Novel compound reagent, preparation method thereof and use method of novel compound reagent in potassium ore flotation
By preparing a novel compound reagent, the problem of poor dispersibility of traditional collectors at low temperatures was solved, the flotation efficiency and recovery rate of potassium salts were improved, and efficient potassium salt separation under low temperature conditions was achieved.
Patent Information
- Application Number
- CN202511693571.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-18
- Publication Date
- 2026-01-16
AI Technical Summary
Traditional collector octadecylamine exhibits poor dispersibility and high solution viscosity at low temperatures, resulting in low potassium salt flotation recovery rates in salt lakes.
A novel compound reagent was prepared by mixing octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a specific ratio, adding deionized water, heating and stirring, adding acid dropwise, and then cooling. This reagent was used for potassium ore flotation, and the adsorption performance of the reagent at low temperatures was improved through multi-component functional coupling.
The flotation efficiency of potassium salts is improved at low temperatures, and the amount of reagent used is small, while the effect is better than that of the traditional collector octadecylamine.
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Figure CN121338933A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of potassium ore flotation separation technology, and in particular to a novel compound reagent for potassium chloride flotation separation, its preparation method, and its application in potassium ore flotation. Background Technology
[0002] Potash is a core strategic resource for ensuring stable and high crop yields. As one of the three major fertilizers (nitrogen, phosphorus, and potassium), it directly determines the stability of the global food supply chain. my country's arable land is generally potassium-deficient, with over 70% of its soil having available potassium content below the critical value for crop growth. The average annual demand for potash fertilizer exceeds 12 million tons. However, my country's soluble potash reserves account for only 5% of the global total, and the grade is low with high extraction costs. This has resulted in a potash fertilizer self-sufficiency rate hovering between 50% and 55% for a long time. In 2023, the import dependency rate was still as high as 45% (approximately 6 million tons), with imports exceeding US$2 billion.
[0003] In my country, flotation is the mainstream process for separating potash from low-grade salt lake deposits (accounting for over 90% of production capacity), and its efficiency is highly dependent on the adsorption activity of the collector at the mineral interface. 85% of my country's recoverable potash is concentrated in the Qaidam Basin of Qinghai Province, where the average annual temperature is only 1-5℃ and winter lasts for six months. However, the traditional potassium chloride flotation collector, octadecylamine, exhibits poor flotation efficiency at low temperatures. This is because, under low-temperature conditions, amines have poor solubility / dispersion, high solution viscosity, a sharp drop in molecular kinetic energy, a decrease in the collector diffusion coefficient, and sluggish adsorption kinetics.
[0004] Developing a highly efficient collector for potash in salt lakes under low-temperature conditions has become a key breakthrough in unlocking potash production capacity in high-altitude and cold regions. Summary of the Invention
[0005] In view of the shortcomings of the prior art, the purpose of this invention is to provide a novel compound reagent for potassium chloride flotation separation, its preparation method, and its application method in potassium ore flotation, in order to solve the problem that the traditional collector octadecylamine has poor dispersibility and high solution viscosity under low-temperature conditions, resulting in low potassium salt flotation recovery rates in salt lakes, thereby improving the flotation efficiency of potassium salts. The technical solution adopted by this invention includes:
[0006] This invention provides a novel compound drug, the preparation method of which includes the following steps:
[0007] S1. Mix octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a certain proportion, add deionized water, and obtain a mixed solution;
[0008] S2. Heat the mixed solution obtained in step S1 to 60-80℃, stir continuously at a certain speed, and add acid dropwise. After the addition is completed, continue stirring for a period of time, and then cool to obtain the novel compound drug.
[0009] Preferably, the ratio of octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate is 10-13:1-2:0.5-1.
[0010] Preferably, the acid can be one or more of hydrochloric acid, sulfuric acid, and acetic acid.
[0011] Preferably, the mass of the acid is 20-50% of octadecylamine.
[0012] Preferably, the stirring speed is 600-1000 r / min.
[0013] Preferably, the concentration of the compound drug is 0.5-5%.
[0014] The present invention also provides a novel compound drug prepared by the above-described preparation method.
