Preparation method of ilmenite flotation collector and application thereof
Patent Information
- Application Number
- CN202411118192.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-15
- Publication Date
- 2026-10-09
- Estimated Expiration
- 2044-08-15
AI Technical Summary
但存在原料种类多,合成工序较为复杂的不足
1、亚油酸羟肟酸钠能与钛铁矿表面的铁、钛活性位点发生选择性螯合作用,增加了捕收剂对于钛铁矿的选择性;因烷基中的碳链长,其捕收能力强。钙羧酸经过高温皂化后具有较好的起泡性能和捕收能力,综合运用可减少捕收剂的用量,降低浮选药剂成本,具有广阔的工业化前景。
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Figure CN118831725B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of mineral processing technology, and particularly relates to a method for preparing an ilmenite flotation collector and its application. Background Technology
[0002] Titanium, as a strategic metal, is widely used in environmental protection, medical equipment, aerospace, transportation, and military fields due to its superior and unique corrosion resistance and coating properties. Effective separation of ilmenite is crucial for converting titanium ore into high-value-added products. Flotation is the most widely used beneficiation process for ilmenite separation, and the selection of surface chemistry and flotation reagents is extremely important. The versatility of this process depends on the correct use of flotation reagents, which are added to the pulp to induce differences in wettability between ilmenite and other minerals in the ore. Collectors play a vital role in the flotation of ilmenite. Therefore, the research and application of collectors are of great significance for the efficient utilization of ilmenite.
[0003] The main types of collectors for ilmenite flotation include fatty acids, alkyl phosphates, styrene phosphonic acids, arsenic acids, and hydroxamic acids. Fatty acids are the most widely used collectors in ilmenite flotation, but commonly used fatty acid collectors have disadvantages such as poor selectivity, large dosage, and poor solubility and dispersibility at room temperature. Styrene phosphonic acids and alkyl phosphate collectors have complex synthesis, low yield, and high cost, hindering their application in industrial flotation. Arsenic acid exhibits significant selectivity and excellent performance in ilmenite flotation. However, due to its high toxicity, its industrial application has been prohibited. Hydroxamic acids are composed of carbon chains with -R and -CONHOH groups. In comparison, hydroxamic acid collectors exhibit higher flotation selectivity because the oxyxamic acid group (-CONHOH) can form stable hydrophobic chelates with iron and titanium metals. However, hydroxamic acid collectors generally suffer from low collecting capacity and weak antioxidant properties due to their short carbon chain (usually less than 10 carbon atoms). To improve the flotation efficiency of ilmenite, some mineral processing scientists have conducted extensive research on collector development. The invention patent application No. 201710942256.8, entitled "A Preparation Method and Application of an Ilmenite Flotation Collector," discloses a collector for ilmenite flotation synthesized using waste cooking oil, methanol, concentrated sulfuric acid, hydroxylamine hydrochloride, water, and sodium hydroxide as raw materials, achieving good beneficiation indicators in the separation of ilmenite ore containing pyrite. However, due to the complex composition of waste cooking oil, the stability and applicability of the final synthesized collector to ilmenite still need to be verified. The invention patent application No. 201610695809.X, entitled "An Ilmenite Flotation Collector and Its Preparation Method and Application," discloses a collector for ilmenite flotation synthesized from cottonseed oil, mixed fatty acids, triethylenetetramine hexamethylphosphonic acid, higher fatty acid hydroxyxamic acid, and strong alkali, achieving good beneficiation indicators. However, it suffers from drawbacks such as the large variety of raw materials and the relatively complex synthesis process. Therefore, the research and development of novel and efficient flotation collectors is of great significance for the development and utilization of ilmenite resources and the sustainable development of related industries. Summary of the Invention
[0004] To address the aforementioned technical problems, this invention proposes a method for preparing an ilmenite flotation collector and its application. This invention overcomes the shortcomings of existing collectors, improves the collection effect on minerals, reduces reagent costs, and is environmentally friendly.
