The R1 is C1~C 10 Alkyl, R2 is H, C1~C 10 The alkyl group; wherein R3 is C1~C 10 The alkyl group;

[0012] The M a 、M b is H, Na, K or NH4 alone.

[0013] The innovative research of the present invention shows that the collector a and / or collector b used as collectors for ilmenite has excellent capture selectivity and can efficiently and selectively target titanium in ilmenite, thereby improving its capture capacity and selectivity. Moreover, the collector of the present invention can unexpectedly adapt to the flotation requirements of fine-grained ilmenite, and can still obtain excellent titanium capture capacity and selectivity during the flotation process of fine-grained ilmenite.

[0014] In the present invention, the collector for flotation of ilmenite comprises the collector a and the collector b, wherein the content of the collector a is above 10wt.%, preferably above 20wt.%, more preferably 10-80wt.%, more preferably 15-30wt.%, and most preferably 18-22wt.%. Studies have shown that at the preferred ratio, better synergy can be obtained, which helps to further enhance the titanium-iron separation effect and selectivity of fine-grained minerals.

[0015] The present invention shows that the combination of collector a and collector b can help further enhance the ilmenite capture capacity and titanium-iron separation selectivity based on the intramolecular and intermolecular synergy of collector a and b, especially for fine-grained ilmenite, which can also obtain excellent titanium capture performance and selectivity.

[0016] The present invention also provides a flotation reagent for flotation of ilmenite, which comprises the collector of the present invention.

[0017] The flotation agent for flotation of ilmenite described in the present invention may contain other flotation components allowed to be added in the industry, for example, it may also contain a flotation aid comprising at least one of a pH regulator, a frother, and the like.

[0018] In the present invention, the pH regulator can be a component known in the industry, for example, it can include at least one of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, and acetic acid. It should be noted that the selected pH regulator can not only achieve the pH control effect, but also play a certain role in inhibiting gangue.

[0019] The foaming agent includes, for example, 2 # At least one of oil, terpineol, methyl isobutyl carbinol, cresol oil, and polyethylene glycol ether.

[0020] In the present invention, the components of the flotation reagent exist independently of each other before use, or exist in the form of partial mixing or complete mixing. In addition, the dosage of each component can also be reasonably adjusted according to the flotation needs and efficiency.

[0021] The present invention also provides a method for flotation of ilmenite, which uses the collector as a collector to flotation the ilmenite to obtain ilmenite concentrate.

[0022] In the present invention, the ilmenite can be any form and grade of ilmenite to be selected, but considering that the collector described in the present invention still has excellent capture performance and selectivity for fine-grained minerals compared to the prior art, using it for fine-grained ilmenite may obtain better economic value than the prior art.

[0023] In the present invention, the ilmenite flotation ore is fine-grained ilmenite, and the mass proportion of -38μm fine particles is greater than 40%.

[0024] Preferably, the titanium grade (TiO2 content) of the ilmenite is below 21 wt.% (for example, it can be 20.0 wt.% to 21.0 wt.%, and further can be 20.5 to 20.7 wt.%).

[0025] In the present invention, the collector of the present invention can be used for the flotation of the ilmenite based on the existing conventional flotation equipment and ideas.

[0026] In the present invention, the amount of the collector used in the flotation stage can be adjusted as needed, for example, it can be 2000 to 3000 g / t, and further 2400 to 2600 g / t.

[0027] In the present invention, the ilmenite ore can be floated based on the flotation reagent of the present invention to obtain the ilmenite concentrate.

[0028] Furthermore, the flotation aid in the flotation reagent includes a pH regulator, wherein the amount of the pH regulator is 2000-2800 g / t, and further can be 2400-2600 g / t.

[0029] The flotation reagent may also contain a frother, and the amount thereof may be adjusted as required, for example, 10 to 400 g / t, or further 20 to 150 g / t.

[0030] In the present invention, an optional flotation method specifically includes a desulfurization flotation step and a flotation process of roughing the desulfurization flotation process, and further includes a two-stage concentration process of the roughing concentrate.

[0031] The reagents in the desulfurization process include a pH regulator, a xanthate collector and a foaming agent, wherein the dosage of the pH regulator can be 1000-1500 g / t; the dosage of the xanthate collector can be 200-300 g / t, and the dosage of the foaming agent can be 20-100 g / t.

[0032] In the roughing stage, the dosage of pH adjuster is 300-800 g / t, and further can be 400-600 g / t; the dosage of collector can be 1600-2200 g / t, and further can be 1700-1900 g / t.