[0015] This invention also provides a method for using a novel compound reagent in potash ore flotation, the method comprising:
[0016] The ore sample was sieved to below -0.074 mm and a saturated solution was prepared. The ore sample and the saturated solution were mixed and placed in a flotation machine. After stirring for 3-5 minutes, a potassium salt slurry was obtained. A new compound reagent was added. After adding the reagent, the mixture was stirred for 2-5 minutes and flotation was started. The flotation froth obtained was potassium chloride concentrate, and the bottom of the tank was tailings.
[0017] Preferably, the concentration of the potash slurry is 30-55%.
[0018] Preferably, the amount of the novel compound drug added is 2-20 mg / L.
[0019] The present invention has the following beneficial effects:
[0020] 1. This invention mixes octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a ratio of 10-13:1-2:0.5-1 to prepare a novel compound reagent. Through the functional coupling of multiple components, the prepared reagent can be applied to the flotation of potassium chloride ore under low temperature conditions.
[0021] 2. Long-chain amines, acting as hydrophobic anchoring groups, provide mineral recognition capabilities. At low temperatures, amines exhibit high solubility and dispersibility, reducing pulp viscosity and increasing molecular kinetic energy. The compounded components significantly lower the solution freezing point and enhance interfacial spreading, enabling refined interfacial control. Through a three-dimensional synergistic effect of electrostatic attraction, hydrogen bonding, and hydrophobic association, the thickness of the hydration layer on the potassium chloride surface is compressed, effectively overcoming the low-temperature wetting barrier. The collector diffusion coefficient increases, thereby improving the adsorption performance for potassium ions and enhancing the flotation efficiency of potassium salts at low temperatures.
[0022] 3. The flotation effect is better than that of the traditional collector octadecylamine, and the amount of octadecylamine compound reagent used is less. Attached Figure Description
[0023] Figure 1 This is a schematic flowchart of a novel compound drug preparation method provided in an embodiment of the present invention. Detailed Implementation
[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0025] In the description of this invention, it should be noted that the terms "center," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "top surface," "bottom surface," "inner," "outer," "inner side," and "outer side," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.
[0026] In the description of this invention, "several" means one or more, "multiple" means two or more, "greater than," "less than," and "exceeding" are understood to exclude the stated number, while "above," "below," and "within" are understood to include the stated number. Where the terms "first," "second," and "third" are used for descriptive purposes and to distinguish technical features, they should not be construed as indicating or implying relative importance, or implicitly indicating the number of indicated technical features, or implicitly indicating the sequential relationship of the indicated technical features.
[0027] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," "linking," and "setting" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances. The embodiments of this invention will now be described according to its overall structure.
[0028] Figure 1 This is a schematic flowchart illustrating a novel compound drug preparation method provided in an embodiment of the present invention. (See attached diagram.) Figure 1A method for preparing a novel compound drug includes the following steps:
[0029] S1. Mix octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a certain proportion, add deionized water, and obtain a mixed solution;
[0030] S2. Heat the mixed solution obtained in step S1 to 60-80℃, stir continuously at a certain speed, and add acid dropwise. After the addition is completed, continue stirring for a period of time, and then cool to obtain the novel compound drug.
[0031] In a preferred embodiment, the ratio of octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate is 10-13:1-2:0.5-1.
[0032] In a preferred embodiment, the acid may be one or more of hydrochloric acid, sulfuric acid, and acetic acid.
[0033] In a preferred embodiment, the mass of the acid is 20-50% of octadecylamine.
[0034] In a preferred embodiment, the stirring speed is 600-1000 r / min.
[0035] In a preferred embodiment, the concentration of the compound drug is 0.5-5%.
[0036] A novel compound drug is prepared by the above-described preparation method.
[0037] A method for using a novel compound reagent in potash ore flotation, the method comprising:
[0038] The ore sample was sieved to below -0.074 mm and a saturated solution was prepared. The ore sample and the saturated solution were mixed and placed in a flotation machine. After stirring for 3-5 minutes, a potassium salt slurry was obtained. A new compound reagent was added. After adding the reagent, the mixture was stirred for 2-5 minutes and flotation was started. The flotation froth obtained was potassium chloride concentrate, and the bottom of the tank was tailings.