[0005] To achieve the above objectives, the present invention provides the following technical solution: A flotation collector for ilmenite includes linoleic acid hydroxamic acid crystals added to its components; the linoleic acid hydroxamic acid crystals are made from hydroxylamine, methyl linoleate, sodium hydroxide, and hydrochloric acid.
[0006] Furthermore, the method for preparing the linoleic acid hydroxamic acid crystals includes the following steps: Hydroxylamine was prepared as a raw material to form an aqueous solution of hydroxylamine. Methyl linoleate was added dropwise to the aqueous solution of hydroxylamine. After the addition was completed, the mixture was stirred at 45-55°C for 2-3 hours to convert the ester group in the molecular structure of methyl linoleate into isohydroxamic acid. Continue to add hydroxylamine and sodium hydroxide to the system, and stir at 45-55℃ for 1-2 hours to fully convert methyl linoleate into sodium isohydroxamic acid salt; Hydrochloric acid was added to the system to convert sodium hydroxamic acid salt into hydroxamic acid crystal precipitate; the precipitate was then obtained by rotary evaporation.
[0007] Furthermore, the concentration of the hydroxylamine aqueous solution is 20-40 wt%; The molar ratio of hydroxylamine to methyl linoleate in the aqueous hydroxylamine solution is (1.5-3):1; The molar ratio of sodium hydroxide to methyl linoleate is (2-4):1; The molar ratio of hydroxylamine to methyl linoleate added in the second addition was (2-4):1; The molar ratio of hydrochloric acid to methyl linoleate is (1.5-3):1.
[0008] Furthermore, the raw materials of the ilmenite flotation collector include the following components in parts by mass: 25-35 parts of linoleic acid hydroxamic acid crystals, 5-10 parts of calcium carboxylic acid, 15-20 parts of sodium hydroxide, and 25-35 parts of water.
[0009] This invention also provides a method for preparing an ilmenite flotation collector, comprising the following steps: weighing linoleic acid hydroxamic acid crystals, calcium carboxylic acid, sodium hydroxide and water by mass, reacting at 140-180℃ for 1-3 hours to obtain a paste, which is the ilmenite flotation collector.
[0010] The technical principle of this invention is as follows: The ester group (-COOCH3) in the molecular structure of methyl linoleate is converted into hydroxamic acid (-CONHOH) through the reduction of hydroxylamine (NH2OH). Excess hydroxylamine and sodium hydroxide are added to fully convert methyl linoleate into sodium hydroxamic acid salt (-CONHONa). Hydrochloric acid (HCl) is added to promote the conversion of sodium hydroxamic acid salt into hydroxamic acid crystals. Finally, a saponification reaction is used to convert the hydroxamic acid crystals into sodium hydroxamic acid salt, while simultaneously converting the carboxylic acid (-COOH) and sulfonic acid (-SO3H) in the calcium carboxylic acid molecular structure into sodium carboxylate salt and sodium sulfonate salt, thus improving the solubility properties of the novel drug.
[0011] The synthesis route of the ilmenite flotation collector in this invention is as follows: The present invention also provides an application of the aforementioned ilmenite flotation collector in ilmenite flotation.
[0012] The present invention also provides a flotation method for ilmenite, comprising the following steps: grinding the raw ilmenite, adjusting the pulp pH to 8.0-9.5, using sodium hexametaphosphate and carboxymethyl cellulose (CMC) as inhibitors, using the ilmenite flotation collector as the collector, and performing a closed-circuit process of one roughing, one scavenging, three cleaning, and middlings return, to obtain tailings and concentrate respectively.
[0013] Furthermore, during the roughing process, the ilmenite flotation collector is added during the roughing, scavenging, and third cleaning processes, wherein the amount added during the roughing process is 1000 g / ton; the amount added during the scavenging process is 400 g / ton; and the amount added during the third cleaning process is 100 g / ton.
