CN113369021A - Fluorite anion-nonionic association body collecting agent, preparation method and application method thereof - Google Patents
Fluorite anion-nonionic association body collecting agent, preparation method and application method thereof Download PDFInfo
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- CN113369021A CN113369021A CN202110506111.XA CN202110506111A CN113369021A CN 113369021 A CN113369021 A CN 113369021A CN 202110506111 A CN202110506111 A CN 202110506111A CN 113369021 A CN113369021 A CN 113369021A
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- fluorite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/018—Mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/002—Inorganic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/007—Modifying reagents for adjusting pH or conductivity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a fluorite anion-nonionic association body collecting agent, a preparation method and an application method thereof, and the method adopts a method of assembling an oleic acid anion surfactant and an alkylamide nonionic surfactant interface, oleic acid and alkylamide are mixed according to different proportions, stirred for 30-60min at a constant temperature of 60-80 ℃ until being fully dissolved, so that the anion-nonionic association body collecting agent is obtained, and is applied to flotation of fluorite and calcite. The invention utilizes the synergistic capability of the nonionic surfactant, effectively improves the selectivity and the adaptability of the oleic acid anion collecting agent, creates conditions for the flotation separation of fluorite and calcite, and has important significance for the efficient recycling of associated fluorite resources.
Description
Technical Field
The invention relates to a preparation method of an assembled collecting agent, in particular to preparation of an anionic-nonionic collecting agent and application of the anionic-nonionic collecting agent in a fluorite flotation process, and belongs to the technical field of preparation and application of mineral flotation collecting agents.
Background
Fluorite is a non-renewable non-metallic mineral resource, is known as the second rare earth, and has calcium fluoride (CaF) as the main component2) The mineral resource is an important strategic mineral resource and is widely applied to traditional industries such as metallurgy, chemical industry and building materials, and emerging industries such as new energy and new materials. China is the largest fluorite producing country in the world and also the largest fluorite consuming country in the world, and with the rapid development of national economy, the market demand of fluorite is increased rapidly. China is in the Pacific ocean mineralization zone, fluorite resources are rich, but high-quality fluorite reserves are few, the reserves of multi-metal complex associated fluorite are large, and the complex associated fluorite gradually becomes a main body for developing and utilizing the fluorite resources along with the increasing exhaustion of the reserves of the high-quality single fluorite resources.
However, the mineral co-association embedding relationship of the associated fluorite is complex, the gangue minerals are various, the traditional oleic acid anion collecting agent is poor in selectivity, weak in adaptability and insufficient in low-temperature resistance, and the influence of factors such as calcium-containing gangue minerals, temperature, water quality and impurity ions on fluorite flotation is difficult to overcome, so that the recovery efficiency of the associated fluorite is low. Therefore, the development of a complex associated fluorite high-efficiency flotation collector is urgently needed, the comprehensive utilization rate of fluorite resources is improved, and the healthy sustainable development of the fluorite industry in China is promoted.
According to the method, an oleic acid anionic surfactant and an alkylamide nonionic surfactant interface are assembled, oleic acid and alkylamide are mixed in different proportions, and are stirred for 30-60min at a constant temperature of 60-80 ℃ until the oleic acid and the alkylamide nonionic surfactant are fully dissolved, so that an anionic-nonionic association body collecting agent is obtained and is applied to flotation of fluorite and calcite. The invention utilizes the synergistic capability of the nonionic surfactant, effectively improves the selectivity and the adaptability of the oleic acid anion collecting agent, creates conditions for the flotation separation of fluorite and calcite, and has important significance for the efficient recycling of associated fluorite resources.
Disclosure of Invention
In view of the above, the invention aims to provide a fluorite anionic-nonionic associated body collector, a preparation method and an application method thereof, and the fluorite anionic-nonionic associated body collector is prepared by adopting an interfacial assembly method of oleic acid anionic surfactant and alkylamide nonionic surfactant, mixing oleic acid and alkylamide in different proportions, stirring for 30-60min at a constant temperature of 60-80 ℃ until the oleic acid and the alkylamide are fully dissolved to obtain the anionic-nonionic associated body collector, and is applied to flotation of fluorite and calcite. The selectivity and the adaptability of the oleic acid anion collecting agent are effectively improved by utilizing the synergistic capability of the nonionic surfactant.
