Phosphorite desilicication and magnesium removal collecting agent and preparation method and application thereof

By using a collector composed of modified fatty acids, sodium oleate and organic alcohols, high magnesium and high silicon phosphate ore flotation, the problems of long process flow, many agents and high cost in the prior art are solved, and efficient and simple phosphorus concentrate production is achieved.

CN119793707AActive Publication Date: 2025-04-11GANFENG LITHIUM CO LTD
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Patent Information

Application Number
CN202411903951.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-23
Publication Date
2025-04-11
Estimated Expiration
2044-12-23

AI Technical Summary

Technical Problem

The existing high-magnesium and high-silicon phosphate flotation process has a long process flow and a wide variety of agents, which makes it difficult to recycle backwater, which increases the cost of ore dressing and reduces the yield of phosphorus concentrate.

Method used

The phosphate ore desilicate and demagnesium collector consisting of modified fatty acids, sodium oleate and organic alcohols are used to effectively sort the phosphate ore with low grade and high silicon and high magnesium. Through the positive flotation and reverse flotation processes, high grade and high recovery phosphorus concentrate production is achieved.

Benefits of technology

It significantly improves the ore dressing effect of phosphate ore, simplifies the ore dressing process, reduces the flotation cost, and improves the grade and recovery rate of phosphate concentrate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a phosphorite desilicication and magnesium removal collecting agent as well as a preparation method and application thereof. The collecting agent comprises the following main components: 30-45% of modified fatty acid; 40 to 60 percent of sodium oleate; and 1-10% of organic alcohol is prepared to obtain the phosphorite collecting agent. The preparation method of the phosphorite desilicication and magnesium removal collecting agent comprises the steps that oleic acid and 10-98% sulfuric acid are mixed according to the mass ratio of 1: (5-10), heated at the temperature of 40-120 DEG C and evenly stirred, and a first mixture is formed; adding 1-10% by mass of lauric acid and 5-10% by mass of tall oil into the uniformly stirred first mixture, and fully stirring and mixing to obtain modified fatty acid; heating and uniformly stirring the modified fatty acid and sodium oleate at the temperature of 40-60 DEG C to obtain a second mixture; and when stirring is kept, organic alcohol is dropwise added into the second mixture at the speed of 60-180 dpm, stirring is conducted till uniform mixing is achieved, the collecting agent is prepared, high-grade and high-recovery-rate phosphate concentrate can be obtained through the collecting agent, and the ore dressing effect of phosphorite is remarkably improved.
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Description

Technical Field

[0001] The invention relates to the technical field of pharmaceutical chemistry and mineral processing engineering, and in particular to a phosphate ore desiliconization and demagnesiumization collector and a preparation method and application thereof. Background Art

[0002] Phosphate rock is a multifunctional mineral resource, and one of its most important application areas is as a raw material for the production of phosphate fertilizers. Phosphate fertilizers play an indispensable role in agricultural production and are crucial to increasing crop yields and improving crop quality. In addition, phosphate rock is also widely used in the manufacture of chemical products such as yellow phosphorus and phosphates, which also occupy an important position in many industries such as chemicals, medicine, and food. In recent years, with the vigorous development of the new energy industry, the demand for phosphate rock for battery materials such as iron phosphate and lithium iron phosphate has grown rapidly.

[0003] At present, phosphorus-containing minerals mainly exist in the form of calcium phosphates, which can be divided into five types according to the different carbon dioxide content in the minerals. In my country, the common type of phosphate ore is carbon fluoroapatite, also known as collophanite, which has a high phosphorus content but is often accompanied by gangue minerals such as dolomite, calcite and quartz. About 80% of the world's apatite is enriched by various mineral processing methods. For complex phosphate ores containing magnesium and silicon, a combined process of forward and reverse flotation is usually used for treatment. This process requires a wide variety of reagents and a relatively complex process.