[0033] The pH adjusting agent in the second concentration stage is 300-800 g / t, and can be further 400-600 g / t; the collecting agent is 100-500 g / t, and can be further 200-400 g / t.

[0034] Beneficial Effects

[0035] The research of the present invention shows that the compounds of the structure of Formula 1 and / or Formula 2 have excellent specific capture ability for ilmenite. Using them as collectors for ilmenite can effectively improve the capture rate and selectivity of ilmenite. In addition, combining Formula 1 and Formula 2 can further achieve the combined synergy between molecules, further enhance the flotation ability of ilmenite, and especially improve the flotation effect of fine-grained ilmenite. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] Figure 1 This is the flotation flow chart of Example 1. DETAILED DESCRIPTION

[0037] In the present invention, the compound of formula 1 is typically represented by formula 1-A, and its specific structure is:

[0038]

[0039] The compound of formula 2 is typically exemplified by formula 2-A, and its specific structure is:

[0040]

[0041] Comparative structural compounds, the specific structure is:

[0042]

[0043]

[0044] The mineral to be selected described in the present invention can be ilmenite of any grade. In order to further verify the collection ability of the collector of the present invention, the present invention particularly selects fine-grained ilmenite. For example, as an optional scheme, the fine-grained ilmenite selected below is the strong magnetic concentrate of the titanium beneficiation plant of Panzhihua Iron and Steel Group.

[0045] In the present invention, the collector of the present invention can be used to float the mineral based on conventional flotation means and principles. For example, as an optional embodiment, the flotation process can be as follows:

[0046] Example

[0047] The effect of the collector of the present invention was verified by using an open circuit flotation test process. Figure 1 This is the open circuit flotation flow chart. The steps are:

[0048] Step 1: Weigh 800 g of fine-grained ilmenite flotation ore (the mass proportion of -38 μm fine particles is greater than 40%, and the grade of TiO2 is 20.55±0.1wt.%).

[0049] Step 2: In the desulfurization flotation operation, the order of adding drugs is pH regulator sulfuric acid and sulfide ore collector xanthate. The dosage and slurry mixing time are as follows: Figure 1 After the addition of chemicals, desulfurization flotation was performed for 5 minutes to obtain sulfur concentrate.

[0050] Step 3: In the ilmenite flotation operation, the order of adding chemicals is pH regulator (such as sulfuric acid) and ilmenite collector (see the following cases), and the dosage and slurry mixing time are as follows: Figure 1 After the addition of chemicals, four products, namely, titanium concentrate, middlings 1, middlings 2 and tailings, were obtained by open-circuit flotation of ilmenite through 5-minute roughing, 5-minute concentrating I and 5-minute concentrating Ⅰ.

[0051] Step 4, results and analysis. Each group of open circuit flotation tests was repeated multiple times, and the results of the embodiment are the average values ​​of the various items repeated 3-5 times. Except for using different collectors in each implementation case, other conditions are completely the same, such as reagent dosage, temperature, slurry mixing and flotation time. Referring to the TiO2 grade / recovery rate of the titanium concentrate obtained in the two groups of experiments, the collection effect of the collector of the present invention is compared.

[0052] In the above Figure 1 Based on the flotation of the samples, the collectors and conditions of each case were adjusted. The steps and results were as follows:

[0053] Example 1 - Single Collector Solution

[0054] The collector is a single collector, and the experimental groups are:

[0055] Group A: The collector is of formula 1-A;

[0056] Group B: The collector is Formula 2-A;

[0057] Comparative group a: the collector is formula 3-A;

[0058] Comparative group b: the collector is formula 4-A;

[0059] Comparative group c: the collector is formula 5-A;

[0060] Comparative group d: the collector is sodium oleate;

[0061] The results of each group are shown in Table 1:

[0062] Table 1

[0063]

[0064]

[0065] It can be seen from Example 1 that the use of Formula 1-A and Formula 2-A described in the present invention as collectors can adapt to the characteristics of fine-grained ilmenite and obtain a more ideal collection effect.

[0066] Example 2 - Binary Collector Solution

[0067] The collector is a binary composite collector, and the experimental groups are:

[0068] Group A: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:1;

[0069] Group B: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:2;

[0070] Group C: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 2:1;

[0071] Comparative group a: the collectors are Formula 1-A and Formula 4-A in a weight ratio of 1:1;

[0072] Comparative group b: the collectors are Formula 2-A and Formula 3-A in a weight ratio of 1:1;

[0073] The results of each group are shown in Table 2:

[0074] Table 2

[0075]

[0076]

[0077] It can be seen from Examples 1 and 2 that the combination of Formula 1 and Formula 2 can further enhance the synergy, and the formula of Group B (Formula 1-A and Formula 2-A with a weight ratio of 1:2) has the best flotation effect, can better adapt to the characteristics of fine-grained ilmenite, and can obtain a more ideal capture effect.