In order to achieve the purpose, the technical scheme is as follows:
a fluorite anion-nonionic association body collector is characterized by comprising oleic acid, sodium hydroxide and alkylamide nonionic surfactants.
Further, the alkyl amide nonionic surfactant is a surfactant with different hydrocarbon chain structures, such as palmitic acid amide, oleic acid amide and erucic acid amide.
A preparation method of a fluorite anion-nonionic associated body collecting agent is characterized by comprising the following steps: respectively and fully mixing oleic acid, sodium hydroxide and alkylamide according to a certain molar ratio, adding a proper amount of water, and stirring at a certain temperature until the mixture is fully dissolved to obtain the fluorite anion-nonionic associated body collecting agent.
Further, the molar ratio of the oleic acid to the sodium hydroxide to the alkylamide is in the range of 9-6: 9-6: 1-4, wherein the molar ratio of the oleic acid to the sodium hydroxide is the same.
Further, the stirring temperature is 60-80 ℃.
Further, the stirring time is 30-60 min.
The application method of the fluorite anionic-nonionic associated body collector is characterized in that the fluorite anionic-nonionic associated body collector can be used for flotation of fluorite and calcite minerals.
Further, the application method comprises the following steps:
s1: preparing a fluorite anion-nonionic associated body collecting agent according to the proportion;
s2: weighing fluorite or calcite minerals, adding deionized water, adjusting the pH value of ore pulp, and adding a proper amount of fluorite anion-nonionic associated body collecting agent for flotation;
s3: and respectively filtering, drying and weighing the foam product and the tailings, and calculating the recovery rate of fluorite or calcite.
Further, the fluorite anion-nonionic association collector preparation concentration in the step S1 is 8 × 10-4mol/L-2.4×10-3mol/L。
Further, in the step S2, the granularity of the fluorite or calcite mineral is 0.038mm-0.074mm, the flotation pH is 7-8, the pH regulator is hydrochloric acid or sodium carbonate solution with the concentration of 1%, and the dosage of the anionic-nonionic associated body collector is 2-6 multiplied by 10-5mol/L。
Has the advantages that:
the invention has the beneficial effects that:
(1) according to the invention, the anionic-nonionic surfactant is assembled and compounded, and the selectivity, low temperature resistance and hard water resistance of the oleic acid anionic collector are improved by using the low temperature resistance, hard water resistance and other properties of the alkylamide nonionic surfactant;
(2) the invention utilizes the synergistic effect of different surfactants, improves the collecting performance of the traditional oleic acid collecting agent, and creates conditions for the efficient recovery of complex associated fluorite;
(3) the anionic-nonionic associated complex collecting agent provided by the invention is simple in preparation process and wide in application range, and effectively solves the problem that complex associated fluorite, calcite and other calcium-containing minerals are difficult to separate efficiently.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1: flotation of monomineral ores
Oleic acid, sodium hydroxide and oleamide are mixed according to the proportion of 9:9:1, 8:8:2, 7:7:3 and 6:6:4 respectively to prepare the mixture with the concentration of 8 multiplied by 10-4And (3) mol/L, stirring for 30min at the constant temperature of 60 ℃ until the anion-nonionic associated body collector is fully dissolved, and obtaining the anion-nonionic associated body collector. Oleic acid and sodium hydroxide are mixed according to the molar ratio of 1:1 to prepare the mixture with the concentration of 8 multiplied by 10-4And (3) mol/L, stirring for 30min at the constant temperature of 60 ℃ until the sodium oleate is fully dissolved, and obtaining the single anionic sodium oleate collecting agent. In the fluorite and calcite single-mineral flotation experiment, an XFG hanging tank flotation machine is adopted, 2g of fluorite pure mineral with the granularity of 0.038mm-0.074mm is weighed, 40mL of deionized water is added, hydrochloric acid or sodium carbonate solution with the concentration of 1% is used for adjusting the pH value of ore pulp to 7 after stirring for 3min, then the anion-nonionic association body collecting agent or the single anion sodium oleate collecting agent is added, and flotation is carried out after stirring for 3 min. The concentration of the collecting agent is 2 multiplied by 10 and can be obtained through pure mineral flotation experiments-5When mol/L is adopted, when single sodium oleate is used as a collecting agent, the recovery rates of fluorite and calcite are both more than 80%, the recovery rate of calcite is higher than that of fluorite, the difference between the recovery rates of fluorite and calcite reaches the maximum by adopting an anionic-nonionic association body collecting agent with the ratio of 8:8:2, at the moment, the recovery rate of fluorite is 80%, and the recovery rate of calcite is reduced to be less than 40%. The result shows that the anionic-nonionic associated collector shows good selectivity and weaker collecting capability on calcite compared with a single sodium oleate anionic collector, and is beneficial to flotation separation of fluorite and calcite.