[0004] However, the existing flotation process of high-magnesium and high-silicon phosphate ore has some problems, such as long process flow and many types of reagents, which make it difficult to recycle the return water during the flotation process, thereby increasing the beneficiation cost and reducing the yield of phosphate concentrate. Therefore, it is of great significance to develop a collector with superior performance and easy to use, and optimize the flotation process to improve the enrichment efficiency of complex magnesium-containing and silicon-containing phosphate ores or low-grade phosphate ores. Summary of the invention

[0005] In view of the above situation, the present invention provides a phosphate rock desiliconization and demagnesiumization collector and a preparation method and application thereof to solve the technical problems raised by the background technology.

[0006] The technical solution of the present invention is: a collector for desiliconizing and demagnesizing phosphate ore, the collector comprising the following components by mass percentage:

[0007] Modified fatty acids: 30-45%;

[0008] Sodium oleate: 40-60%;

[0009] Organic alcohol: 1-10%.

[0010] The phosphate ore desiliconization and demagnesiumization collector proposed in the present invention has the following beneficial effects:

[0011] The self-prepared collector is mainly composed of modified fatty acid (30-45%), fatty acid salt (40-60%) and organic alcohol component (1-10%), and the self-prepared collector can effectively separate low-grade phosphate ore containing high silicon and high magnesium gangue minerals. For high silicon and high magnesium phosphate ore, within the range of -200 mesh grinding fineness accounting for 60-70%, high-grade and high recovery rate phosphate concentrate can be obtained, which significantly improves the beneficiation effect of phosphate ore.

[0012] In addition, the phosphate ore desiliconization and demagnesiumization collector provided by the present invention may also have the following additional technical features:

[0013] Preferably, the modified fatty acid is prepared by mixing oleic acid and sulfuric acid, heating and modifying them, and then adding lauric acid and tall oil.

[0014] Preferably, the modified fatty acid is composed of the following components by mass percentage:

[0015] Sulfate oleate: 80-95%;

[0016] Lauric acid: 1-10%;

[0017] Tall oil: 5-10%;

[0018] The oleic acid sulfate is prepared by mixing oleic acid and sulfuric acid in a mass ratio of 1:(5-10), wherein the mass fraction of the sulfuric acid is 10-98%.

[0019] Preferably, the organic alcohol includes any one or more combinations of terpineol, methyl isobutyl carbinol, C6-C8 mixed fatty alcohols and sec-octanol.

[0020] A method for preparing a phosphate rock desiliconization and demagnesiumization collector comprises the following steps:

[0021] Mixing oleic acid and 10-98% sulfuric acid in a mass ratio of 1:(5-10), heating at a temperature of 40-120° C. and stirring uniformly to form a first mixture;

[0022] Adding 1 to 10% by mass of lauric acid and 5 to 10% by mass of tall oil to the first mixture that has been stirred evenly, and stirring and mixing the mixture thoroughly to obtain a modified fatty acid;

[0023] Under the temperature condition of 40-60° C., heating and stirring the modified fatty acid and sodium oleate to obtain a second mixture;

[0024] While stirring, organic alcohol is added dropwise to the second mixture at a rate of 60 to 180 dpm, and stirred until the mixture is uniformly mixed to prepare a collector.

[0025] In addition, the present invention also provides the use of the above-mentioned collector for desiliconization and demagnesiumization of phosphate ore, wherein the collector is used for flotation of phosphate ore, comprising the following steps:

[0026] Using the collector to fully float the magnesium-containing phosphate ore;

[0027] Adjust pH or add inhibitors to perform reverse flotation to separate magnesium-containing minerals and phosphate rocks;

[0028] Through the above steps, only one collector is added to desiliconize and demagnesium the magnesium-containing phosphate ore.