[0014] Furthermore, the inhibitor is added during the roughing process, the scavenging process, and the first cleaning process; wherein during the roughing process, the amount of sodium hexametaphosphate added is 200 g / ton; the amount of carboxymethyl cellulose added is 20 g / ton; and the amount added during the scavenging process and the first cleaning process is halved in turn.
[0015] Compared with the prior art, the present invention has the following advantages and technical effects: 1. Sodium hydroxamic acid can selectively chelate with the iron and titanium active sites on the surface of ilmenite, increasing the selectivity of the collector for ilmenite; due to the long carbon chain in the alkyl group, its collecting ability is strong. Calcium carboxylic acid, after high-temperature saponification, has good foaming properties and collecting ability. Its combined use can reduce the amount of collector used, lower the cost of flotation reagents, and has broad industrial application prospects.
[0016] 2. This flotation collector exhibits excellent dispersibility at room temperature, achieving superior flotation results. Compared to traditional sodium oleate and salicylhydroxyxamic acid collectors, it increases titanium concentrate grade by 1-2% and titanium recovery rate by 15-30%.
[0017] 3. The preparation process is simple and highly operable. There is no discharge of waste gas, wastewater, or solid waste in the production, preparation, and use stages, resulting in significant environmental benefits. Attached Figure Description
[0018] The accompanying drawings, which form part of this application, are used to provide a further understanding of this application. The illustrative embodiments and descriptions of this application are used to explain this application and do not constitute an undue limitation of this application. In the drawings: Figure 1 This is a process flow diagram of the collector prepared in this invention in the beneficiation of ilmenite. Detailed Implementation
[0019] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.
[0020] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.
[0021] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.
[0022] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be readily apparent to those skilled in the art. This specification and embodiments are merely exemplary.
[0023] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.
[0024] A method for preparing an ilmenite flotation collector includes the following steps: (1) Prepare an aqueous solution of hydroxylamine with a concentration of 20-40wt% in a three-necked flask equipped with an electric stirrer and a thermometer; add methyl linoleate dropwise to the aqueous solution of hydroxylamine, and control the molar ratio of methyl linoleate to hydroxylamine to be 1:(1.5-3), such as 1:2. After the addition is completed, stir at 45-55℃ for 2-3 hours. (2) Add hydroxylamine and sodium hydroxide to step (1), and control the molar ratio of hydroxylamine (the amount of hydroxylamine added in this step) to methyl linoleate to be (2-4):1 (e.g., 2:1, 3:1, 4:1), and control the molar ratio of sodium hydroxide to methyl linoleate to be (2-4):1 (e.g., 2:1, 3:1, 4:1), and stir at 45-55℃ for 1-2 hours; (3) Add hydrochloric acid to (2) and control the molar ratio of hydrochloric acid to methyl linoleate to be (1.5-3):1, such as 1.5:1, 2:1, 3:1. Use a spiral evaporator to crystallize it completely to obtain linoleic acid hydroxamic acid crystals. (4) Add linoleic acid hydroxamic acid crystals (25-35 parts), calcium carboxylic acid (5-10 parts), sodium hydroxide (15-20 parts) and water (25-35 parts) to a reaction vessel and react at 140-180℃ (such as 140℃, 160℃, 180℃) for 1-3 hours to obtain a paste, which is the ilmenite flotation collector.
[0025] A flotation method for ilmenite includes the following steps: grinding the raw ilmenite, adjusting the pulp pH to 8.0-9.5, using sodium hexametaphosphate and carboxymethyl cellulose (CMC) as depressants, and the ilmenite flotation collector as the collector, performing a closed-circuit process of one roughing, one scavenging, three cleaning, and middlings return, respectively, to obtain tailings and concentrate. The roughing, scavenging, and cleaning processes can be implemented using conventional methods in the art; specific operating parameters are not considered as criteria for evaluating the inventiveness of this invention and will not be elaborated further.