Example 2: flotation of monomineral ores
Oleic acid, sodium hydroxide and oleamide are mixed according to the proportion of 9:9:1, 8:8:2, 7:7:3 and 6:6:4 respectively to prepare the mixture with the concentration of 2.4 multiplied by 10-3And (3) mol/L, stirring for 60min at the constant temperature of 80 ℃ until the anion-nonionic associated body collector is fully dissolved, and obtaining the anion-nonionic associated body collector. Oleic acid and sodium hydroxide are mixed according to the molar ratio of 1:1 to prepare the mixture with the concentration of 2.4 multiplied by 10-3mol/And L, stirring for 60min at the constant temperature of 80 ℃ until the sodium oleate is fully dissolved, thereby obtaining the single anionic sodium oleate collecting agent. In the fluorite and calcite single-mineral flotation experiment, an XFG hanging tank flotation machine is adopted, 2g of calcite pure mineral with the granularity of 0.038-0.074 mm is weighed, 40mL of deionized water is added, hydrochloric acid or sodium carbonate solution with the concentration of 1% is used for adjusting the pH value of ore pulp to 8 after stirring for 3min, then the anion-nonionic association body collecting agent or the single anion sodium oleate collecting agent is added, and flotation is carried out after stirring for 3 min. The concentration of the collecting agent is 6 multiplied by 10 and can be obtained through pure mineral flotation experiments-5When the mol/L ratio is higher than that of fluorite, the recovery rates of fluorite and calcite are both more than 90%, and the recovery rate of calcite is higher than that of fluorite, and the difference between the recovery rates of fluorite and calcite is the largest by adopting the anionic-nonionic association body collecting agent with the ratio of 8:8:2, at the moment, the recovery rate of fluorite is 90%, and the recovery rate of calcite is reduced to be less than 50%. The result shows that the anionic-nonionic associated collector shows good selectivity and weaker collecting capability on calcite compared with a single sodium oleate anionic collector, and is beneficial to flotation separation of fluorite and calcite.
Example 3: flotation of complex minerals
Taking certain tungsten and molybdenum associated fluorite from Chenzhou, Hunan province as research object, CaF in raw ore215% of CaCO3The content is 8%, and the main gangue minerals are garnet, calcite, feldspar and quartz. Mixing oleic acid, sodium hydroxide and oleamide according to the molar ratio of 9:9:1, 8:8:2, 7:7:3 and 6:6:4, stirring for 60min in a constant-temperature water bath kettle at 80 ℃ until the mixture is fully dissolved, and preparing the anion-nonionic associative body collecting agent with the concentration of 5%. The fluorite rough concentration adopts sodium carbonate as a pH regulator, water glass as an inhibitor and an anion-nonionic association body collector, the flotation pH is 9.5-10, the water glass dosage is 2000g/t, the collector dosage is 350g/t, the concentration adopts acidified water glass as the inhibitor, and a 1-coarse-1-sweep-5-fine flotation process is adopted. The result shows that when the ratio is 8:8:2, the selectivity of the anion-nonionic associated body collecting agent is the best, the grade and the recovery rate of fluorite are both the highest, at the moment, the grade of fluorite concentrate is more than 90%, and the recovery rate is 65%. The results show that the method has the advantages of high yield,the anion-nonionic associated collector shows good collecting capacity and selectivity, is beneficial to separation of fluorite and calcite in a concentration stage, and can realize high-efficiency recovery rate utilization of complex associated fluorite.