[0029] In addition, the application of the phosphate ore desiliconization and demagnesiumization collector provided by the present invention may also have the following additional technical features:

[0030] Preferably, the application comprises the following steps:

[0031] (a) subjecting the ore pulp after crushing, grinding and slurry conditioning to flotation tests of direct flotation-coarse-fine desiliconization and reverse flotation-coarse-fine demagnesiumization and one-time scavenging to obtain flotation concentrate;

[0032] Wherein, the dosage of the inhibitor and the collector added in the roughing I stage of the positive flotation is 1-2 kg / t;

[0033] The collector dosage used in the sweeping stage is 1 / 3 to 1 / 2 of the dosage of the roughing I;

[0034] In the roughing II stage of the reverse flotation, only sulfuric acid is added as a pH adjuster and inhibitor;

[0035] No reagent is added in the direct flotation concentration I and the reverse flotation concentration II stages;

[0036] The concentration I and the scavenging of the ore are returned to a roughing process;

[0037] The middlings from the roughing II and the cleaning II are returned to the roughing II;

[0038] The flotation time is 3 to 5 minutes;

[0039] The flotation concentrate is obtained through the above flotation process;

[0040] (b) washing and drying the flotation concentrate to obtain a phosphate concentrate product.

[0041] Preferably, during the flotation process of high-silicon phosphate ore, the grinding fineness is controlled to be: -200 mesh accounts for 50% to 60%, and the total amount of -45um is less than 20%.

[0042] Preferably, the slurry concentration of the roughing selection I and the roughing selection II is 30-40wt%, and the concentration of the fine selection I, the fine selection II and the scavenging selection is 20-30wt%.

[0043] Preferably, the pH of the slurry is 2-4. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 It is a flotation process flow chart of the present invention. DETAILED DESCRIPTION

[0045] In order to facilitate understanding of the present invention, the present invention will be described more fully below with reference to various embodiments, but the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present invention more thorough and comprehensive.

[0046] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more related listed items.

[0047] The embodiment of the present invention provides a phosphate rock desiliconization and demagnesiumization collector, which is composed of modified fatty acid, sodium oleate and organic alcohol.

[0048] In the present invention, the modified fatty acid in the collector is 30-45% by mass, for example, 30%, 37%, 40% or 45%, etc., but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0049] The mass percentage of sodium oleate in the collector is 40-60%, for example, 40%, 45%, 50%, 55% or 60%, but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0050] The mass percentage of the organic alcohol in the collector is 1-10%, for example, 1%, 3%, 5%, 8% or 10%, etc., but is not limited to the listed values, and other values ​​not listed within the range are also applicable.

[0051] The modified fatty acid is prepared by mixing oleic acid and sulfuric acid, heating and modifying them, and then adding lauric acid and tall oil.

[0052] The modified fatty acid is composed of the following components by mass percentage:

[0053] Sulfate oleate: 80-95%;

[0054] Lauric acid: 1-10%;

[0055] Tall oil: 5-10%;

[0056] The oleic acid sulfate is prepared by mixing oleic acid and sulfuric acid in a mass ratio of 1:(5-10), wherein the mass fraction of the sulfuric acid is 10-98%.

[0057] In the present invention, the mass percentage of oleic acid sulfate in the modified fatty acid is 80-95%, for example, it can be 80%, 83%, 88%, 90% or 95%, but it is not limited to the listed values, and other values ​​not listed in the range are also applicable;

[0058] The lauric acid in the modified fatty acid is 1-10% by mass, for example, 1%, 3%, 6%, 8% or 10%, etc., but is not limited to the listed values, and other values ​​not listed within the range are also applicable;

[0059] The mass percentage of tall oil in the modified fatty acid is 5-10%, for example, 5%, 7%, 9% or 10%, but is not limited to the values ​​listed, and other values ​​not listed within the range are also applicable.

[0060] The preparation method of the oleic acid sulfate is to mix oleic acid and sulfuric acid in a mass ratio of 1:5 to 1:10, wherein the mass fraction of sulfuric acid in the mixture is 10% to 98%. Specifically, the mass ratio of oleic acid to sulfuric acid can be 1:5, 1:6, 1:8 or 1:10, etc., and the mass fraction of sulfuric acid can be 10%, 30%, 60%, 80% or 98%, etc., but is not limited to these listed values. Within this range, other values ​​not explicitly listed are also applicable to the preparation of oleic acid sulfate.