[0026] Unless otherwise specified, the term "parts" in this invention refers to parts by weight.
[0027] All raw materials used in this invention were purchased from the market.
[0028] The technical solution of the present invention will be further illustrated by the following embodiments.
[0029] Example 1 Preparation of flotation collector for ilmenite: (1) Prepare a 20wt% aqueous solution of hydroxylamine in a three-necked flask equipped with an electric stirrer and a thermometer. Add methyl linoleate dropwise to the solution, controlling the molar ratio of methyl linoleate to hydroxylamine to be 1:2. After the addition is complete, stir at 45°C for 2 hours. (2) Add hydroxylamine and sodium hydroxide to step (1), and control the molar ratio of hydroxylamine to methyl linoleate to be 2:1 and the molar ratio of sodium hydroxide to methyl linoleate to be 2:1. Stir at 45°C for 1 hour. (3) Add 0.5 mol / L hydrochloric acid to (2) and control the molar ratio of hydrochloric acid to methyl linoleate to be 1.5:1. Then use a spiral evaporator to crystallize it completely to obtain linoleic acid hydroxamic acid crystals. (4) Linoleic acid hydroxamic acid crystals (35 parts), calcium carboxylic acid (10 parts), sodium hydroxide (20 parts) and water (25 parts) are added to a reaction vessel and reacted at 140°C for 3 hours to obtain a paste, which is the ilmenite flotation collector.
[0030] Application Example 1 The ilmenite used in this application example is a raw ore from Panzhihua with a grade of 16.862% TiO2, 17.32% Fe, and 0.13% S. The main metallic mineral in the ore is ilmenite, with minor and trace amounts of hematite and pyrite; gangue minerals include pyroxene, dolomite, quartz, feldspar, and olivine.
[0031] A flotation method for ilmenite includes the following steps: The raw ilmenite is ground (85% of the particles are -0.074mm); the pulp pH is adjusted to 8.5 using sodium hydroxide solution; 200 g / ton sodium hexametaphosphate and 20 g / ton carboxymethyl cellulose are used as depressants; and 1000 g / ton of the prepared ilmenite flotation collector is used as the collector. One roughing and one scavenging process are then performed (after the roughing process, sodium hydroxide is used again to adjust the pulp pH to 8.5 in the roughing tailings, and 100 g / ton sodium hexametaphosphate is added). A closed-circuit process using 10 g / ton carboxymethyl cellulose and 400 g / ton ilmenite flotation collector, three cleaning steps (Cleansing I: after roughing, sodium hydroxide is used to adjust the pulp pH to 8.5 in the roughing concentrate, and 50 g / ton sodium hexametaphosphate and 5 g / ton carboxymethyl cellulose are added; Cleansing III: after Cleansing II, sodium hydroxide is used to adjust the pulp pH to 8.5, and 100 g / ton ilmenite flotation collector is added), and middlings are sequentially returned, yielding tailings and titanium concentrate respectively (see details for specific process). Figure 1 ).
[0032] Experimental results: Using the ilmenite flotation collector prepared in Example 1, according to... Figure 1 After separation using the flotation process and reagent preparation method, the titanium concentrate grade was 47.83%, and the titanium recovery rate was 86.12%. Compared with traditional sodium oleate and salicylic acid collectors (process and...), the titanium concentrate yield was significantly higher. Figure 1 Similarly, sodium oleate and salicylic acid replaced the new collectors respectively, increasing the titanium concentrate grade by 1.5% and 1.8%, and the titanium recovery rate by 16.2% and 24.5%.
