Novel compound reagent for potassium chloride flotation separation as well as preparation method and use method of novel compound reagent
By preparing a compound reagent consisting of octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate, the problem of low flotation efficiency of potassium chloride under low temperature conditions was solved, achieving efficient separation and improved selectivity of potassium salts at low temperatures.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-18
- Publication Date
- 2026-03-13
AI Technical Summary
The traditional potassium chloride flotation collector, octadecylamine, has poor flotation efficiency at low temperatures, resulting in a decrease in potassium salt grade. Existing technologies are difficult to use for efficient separation of potassium salts in frigid regions.
A novel compound reagent was prepared by mixing octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate in a specific ratio, adding deionized water, heating, and then adding acid dropwise. This reagent improves the dispersibility of the solution and reduces its viscosity, and is used for potassium chloride flotation separation.
It improves the efficiency and selectivity of potassium chloride flotation, is superior to the traditional collector octadecylamine, and is suitable for the efficient separation of potassium salts under low temperature conditions, reducing the amount of reagent used.
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Figure CN121649047A_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 method. Background Technology
[0002] Potassium salts are a core strategic resource for ensuring stable and high crop yields. As one of the three major fertilizers (nitrogen, phosphorus, and potassium), they directly determine the stability of the global food supply chain. Generally speaking, existing arable land is generally deficient in potassium, with more than 70% of soil having available potassium content below the critical value for crop growth, and the average annual demand for potassium fertilizer exceeding 12 million tons.
[0003] Currently, flotation is the mainstream process for separating potash from low-grade salt lake ores (accounting for over 90% of production capacity), and its efficiency is highly dependent on the adsorption activity of the collector at the mineral interface. Of this, 85% of recoverable potash is concentrated in frigid regions with average annual temperatures of only 1-5°C and winters lasting up to 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 order to solve the problem that under existing low-temperature conditions, the flotation efficiency and selectivity of the traditional potassium chloride flotation collector, octadecylamine, decrease as the potassium salt grade decreases during the flotation process, thereby improving the flotation efficiency and adsorption separation performance of potassium salts. The technical solution adopted by this invention includes: This invention provides a method for preparing a novel compound reagent for potassium chloride flotation separation, the preparation method comprising the following steps: S1. Mix octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate in a certain proportion, add deionized water, and obtain a mixed solution; 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.
[0006] Preferably, in step S1, the ratio of octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate is 10-13:1-2:0.5-1.
[0007] Preferably, in step S2, the acid can be one or more of hydrochloric acid, sulfuric acid, and acetic acid.
[0008] Preferably, in step S2, the mass of the acid is 20-50% of octadecylamine.
[0009] Preferably, the sodium alkylbenzene sulfonate has a carbon chain number of 8-16.
[0010] Preferably, the concentration of the compound drug is 0.5-5%.
[0011] The present invention also provides a novel compound reagent for potassium chloride flotation separation prepared by the above preparation method.
[0012] This invention also provides a method for using a novel compound reagent for potassium chloride flotation separation, the method comprising: 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.
[0013] Preferably, the concentration of the potash slurry is 30-55%.
[0014] Preferably, the amount of the novel compound drug added is 1-25 mg / L.
[0015] The present invention has the following beneficial effects: This invention prepares a novel compound reagent by mixing octadecylamine, sodium alkylbenzenesulfonate, and ethylenediaminetetramethylene phosphate in a ratio of 10-13:1-2:0.5-1. Through multi-component functional coupling, sodium alkylbenzenesulfonate and ethylenediaminetetramethylene phosphate can improve solution dispersibility and reduce solution viscosity, thereby improving flotation efficiency. It can be applied to the flotation separation of potassium chloride under low-temperature conditions. 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. Attached Figure Description
[0016] Figure 1 This is a schematic flowchart illustrating a method for preparing a novel compound reagent for potassium chloride flotation separation, as provided in an embodiment of the present invention. Detailed Implementation
[0017] 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.
[0018] 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", "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 limiting this invention.
[0019] 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.
[0020] 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.
[0021] Figure 1 This is a schematic flowchart illustrating a method for preparing a novel compound reagent for potassium chloride flotation separation, as provided in an embodiment of the present invention. (See attached diagram.) Figure 1 A method for preparing a novel compound reagent for potassium chloride flotation separation includes the following steps: S1. Mix octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate in a certain proportion, add deionized water, and obtain a mixed solution; 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.
[0022] The stirring speed is 600-1100 r / min.
[0023] In a preferred embodiment, in step S1, the ratio of octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate is 10-13:1-2:0.5-1.
[0024] In a preferred embodiment, in step S2, the acid may be one or more of hydrochloric acid, sulfuric acid, and acetic acid.
[0025] In a preferred embodiment, in step S2, the mass of the acid is 20-50% of octadecylamine.
[0026] In a preferred embodiment, the sodium alkylbenzene sulfonate has a carbon chain number of 8-16.
[0027] In a preferred embodiment, the concentration of the compound drug is 0.5-5%.
[0028] A novel compound reagent for potassium chloride flotation separation is prepared by the above-described preparation method.