[0061] The organic alcohol includes terpineol, methyl isobutyl carbinol, C6 to C8 mixed fatty alcohol and sec-octanol. Any one of these alcohols can be used alone, or any two or more of them can be used in combination. In an embodiment of the present invention, the specific selection of organic alcohols may include but is not limited to: using terpineol alone, using methyl isobutyl carbinol alone, a combination of terpineol and methyl isobutyl carbinol, a combination of methyl isobutyl carbinol and C6 to C8 mixed fatty alcohol and sec-octanol, a combination of terpineol and methyl isobutyl carbinol and C6 to C8 mixed fatty alcohol, etc. Within this scope, other combinations not explicitly listed are also applicable to the present invention.

[0062] The embodiment of the present invention also provides a method for preparing a phosphate ore desiliconization and demagnesiumization collector, comprising the following steps:

[0063] Mixing oleic acid and 10-98% sulfuric acid in a mass ratio of 1:(5-10), heating at a temperature of 40-120° C. and stirring uniformly to form a first mixture;

[0064] Adding 1 to 10% by mass of lauric acid and 5 to 10% by mass of tall oil to the first mixture that has been stirred evenly, and stirring and mixing the mixture thoroughly to obtain a modified fatty acid;

[0065] Under the temperature condition of 40-60° C., heating and stirring the modified fatty acid and sodium oleate to obtain a second mixture;

[0066] While stirring, organic alcohol is added dropwise to the second mixture at a rate of 60 to 180 dpm, and stirred until the mixture is uniformly mixed to prepare a collector.

[0067] In the present invention, the temperature condition is set between 40°C and 60°C, and the specific temperature can be selected as 40°C, 50°C or 60°C. At the same time, the rate of adding the organic alcohol to the second mixture is controlled within the range of 60 drops per minute (dpm) to 180 drops per minute (dpm), and the specific drop rate can be selected as 60dpm, 100dpm, 120dpm, 160dpm or 180dpm. These specific temperature and drop rate values ​​are only examples, and the implementation of the present invention is not limited to these listed values, and other values ​​not explicitly listed within the range are also applicable.

[0068] The embodiment of the present invention further proposes an application of a collector for desiliconization and demagnesiumization of phosphate ore, wherein the collector is used for flotation of phosphate ore, and comprises the following steps:

[0069] Using the collector to fully float the magnesium-containing phosphate ore;

[0070] Adjust pH or add inhibitors to perform reverse flotation to separate magnesium-containing minerals and phosphate rocks;

[0071] Through the above steps, only one collector is added to desiliconize and demagnesium the magnesium-containing phosphate ore.

[0072] The application comprises the following steps:

[0073] (a) subjecting the ore pulp after crushing, grinding and slurry conditioning to flotation tests of direct flotation-coarse-fine desiliconization and reverse flotation-coarse-fine demagnesiumization and one-time scavenging to obtain flotation concentrate;

[0074] Wherein, the dosage of the inhibitor and the collector added in the roughing I stage of the positive flotation is 1-2 kg / t;

[0075] The collector dosage used in the sweeping stage is 1 / 3 to 1 / 2 of the dosage of the roughing I;

[0076] In the roughing II stage of the reverse flotation, only sulfuric acid is added as a pH adjuster and inhibitor;

[0077] No reagent is added in the direct flotation concentration I and the reverse flotation concentration II stages;

[0078] The concentration I and the scavenging of the ore are returned to a roughing process;

[0079] The middlings from the roughing II and the cleaning II are returned to the roughing II;

[0080] The flotation time is 3 to 5 minutes;

[0081] The flotation concentrate is obtained through the above flotation process;

[0082] In the present invention, the time parameter of the flotation process has a certain flexibility and can be set to 3 minutes, 3.5 minutes, 4 minutes, 4.5 minutes or 5 minutes. These specific time points are only examples, and are intended to illustrate that the flotation time can be adjusted within a relatively wide range to adapt to different process requirements and ore characteristics. The implementation of the present invention is not limited to these listed time points, and other time values ​​not explicitly listed within the range are also applicable.