[0033] Example 2 Preparation of flotation collector for ilmenite: (1) Prepare a 30wt% aqueous solution of hydroxylamine in a three-necked flask equipped with an electric stirrer and a thermometer. Add methyl linoleate dropwise to the solution, controlling the molar ratio of methyl linoleate to hydroxylamine to be 1:1.5. After the addition is complete, stir at 50°C for 3 hours. (2) Add hydroxylamine and sodium hydroxide to step (1), and control the molar ratio of hydroxylamine to methyl linoleate to be 3:1 and the molar ratio of sodium hydroxide to methyl linoleate to be 3:1. Stir at 50°C for 2 hours. (3) Add 0.5 mol / L hydrochloric acid to (2) and control the molar ratio of hydrochloric acid to methyl linoleate to be 2:1. Then use a spiral evaporator to crystallize it completely to obtain linoleic acid hydroxamic acid crystals. (4) Linoleic acid hydroxamic acid crystals (30 parts), calcium carboxylic acid (10 parts), sodium hydroxide (15 parts) and water (30 parts) are added to a reaction vessel and reacted at 160°C for 2 hours to obtain a paste, which is the ilmenite flotation collector.
[0034] Application Example 2 The ilmenite used in this application example is a raw ore from Yunnan Province with a grade of 18.32% TiO2, 19.92% Fe, and 0.08% S. The main metallic mineral in the ore is ilmenite, with minor and trace amounts of magnetite, hematite, and pyrite; gangue minerals include pyroxene, dolomite, quartz, feldspar, and olivine.
[0035] The flotation method for ilmenite is the same as in Application Example 1, except that the pH is always maintained at 8.0.
[0036] Experimental results: Using the ilmenite flotation collector prepared in Example 1, according to... Figure 1 After separation using the flotation process (pH=8.0) and reagent preparation method, the titanium concentrate grade was 48.23%, and the titanium recovery rate was 87.35%. Compared with traditional sodium oleate and salicylic acid collectors (process and...), the titanium concentrate yield was significantly higher. Figure 1 Similarly, sodium oleate and salicylic acid replaced the new collectors respectively, increasing the titanium concentrate grade by 1.1% and 1.9%, and the titanium recovery rate by 18.2% and 29.2%.
[0037] Example 3 Preparation of flotation collector for ilmenite: (1) Prepare a 40wt% aqueous solution of hydroxylamine in a three-necked flask equipped with an electric stirrer and a thermometer. Add methyl linoleate dropwise to the solution, controlling the molar ratio of methyl linoleate to hydroxylamine to be 1:3. After the addition is complete, stir at 55°C for 2 hours. (2) Add hydroxylamine and sodium hydroxide to step (1), and control the molar ratio of hydroxylamine to methyl linoleate to be 4:1 and the molar ratio of sodium hydroxide to methyl linoleate to be 4:1. Stir at 55°C for 2 hours. (3) Add 0.5 mol / L hydrochloric acid to (2) and control the molar ratio of hydrochloric acid to methyl linoleate to 3:1. Then use a spiral evaporator to crystallize it completely to obtain linoleic acid hydroxamic acid crystals. (4) Linoleic acid hydroxamic acid crystals (25 parts), calcium carboxylic acid (5 parts), sodium hydroxide (20 parts) and water (35 parts) are added to a reaction vessel and reacted at 180°C for 1 hour to obtain a paste, which is the ilmenite flotation collector.
[0038] Application Example 3 The ilmenite used in this application example is a raw ore from Yunnan Province with a grade of 15.42% TiO2, 14.32% Fe, and 0.12% S. The main metallic mineral in the ore is ilmenite, with minor and trace amounts of magnetite, hematite, and pyrite; gangue minerals include pyroxene, dolomite, quartz, feldspar, and olivine.
[0039] The flotation method for ilmenite is the same as in Application Example 1, except that the pH is always maintained at 9.0.