[0029] A method for using a novel compound reagent for potassium chloride flotation separation, the method comprising: 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.
[0030] In a preferred embodiment, the concentration of the potash slurry is 30-55%.
[0031] In a preferred embodiment, the amount of the novel compound drug added is 1-25 mg / L.
[0032] Example 1
[0033] In this embodiment, octadecylamine, sodium dodecylbenzenesulfonate, and ethylenediaminetetramethylene phosphate 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.
[0034] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system: 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.
[0035] Prepare a saturated sodium chloride solution by placing 100 ml of the saturated sodium chloride solution in a flotation machine and adding 20 g of sodium chloride. After stirring for 4 min, add 5 mg / L of the above-mentioned 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.
[0036] Comparative Example 1: The process is the same as in Example 1, except that the compound drug is replaced with octadecylamine.
[0037] Table 1. Experimental adsorption and recovery effects of Example 1 and Comparative Example 1
[0038]
[0039] Example 2
[0040] In this embodiment, octadecylamine, sodium hexadecylbenzenesulfonate, and ethylenediaminetetramethylene phosphate are mixed in a ratio of 11:2:1, 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.
[0041] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system: 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 the slurry 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.
[0042] 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 the slurry 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 froth.
[0043] Comparative Example 2: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0044] Table 2. Experimental adsorption and recovery effects of Example 2 and Comparative Example 2
[0045]
[0046] Example 3
[0047] In this embodiment, octadecylamine, sodium octadecylbenzenesulfonate, and ethylenediaminetetramethylene phosphate 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.
[0048] The above-mentioned compound reagents were used to achieve flotation of a single potassium chloride system: 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.
[0049] 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.
[0050] Comparative Example 3: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0051] Table 3. Experimental adsorption and recovery effects of Example 3 and Comparative Example 3
[0052]
[0053] Example 4
[0054] In this embodiment, octadecylamine, sodium alkylbenzenesulfonate, and ethylenediaminetetramethylene phosphate are mixed in a ratio of 9:1:1, 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.
[0055] The above-mentioned compound reagents were used to achieve flotation of the potash ore system: Prepare a saturated solution of the actual mineral sample. The actual mineral sample was sieved to below -0.074 mm. The actual mineral sample used in the experiment was collected from the positive flotation workshop of the Salt Lake Group, and its potassium content was 15.63%. Place 100 ml of the saturated solution of the actual mineral sample into the flotation machine and add 20 g of the actual mineral sample. After stirring the slurry for 4 minutes, add 1 mg / L and 5 mg / L reagents respectively. After adding the reagents, stir for 5 minutes and then start flotation (experimental temperature: 20℃). After drying the flotation froth, calculate the recovery rate.
[0056] Comparative Example 4: The process is the same as in Example 1, except that the reagent is replaced with octadecylamine.
[0057] Table 4. Experimental adsorption and recovery effects of Example 4 and Comparative Example 4
[0058]
[0059] In summary, this invention provides a novel compound reagent for the flotation separation of potassium chloride and its preparation method. Octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate are mixed in a ratio of 10-13:1-2:0.5-1 to prepare the novel compound reagent. Through multi-component functional coupling, it improves solution dispersibility, reduces solution viscosity, and increases flotation efficiency. It can be applied to the flotation separation of potassium chloride under low-temperature conditions. The flotation effect is superior to that of the traditional collector octadecylamine, and the dosage of the compound reagent is less than that of octadecylamine.
[0060] 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 method for preparing a novel compound reagent for potassium chloride flotation separation, characterized in that, The preparation method includes the following steps: S1. Mix octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate in a certain proportion, add deionized water, and obtain a mixed solution; 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.
2. The method for preparing a novel compound reagent for potassium chloride flotation separation according to claim 1, characterized in that, In step S1, the ratio of octadecylamine, sodium alkylbenzene sulfonate, and ethylenediaminetetramethylene phosphate is 10-13:1-2:0.5-1.
3. The method for preparing a novel compound reagent for potassium chloride flotation separation according to claim 1, characterized in that, In step S2, the acid can be one or more of hydrochloric acid, sulfuric acid, and acetic acid.
4. The method for preparing a novel compound reagent for potassium chloride flotation separation according to claim 1, characterized in that, In step S2, the mass of the acid is 20-50% of octadecylamine.
5. The method for preparing a novel compound reagent for potassium chloride flotation separation according to claim 1, characterized in that, The sodium alkylbenzene sulfonate has a carbon chain number of 8-16.
6. The method for preparing a novel compound reagent for potassium chloride flotation separation according to claim 1, characterized in that, The concentration of the compound drug is 0.5-5%.
7. A novel compound reagent for potassium chloride flotation separation prepared by the preparation method according to any one of claims 1-6.
8. A method for using a novel compound reagent for potassium chloride flotation separation, characterized in that, The method of using the novel compound preparation according to claim 7 includes: 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.
9. The method of using the novel compound reagent for potassium chloride flotation separation according to claim 8, characterized in that, The concentration of the potash slurry is 30-55%.
10. The method of using the novel compound reagent for potassium chloride flotation separation according to claim 8, characterized in that, The dosage of the novel compound drug is 1-25 mg / L.