[0039] In a preferred embodiment, the concentration of the potash slurry is 30-55%.
[0040] In a preferred embodiment, the amount of the novel compound drug added is 2-20 mg / L.
[0041] This invention mixes octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a ratio of 10-13:1-2:0.5-1 to prepare a novel compound reagent. Through multi-component functional coupling, the prepared reagent can be applied to the flotation of potash ore under low-temperature conditions.
[0042] Long-chain amines, acting as hydrophobic anchoring groups, provide mineral recognition capabilities. At low temperatures, amines exhibit high solubility and dispersibility, reducing pulp viscosity and increasing molecular kinetic energy. The compounded components significantly lower the solution freezing point and enhance interfacial spreading, enabling refined interfacial control. Through a three-dimensional synergistic effect of electrostatic attraction, hydrogen bonding, and hydrophobic association, the thickness of the hydration layer on the potassium chloride surface is compressed, effectively overcoming the low-temperature wetting barrier. The collector diffusion coefficient increases, thereby improving the adsorption performance for potassium ions and enhancing the flotation efficiency of potassium salts at low temperatures.
[0043] The novel compound reagent of this invention has a better flotation effect than the traditional collector octadecylamine, and requires less dosage compared to the octadecylamine compound reagent.
[0044] Example 1
[0045] In this embodiment, octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate are mixed in a ratio of 10:0.5:1, stirred continuously at 1000 r / min at 80°C, while a 40% acetic acid solution is added dropwise. After the addition is complete, stirring is continued for 10 min, and the mixture is cooled to obtain a 2% solution, which is the compound drug.
[0046] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system:
[0047] Prepare a saturated potassium chloride solution. Place 100 ml of the saturated potassium chloride solution in a flotation machine and add 20 g of potassium chloride. After stirring for 4 min, add 5 mg / L of the above compound reagent. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0048] Prepare a saturated sodium chloride solution. Place 100 ml of the saturated sodium chloride solution in a flotation machine and add 20 g of sodium chloride. After stirring for 4 min, add 5 mg / L of the above compound reagent. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0049] Comparative Example 1: The process is the same as in Example 1, except that the compound drug is replaced with octadecylamine.
[0050] Table 1. Experimental adsorption and recovery effects of Example 1 and Comparative Example 1
[0051]
[0052] Example 2
[0053] In this embodiment, octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate are mixed in a ratio of 12:2:0.5, stirred continuously at 1000 r / min at 80°C, while a 40% acetic acid solution is added dropwise. After the addition is complete, stirring is continued for 10 min, and the mixture is cooled to obtain a 2% solution, which is the compound drug.
[0054] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system:
[0055] Prepare a saturated potassium chloride solution. Place 100 ml of the saturated potassium chloride solution in a flotation machine and add 20 g of potassium chloride. After stirring for 4 min, add 4 mg / L of collector. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0056] Prepare a saturated sodium chloride solution. Place 100 ml of the saturated sodium chloride solution in a flotation machine and add 20 g of sodium chloride. After stirring for 4 min, add 4 mg / L of collector. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0057] Comparative Example 2: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0058] Table 2. Experimental adsorption and recovery effects of Example 2 and Comparative Example 2
[0059]
[0060] Example 3
[0061] In this embodiment, octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate are mixed in a ratio of 12:1:0.5, stirred continuously at 1000 r / min at 80°C, while a 40% acetic acid solution is added dropwise. After the addition is complete, stirring is continued for 10 min, and the mixture is cooled to obtain a 2% solution, which is the compound drug.
[0062] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system:
[0063] Prepare a saturated potassium chloride solution. Place 100 ml of the saturated potassium chloride solution in a flotation machine and add 20 g of potassium chloride. After stirring for 4 min, add 4 mg / L of reagent. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0064] Prepare a saturated sodium chloride solution. Place 100 ml of the saturated sodium chloride solution in a flotation machine and add 20 g of sodium chloride. After stirring for 4 min, add 4 mg / L of reagent. After adding the reagent, stir for 5 min and start flotation (experimental temperature is 20℃). Calculate the recovery rate after drying the flotation foam.