[0040] Experimental results: Using the ilmenite flotation collector prepared in Example 1, according to... Figure 1 After separation using the flotation process (pH=9.0) and reagent preparation method, the titanium concentrate grade was 47.03%, and the titanium recovery rate was 85.12%. Compared with traditional sodium oleate and salicylic acid collectors (process and...), the titanium concentrate yield was significantly higher. Figure 1 Similarly, sodium oleate and salicylic acid replaced the new collectors respectively, increasing the titanium concentrate grade by 1.5% and 1.7%, and the titanium recovery rate by 15.2% and 25.1%.
[0041] Comparative Example 1 Same as Example 1, except that in step (4), the content of linoleic acid hydroxamic acid crystals is adjusted to 20 parts.
[0042] The application example is the same as Application Example 1.
[0043] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process (pH=8.5) and reagent preparation method, the titanium concentrate grade was 47.23%, and the titanium recovery rate was 75.12%. This indicates that when the linoleic acid hydroxamic acid crystal content is below the specified range, compared with the flotation index of Example 1, the recovery rate of ilmenite is significantly lower, while the grade of ilmenite does not change much.
[0044] Comparative Example 2 Same as Example 1, except that in step (4), the content of linoleic acid hydroxamic acid crystals is adjusted to 45 parts.
[0045] The application example is the same as Application Example 1.
[0046] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process (pH=8.5) and reagent preparation method, the titanium concentrate grade was 45.23%, and the titanium recovery rate was 86.52%. This indicates that when the linoleic acid hydroxamic acid crystal content exceeds the specified range, compared with the flotation index of Example 1, the ilmenite grade decreases significantly, while the ilmenite recovery rate remains relatively unchanged.
[0047] Comparative Example 3 Same as Example 1, except that the calcium carboxylic acid content is adjusted to 20 parts in step (4).
[0048] The application example is the same as Application Example 1.
[0049] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process (pH=8.5) and reagent preparation method, the titanium concentrate grade was 45.13%, and the titanium recovery rate was 86.42%. This indicates that when the calcium carboxylic acid content exceeds the specified range, compared with the flotation index of Example 1, the grade of ilmenite decreased by 2 percentage points, while the recovery rate did not change significantly.
[0050] Comparative Example 4 Same as Example 1, except that the calcium carboxylic acid content is adjusted to 2 parts in step (4).
[0051] The application example is the same as Application Example 1.
[0052] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process (pH=8.5) and reagent preparation method, the titanium concentrate grade was 46.13%, and the titanium recovery rate was 84.42%. This indicates that when the calcium carboxylic acid content is below the specified range, the grade and recovery rate of ilmenite decrease compared to the flotation indicators in Example 1.
[0053] Comparative Example 5 Same as Example 2, except that in step (3) and step (4), the sodium hydroxide content is adjusted to 10 parts.
[0054] The application example is the same as Application Example 2.
[0055] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process (pH=8.0) and reagent preparation method, the titanium concentrate grade was 48.36%, and the titanium recovery rate was 83.32%. This indicates that when the sodium hydroxide content is below the specified range, the recovery rate of ilmenite decreases compared to the flotation parameters of Example 2.
[0056] Comparative Example 6 Same as Example 2, except that the sodium hydroxide content in step (4) is adjusted to 30 parts.
[0057] The application example is the same as application example 2.
[0058] Experimental results: Using a novel collector, according to Figure 1 After flotation (pH=8.0) and reagent separation, the titanium concentrate grade was 46.36%, and the titanium recovery rate was 87.75%. This indicates that when the sodium hydroxide content is higher than the specified range, the grade of ilmenite decreases compared to the flotation parameters of Example 2.
[0059] Comparative Example 7 Same as Example 3.
[0060] The application example is the same as application example 3, except that the pH is always maintained at 7.0.
[0061] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process and reagent preparation method, the titanium concentrate grade was 46.15%, and the titanium recovery rate was 75.42%. Compared with the flotation indicators in Example 3, the flotation performance of the novel collector was difficult to achieve effectively when the pH was below the specified range, resulting in a decrease in both the grade and recovery of ilmenite.