[0083] (b) washing and drying the flotation concentrate to obtain a phosphate concentrate product.

[0084] Among them, the dosage of scavenging agents is 1 / 3 to 1 / 2 of that of roughing selection; except for the addition of collectors in roughing selection I and scavenging selection, no collectors are added during the selection process, and only inhibitors are added in selection I, which is 1 / 2 to 1 / 3 of that in roughing selection, and only acids are added as inhibitors and pH adjusters in roughing selection II and selection II.

[0085] The grinding fineness of low-grade phosphate ore with complex embedded particle size should be relatively controlled according to the difference in the content of gangue minerals. For example, the grinding fineness of high-silicon phosphate ore is controlled within the range of -200 mesh accounting for 50-60%, and the grinding fineness of high-magnesium phosphate ore is controlled within the range of -0.074mm accounting for 70-85%; the grinding fineness of high-silicon and high-magnesium phosphate ore should be controlled within the range of -200 mesh accounting for 60-70%. In the flotation process of high-silicon phosphate ore, due to the relatively fine embedded particle size of silicon-containing minerals and phosphate ore, excessive grinding can easily lead to the generation of fine mud. In the positive flotation desiliconization test, fine mud will interfere with the performance of the collector, thereby affecting the flotation effect. Therefore, there are strict requirements for the grinding fineness of high-silicon phosphate ore:

[0086] The grinding fineness should be controlled between 50% and 60% of the -200 mesh size, and the total amount of the -45 micron (um) size should be less than 20%.

[0087] The following are some examples:

[0088] The grinding fineness can be set to -200 mesh size accounting for 52% and -45 micron size accounting for 18%.

[0089] Another possible control method is to make the -200 mesh size account for 55% while ensuring that the total amount of -45 micron size does not exceed 19%.

[0090] The grinding fineness can also be adjusted to -200 mesh size accounting for 60%, at which time the total amount of -45 micron size should be 15%.

[0091] Another option is to have the -200 mesh fraction account for 57% while requiring the -45 micron fraction to total 17%.

[0092] These specific grinding fineness control parameters are designed to balance the fineness of the ore with the performance of the collector to ensure the efficiency of the flotation process and the quality of the final product. In actual operation, it is necessary to select the appropriate grinding fineness based on the specific characteristics of the ore and the process requirements.

[0093] High-silicon and high-magnesium phosphate ore has strong water absorption and high viscosity. During the grinding and classification process of the phosphate ore, a lot of water will be consumed. In order to adapt to the appropriate concentration of the beneficiation agent, a concentrator is used to further concentrate the slurry. The slurry concentration of the roughing I and the roughing II is 30-40wt%, and the concentration of the concentrating I, the concentrating II and the scavenging is 20-30wt%. The slurry concentration of the roughing I and the roughing II can be 30wt%, 34wt%, 36wt% or 40wt%, etc., and the concentration of the concentrating I, the concentrating II and the scavenging can be 20wt%, 22wt%, 25wt%, 27wt% or 30wt%, etc.

[0094] In the process of reverse flotation and demagnesium removal of phosphate ore, since the phosphate ore is inhibited under acidic conditions, the acidic inhibitor should be added in excess, and the pH of the slurry should be 2-4, so as to obtain high-yield and high-grade phosphate ore. The pH of the slurry is 2, 3 or 4, etc.

[0095] The following is a further description of the embodiments of the present invention in multiple embodiments. The embodiments of the present invention are not limited to the following specific embodiments. Within the scope of the unchanged main rights, appropriate changes can be made to the implementation.

[0096] Example 1

[0097] like Figure 1 , a phosphate ore desiliconization and demagnesiumization collector, the collector is composed of the following components by mass percentage:

[0098] Modified fatty acids: 37%;

[0099] Sodium oleate: 55%;

[0100] Organic alcohol: 8%.