[0065] Comparative Example 3: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0066] Table 3. Experimental adsorption and recovery effects of Example 3 and Comparative Example 3
[0067]
[0068] Example 4
[0069] In this embodiment, octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate are mixed in a ratio of 9:1:0.5, stirred continuously at 1000 r / min at 80°C, while a 40% acetic acid solution is added dropwise. After the addition is complete, stirring is continued for 10 min, and the mixture is cooled to obtain a 2% solution, which is the compound drug.
[0070] The above-mentioned compound reagents were used to achieve flotation of the potash ore system:
[0071] A saturated solution of the actual mineral sample was prepared. The actual mineral sample was sieved to below -0.074 mm. The actual mineral sample used in the experiment was collected from the flotation workshop of Salt Lake Group, and its potassium content was 15.63%. 100 ml of the saturated solution of the actual mineral sample was placed in the flotation machine and 20 g of the sieved actual mineral sample was added. After stirring for 4 min, 3 mg / L of reagent was added respectively. After adding the reagent, the mixture was stirred for 5 min and then flotation was started (experimental temperature was 20℃). The flotation froth was dried and the recovery rate was calculated.
[0072] Comparative Example 4: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0073] Table 4. Experimental adsorption and recovery effects of Example 4 and Comparative Example 4
[0074]
[0075]
[0076] In summary, the present invention provides a novel method for preparing a compound reagent by mixing octadecylamine, sodium oleate, and hydroxyethylidene diphosphonate in a ratio of 10-13:1-2:0.5-1 to prepare a novel compound reagent. Through multi-component functional coupling, the prepared reagent can be applied to the flotation of potassium ore under low-temperature conditions, effectively overcoming the low-temperature wetting barrier, improving the adsorption and separation performance of potassium ions, and improving the flotation efficiency of potassium salts at low temperatures. The flotation effect is better than that of the traditional collector octadecylamine, and the dosage of the compound reagent is less than that of octadecylamine.
[0077] The above description is only a specific embodiment of this application. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of this application, and these improvements and modifications should also be considered within the scope of protection of this application.
Claims
1. A novel combination medicament, characterized in that, The preparation method comprises the following steps: S1, mixing octadecylamine, sodium oleate and hydroxyethylidene diphosphonate in a certain proportion, adding deionized water to obtain a mixed solution; S2, heating the mixed solution obtained in step S1 to 60-80℃, continuously stirring at a certain speed, and adding acid dropwise, continuing to stir for a period of time after the addition is completed, and cooling to obtain the new compound medicament.
2. A method of preparing a novel combination medicament as claimed in claim 1, wherein, In the step S1, the proportion of octadecylamine, sodium oleate and hydroxyethylidene diphosphonate is 10-13:1-2:0.5-1.
3. A method of preparing a novel combination medicament as claimed in claim 1, wherein, In the step S2, the acid can be one or more of hydrochloric acid, sulfuric acid and acetic acid.
4. A method of preparing a novel combination medicament as claimed in claim 1, wherein, In the step S2, the mass of the acid is 20-50% of the octadecylamine.
5. The method of preparing a novel combination of medicaments as claimed in claim 1, wherein, In the step S2, the stirring speed is 600-1000r / min.
6. A method of preparing a novel combination medicament as claimed in claim 1, wherein, The concentration of the compound medicament is 0.5-5%.
7. A new compound medicament formed by the preparation method of any one of claims 1-6.
8. A method of using a novel combination of reagents in the flotation of potassium ores, characterized by, The use method of the new compound medicament of claim 7 comprises: Screening the ore sample to below 0.074mm, and configuring an ore sample saturated solution, mixing the ore sample and the ore sample saturated solution, and then placing them in a flotation machine, stirring for 3-5min to obtain a potassium salt ore slurry, adding the new compound medicament, stirring for 2-5min after adding the medicament, and then starting flotation to obtain a flotation froth as a potassium chloride concentrate and a tank bottom as a tailing.
9. A method of using a novel complexing agent according to claim 8 in the flotation of potassium ores, characterized by, The concentration of the potassium salt ore slurry is 30-55%.
10. A method of using a novel complexing agent according to claim 8 in the flotation of potassium ores, characterized by, The addition amount of the new compound medicament is 2-20mg / L.