[0062] Comparative Example 8 Same as Example 3.
[0063] The application example is the same as application example 3, except that the pH is always maintained at 11.
[0064] Experimental results: Using a novel collector, according to Figure 1 After separation using the flotation process and reagent preparation method, the titanium concentrate grade was 45.35%, and the titanium recovery rate was 85.05%. Compared with the flotation indicators of Example 3, the flotation performance of the new collector decreased when the pH was higher than the specified range, and the grade of ilmenite decreased significantly.
[0065] The above are merely preferred embodiments of this application, but the scope of protection of this application is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the scope of the technology disclosed in this application should be included within the scope of protection of this application. Therefore, the scope of protection of this application should be determined by the scope of the claims.
Claims
1. A flotation collector for ilmenite, characterized in that, Linoleic acid hydroxamic acid crystals are added to the components; the linoleic acid hydroxamic acid crystals are made from hydroxylamine, methyl linoleate, sodium hydroxide and hydrochloric acid. The method for preparing the linoleic acid hydroxamic acid crystals includes the following steps: Hydroxylamine was prepared as a raw material to form an aqueous solution of hydroxylamine. Methyl linoleate was added dropwise to the aqueous solution of hydroxylamine and stirred to convert the ester group in the molecular structure of methyl linoleate into isohydroxamic acid. Continue adding hydroxylamine and sodium hydroxide to the system and continue stirring to fully convert methyl linoleate into sodium isohydroxamic acid salt; Hydrochloric acid was added to the system to convert sodium hydroxamic acid salt into hydroxamic acid crystals; the crystals were then obtained by rotary evaporation. The concentration of the hydroxylamine aqueous solution is 20-40 wt%; The molar ratio of hydroxylamine to methyl linoleate in the aqueous hydroxylamine solution is (1.5-3):1; The molar ratio of sodium hydroxide to methyl linoleate is (2-4):1; The molar ratio of hydroxylamine to methyl linoleate added in the second addition was (2-4):1; The molar ratio of hydrochloric acid to methyl linoleate is (1.5-3):1; The ilmenite flotation collector comprises the following components in parts by weight: 25-35 parts of linoleic acid hydroxamic acid crystals, 5-10 parts of calcium carboxylic acid, 15-20 parts of sodium hydroxide, and 25-35 parts of water.
2. A method for preparing the ilmenite flotation collector as described in claim 1, characterized in that, The process includes the following steps: Weigh linoleic acid hydroxamic acid crystals, calcium carboxylic acid, sodium hydroxide and water by mass, and react them at 140-180℃ for 1-3 hours to obtain a paste, which is the ilmenite flotation collector.
3. The application of the ilmenite flotation collector as described in claim 1 in ilmenite flotation.
4. A flotation method for ilmenite, characterized in that, Includes the following steps: The raw ilmenite is ground, the pulp pH is adjusted to 8.0-9.5, sodium hexametaphosphate and carboxymethyl cellulose are used as inhibitors, and the ilmenite flotation collector described in claim 1 is used as the collector. A closed-circuit process is carried out, consisting of one roughing, one scavenging, three cleaning, and middlings return, to obtain tailings and concentrate respectively.
5. The ilmenite flotation method according to claim 4, characterized in that, During the roughing process, the ilmenite flotation collector is added during the roughing, scavenging, and third cleaning processes. Specifically, the amount added during the roughing process is 1000 g / ton; the amount added during the scavenging process is 400 g / ton; and the amount added during the third cleaning process is 100 g / ton.
6. The ilmenite flotation method according to claim 4, characterized in that, The inhibitors are added during the roughing process, the scavenging process, and the first cleaning process, respectively; wherein, during the roughing process, the amount of sodium hexametaphosphate added is 200 g / ton; the amount of carboxymethyl cellulose added is 20 g / ton; and the amount added is halved in the scavenging process and the first cleaning process.
Citation Information
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