[0101] The preparation method of the above-mentioned phosphate rock desiliconization and demagnesiumization collector comprises the following steps:

[0102] (1) mixing oleic acid and 70% sulfuric acid in a mass ratio of 1:7, heating at 80° C. and stirring to form a first mixture;

[0103] (2) adding 4% by mass of lauric acid and 9% by mass of tall oil to the first mixture that has been stirred uniformly, and stirring and mixing the mixture thoroughly to obtain a modified fatty acid;

[0104] (3) heating the modified fatty acid and sodium oleate at 50° C. and stirring them uniformly to obtain a second mixture;

[0105] (4) While stirring, adding organic alcohol to the second mixture at a rate of 110 dpm, and stirring until the mixture is uniformly mixed to prepare a collector.

[0106] Application Example 1

[0107] This application example provides an application of a collector for desiliconization and demagnesiumization of phosphate ore. The collector is used for phosphate ore flotation. A high-magnesium phosphate ore from a certain place in Yunnan has a raw ore grade of P2O5: 23.12%, MgO: 5.75%, and SiO2: 7.48%. The ore needs to be ground to -200 mesh, accounting for about 75-85%. The process is as follows:

[0108] Using the collector to fully float the magnesium-containing phosphate ore;

[0109] Adjust pH or add inhibitors to perform reverse flotation to separate magnesium-containing minerals and phosphate rocks;

[0110] Through the above steps, only one collector is added to desiliconize and demagnesium the magnesium-containing phosphate ore.

[0111] The specific steps are as follows;

[0112] (a) subjecting the ore pulp after crushing, grinding and slurry conditioning to flotation tests of direct flotation-coarse-fine desiliconization and reverse flotation-coarse-fine demagnesiumization and one-time scavenging to obtain flotation concentrate;

[0113] Wherein, the dosage of the inhibitor and the collector added in the roughing I stage of the positive flotation is 1.5 kg / t;

[0114] The collector dosage used in the sweeping stage is 1 / 3 of the dosage of the roughing I;

[0115] In the roughing II stage of the reverse flotation, only sulfuric acid is added as a pH adjuster and inhibitor;

[0116] No reagent is added in the direct flotation concentration I and the reverse flotation concentration II stages;

[0117] The concentration I and the scavenging of the ore are returned to a roughing process;

[0118] The middlings from the roughing II and the cleaning II are returned to the roughing II;

[0119] The flotation time was 4 minutes;

[0120] The flotation concentrate is obtained through the above flotation process;

[0121] (b) washing and drying the flotation concentrate to obtain a phosphate concentrate product.

[0122] The slurry concentration of the roughing selection I and the roughing selection II is 35wt%, and the concentration of the cleaning selection I, the cleaning selection II and the scavenging selection is 25wt%.

[0123] The pH of the slurry is 3.

[0124] The flotation results of the above application example 1 are shown in Table 1 below:

[0125] Table 1 Flotation test results of high magnesium phosphate ore in Yunnan

[0126]

[0127] In this application example, when the mineral grade is only P2O5: 0.27%, MgO: 5.75%, SiO2: 7.48%, a phosphate concentrate with a recovery rate of 92.17% and a P2O5 grade of 33.39% can be obtained through self-prepared reagent flotation, which proves that the process of the present invention can achieve desiliconization and demagnesium effects on the flotation of high-magnesium phosphate ore.

[0128] Application Example 2

[0129] This application example provides an application of a collector for desiliconization and demagnesiumization of phosphate ore, wherein the collector is used for flotation of phosphate ore. A high-silicon and high-magnesium phosphate ore in Sichuan is selected, and its raw ore grade is P2O5: 20.44%, MgO: 3.39%, SiO2: 19.40%. The ore needs to be ground to -200 mesh, accounting for about 65-70%. The same process as in application example 1 is used.