[0078] Example 3-Binary Collector Formula Optimization Scheme

[0079] The case of combined collector ratio adjustment, the experimental groups are:

[0080] Group A: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:3;

[0081] Group B: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:4;

[0082] Group C: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:5;

[0083] Group D: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:6;

[0084] The results of each group are shown in Table 3:

[0085] Table 3

[0086]

[0087]

[0088] It can be seen from Examples 1 to 3 that optimizing the compounding ratio of Formula 1 and Formula 2 can further enhance the synergy and further improve the collection effect of fine-grained ilmenite. The best collector formula obtained is Formula 1-A and Formula 2-A with a weight ratio of 1:4.

[0089] Example 4

[0090] Compared with the group B of Example 3, the only difference is that the amount of the collector is changed. The experimental groups are:

[0091] Group A: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:4, and the dosages of the collectors for roughing, concentrating I and concentrating Ⅰ are 1600 g / t, 300 g / t and 300 g / t respectively;

[0092] Group B: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:4, and the dosages of the collectors in roughing, concentrating I and concentrating Ⅰ are 2000 g / t, 300 g / t and 300 g / t respectively;

[0093] Group C: The collectors are Formula 1-A and Formula 2-A in a weight ratio of 1:4, and the dosages of the collectors in roughing, concentrating I and concentrating Ⅰ are 2200 g / t, 300 g / t and 300 g / t respectively;

[0094] The results of each group are shown in Table 4:

[0095] Table 4

[0096]

[0097] It can be seen from Examples 3 and 4 that the combination of Formula 1 and Formula 2 still has an excellent collection effect on fine-grained ilmenite even at a lower collector dosage, and when the collector dosage is high, more gangue will be mixed into the flotation concentrate, reducing its selectivity, resulting in a lower grade of titanium concentrate and a lower metal recovery rate. Therefore, the optimal collector dosage is 1800 g / t, 300 g / t and 300 g / t for roughing, concentrating I and concentrating Ⅰ, respectively.

Claims

1. A collector for flotation of ilmenite, characterized in that: Containing a collector a having a structure of Formula 1, and / or a collector b having a structure of Formula 2; The R1 is C1~C 10 Alkyl, R2 is H, C1~C 10 The alkyl group; wherein R3 is C1~C 10 The alkyl group; The M a 、M b is solely H, Na, K or NH4.

2. The collector for flotation of ilmenite according to claim 1, characterized in that: The invention comprises the collector a and the collector b, wherein the content of the collector a is above 10wt.%, preferably above 20wt.%, more preferably 10-80wt.%, further preferably 15-30wt.%, and most preferably 18-22wt.%.

3. A flotation agent for flotation of ilmenite, characterized in that: Contains the collector according to claim 1 or 2.

4. The flotation reagent for flotation of ilmenite according to claim 3, characterized in that: The invention also comprises a flotation aid comprising at least one of a pH adjuster and a frother.

5. The flotation agent for flotation of ilmenite according to claim 4, characterized in that: The pH adjuster includes at least one of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and acetic acid; The foaming agent comprises 2 # At least one of oil, terpineol, methyl isobutyl carbinol, cresol oil, and polyethylene glycol ether.

6. A method for flotation of ilmenite, characterized in that: The collector according to claim 1 or 2 is used as a collector to flotate the ilmenite ore to obtain the ilmenite concentrate.

7. The method according to claim 6, characterized in that The ilmenite flotation ore is micro-particle ilmenite, and the mass proportion of -38μm micro-particles is greater than 40%.

8. The method according to claim 6 or 7, characterized in that The amount of collector used in the flotation stage is 2000-3000 g / t, further 2400-2600 g / t.

9. The method according to any one of claims 6 to 8, characterized in that: The ilmenite ore is floated by using the flotation reagent described in any one of claims 3 to 5 to obtain the ilmenite ore concentrate.

10. The method according to claim 9, characterized in that The flotation agent is the flotation agent according to claim 4 or 5, and the flotation aid comprises a pH regulator, and the dosage of the pH regulator is 2000-2800 g / t, and can further be 2400-2600 g / t.

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