[0130] The flotation results of the above application example 2 are shown in Table 2 below:

[0131] Table 2 Flotation test results of high silicon magnesium phosphate ore in Sichuan

[0132]

[0133] In this application example, when the phosphate ore grade is only P2O5: 20.44%, MgO: 3.39%, SiO2: 19.40%, the grade and recovery rate of P2O5 are 32.03% and 91.18% respectively, and the grades of MgO and SiO2 are 1.22% and 9.15% respectively, which proves that the process of the present invention can achieve the effect of desiliconization and demagnesiumization for the flotation of high-silicon phosphate ore.

[0134] Application Example 3

[0135] This application example provides an application of a phosphate ore desiliconization and demagnesiumization collector, which is used for phosphate ore flotation. A high-silicon and high-magnesium phosphate ore in Hongfu, Yunnan, is selected. The original ore grade is P2O5: 19.65%, MgO: 3.02%, SiO2: 20.32%, and the ore needs to be ground to -200 mesh, accounting for about 65-70%. The same process as in Application Example 1 is used.

[0136] The flotation results of the above application example 3 are shown in Table 3 below:

[0137] Table 3 Flotation test results of high silicon magnesium phosphate ore in Hongfu, Yunnan

[0138]

[0139] In this application example, when the grade of the phosphate ore is only P2O5: 19.65%, MgO: 3.02%, SiO2: 20.32%, the grade and recovery rate of P2O5 are 32.42% and 91.93% respectively, and the grades of MgO and SiO2 are 0.85% and 10.78% respectively, which proves that the process of the present invention can achieve the effect of desiliconization and demagnesiumization for the flotation of high-silicon and high-magnesium phosphate ore.

[0140] In summary, according to the phosphate ore desiliconization and demagnesiumization collector provided by the present invention, and its preparation method and application, the present invention is aimed at phosphate ore containing high silicon and high magnesium, and adopts a self-prepared collector to realize full flotation and desiliconization of magnesium-containing phosphate ore, and then reverse flotation separation of magnesium-containing minerals and phosphate ore is carried out by adjusting pH and inhibitors to realize magnesium removal from phosphate ore. The process has the characteristics of high enrichment concentrate grade and recovery rate for medium and low grade high silicon and high magnesium phosphate ore, simple mineral processing process, low flotation cost, etc.

[0141] The present invention uses a self-prepared collector, which is mainly composed of modified fatty acid (30-45%), fatty acid salt (40-60%) and organic alcohol component (1-10%). This collector can effectively sort low-grade phosphate ore containing high-silicon and high-magnesium gangue minerals. For high-silicon and high-magnesium phosphate ore, in the range of -200 mesh grinding fineness accounting for 60-70%, through the process of positive flotation desiliconization and reverse flotation demagnesiumization, high-grade and high-recovery phosphate concentrate can be obtained, which significantly improves the beneficiation effect of phosphate ore.

[0142] The magnesium-containing phosphate ore is first fully floated using a self-prepared collector, and then the magnesium-containing minerals and phosphate ore are reversely floated and separated only by adjusting the pH and adding inhibitors. This achieves the effect of desiliconizing and demagnesizing the phosphate ore by adding only one collector, reducing the use of different reagents.

[0143] This process simplifies the mineral processing process. Compared with the traditional high-magnesium and high-silicon phosphate ore flotation process, it reduces the complex reagent combination and operation steps, and improves the operability and stability of the mineral processing process.

[0144] Due to the simplified use of reagents and the simplicity of the beneficiation process, the flotation cost is greatly reduced. In the enrichment process of medium and low-grade high-silicon and high-magnesium phosphate ores, the concentrate grade and recovery rate are guaranteed, the cost is effectively controlled, and the economic benefits of phosphate beneficiation are improved.

[0145] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the patent of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A phosphate rock desiliconization and demagnesiumization collector, characterized in that: The collector is composed of the following components by mass percentage: Modified fatty acids: 30-45%; Sodium oleate: 40-60%; Organic alcohol: 1-10%.

2. The phosphate rock desiliconization and demagnesiumization collector according to claim 1, characterized in that: The modified fatty acid is prepared by mixing oleic acid and sulfuric acid, heating and modifying them, and then adding lauric acid and tall oil.

3. The phosphate rock desiliconization and demagnesiumization collector according to claim 1, characterized in that: The modified fatty acid is composed of the following components by mass percentage: Sulfate oleate: 80-95%; Lauric acid: 1-10%; Tall oil: 5-10%; The oleic acid sulfate is prepared by mixing oleic acid and sulfuric acid in a mass ratio of 1:(5-10), wherein the mass fraction of the sulfuric acid is 10-98%.

4. The phosphate rock desiliconization and demagnesiumization collector according to claim 1, characterized in that: The organic alcohol includes any one or more combinations of terpineol, methyl isobutyl carbinol, C6-C8 mixed fatty alcohols and sec-octanol.

5. The method for preparing the phosphate rock desiliconization and demagnesiumization collector according to any one of claims 1 to 4, characterized in that: The following steps are involved: Mixing oleic acid and 10-98% sulfuric acid in a mass ratio of 1:(5-10), heating at a temperature of 40-120° C. and stirring uniformly to form a first mixture; Adding 1 to 10% by mass of lauric acid and 5 to 10% by mass of tall oil to the first mixture that has been stirred evenly, and stirring and mixing the mixture thoroughly to obtain a modified fatty acid; Under the temperature condition of 40-60° C., heating and stirring the modified fatty acid and sodium oleate to obtain a second mixture; While stirring, organic alcohol is added dropwise to the second mixture at a rate of 60 to 180 dpm, and stirred until the mixture is uniformly mixed to prepare a collector.

6. The use of the phosphate ore desiliconization and demagnesiumization collector according to any one of claims 1 to 4, characterized in that: The collector is used for phosphate ore flotation, comprising the following steps: Using the collector to fully float the magnesium-containing phosphate ore; Adjust pH or add inhibitors to perform reverse flotation to separate magnesium-containing minerals and phosphate rocks; Through the above steps, only one collector is added to desiliconize and demagnesium the magnesium-containing phosphate ore.

7. The use of the phosphate rock desiliconization and demagnesiumization collector according to claim 6, characterized in that: The application comprises the following steps: (a) subjecting the ore pulp after crushing, grinding and slurry conditioning to flotation tests of direct flotation-coarse-fine desiliconization and reverse flotation-coarse-fine demagnesiumization and one-time scavenging to obtain flotation concentrate; Wherein, the dosage of the inhibitor and the collector added in the roughing I stage of the positive flotation is 1-2 kg / t; The collector dosage used in the sweeping stage is 1 / 3 to 1 / 2 of the dosage of the roughing I; In the roughing II stage of the reverse flotation, only sulfuric acid is added as a pH adjuster and inhibitor; No reagent is added in the direct flotation concentration I and the reverse flotation concentration II stages; The concentration I and the scavenging of the ore are returned to a roughing process; The middlings from the roughing II and the cleaning II are returned to the roughing II; The flotation time is 3 to 5 minutes; The flotation concentrate is obtained through the above flotation process; (b) washing and drying the flotation concentrate to obtain a phosphate concentrate product.

8. The use of the phosphate rock desiliconization and demagnesiumization collector according to claim 7, characterized in that: During the flotation process of high-silicon phosphate ore, the grinding fineness is controlled as follows: -200 mesh accounts for 50% to 60%, and the total amount of -45um is less than 20%.

9. The use of the phosphate rock desiliconization and demagnesiumization collector according to claim 7, characterized in that: The slurry concentrations of the roughing selection I and the roughing selection II are 30-40wt%, and the concentrations of the concentrating selection I, the concentrating selection II and the scavenging selection are 20-30wt%.

10. The use of the phosphate rock desiliconization and demagnesiumization collector according to claim 7, characterized in that: The pH of the slurry is 2-4.

Citation Information

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