Example 4: flotation of complex minerals
Taking certain tungsten and molybdenum associated fluorite from Chenzhou, Hunan province as research object, CaF in raw ore215% of CaCO3The content is 8%, and the main gangue minerals are garnet, calcite, feldspar and quartz. Mixing oleic acid and sodium hydroxide according to a molar ratio of 1:1, preparing the concentration to be 5%, and stirring for 60min in a constant-temperature water bath kettle at 80 ℃ until the oleic acid and the sodium hydroxide are fully dissolved to obtain the sodium oleate anion collecting agent. The fluorite roughing adopts sodium carbonate as a pH regulator, water glass as an inhibitor, sodium oleate as a collecting agent, the flotation pH is 9.5-10, the using amount of the water glass is 2000g/t, the using amount of the collecting agent is 350g/t, the concentration adopts acidified water glass as the inhibitor, and a 1-coarse-1-sweep-5-fine flotation process is adopted. The result shows that compared with the anion-nonionic associated collector, the single sodium oleate collector has poor selectivity, calcium-containing gangue minerals such as calcite and the like are difficult to inhibit, the fluorite concentrate grade is only 85%, and the recovery rate is 60%. The result shows that the selectivity of the single sodium oleate anion collecting agent is poor, and the high-efficiency separation of the complicated accompanying fluorite and the calcite cannot be realized.
In conclusion, the invention discloses a fluorite anionic-nonionic associated body collecting agent, a preparation method and an application method thereof, wherein an oleic acid anionic surfactant and alkyl amide nonionic surfactant are adopted for interface assembly, oleic acid and alkyl amide are mixed according to different proportions, and are stirred for 30-60min at the constant temperature of 60-80 ℃ until being fully dissolved, so that the anionic-nonionic associated body collecting agent is obtained and is applied to flotation of fluorite and calcite. The invention utilizes the synergistic capability of the nonionic surfactant, effectively improves the selectivity and the adaptability of the oleic acid anion collecting agent, creates conditions for the flotation separation of fluorite and calcite, and has important significance for the efficient recycling of associated fluorite resources.
Although the present invention has been described with reference to the above embodiments, it should be understood that the present invention is not limited to the above embodiments, and those skilled in the art can make various changes and modifications without departing from the scope of the present invention.
Claims (10)
1. A fluorite anion-nonionic association body collector is characterized by comprising oleic acid, sodium hydroxide and alkylamide nonionic surfactants.
2. A fluorite anionic-nonionic associative collector as claimed in claim 1, wherein said alkylamide nonionic surfactant is a surfactant having different hydrocarbon chain structures such as palmitamide, oleamide, erucamide and the like.
3. A preparation method of a fluorite anion-nonionic associated body collecting agent is characterized by comprising the following steps: respectively and fully mixing oleic acid, sodium hydroxide and alkylamide according to a certain molar ratio, adding a proper amount of water, and stirring at a certain temperature until the mixture is fully dissolved to obtain the fluorite anion-nonionic associated body collecting agent.
4. A method of making a fluorite anionic-nonionic associative collector according to claim 3, wherein said oleic acid, sodium hydroxide, and alkylamide are present in a molar ratio ranging from 9 to 6: 9-6: 1-4, wherein the molar ratio of the oleic acid to the sodium hydroxide is the same.
5. A method of preparing a fluorite anionic-nonionic associative collector according to claim 3, wherein said agitation temperature is in the range of 60 to 80 ℃.
6. The method of preparing a fluorite anionic-nonionic associative collector according to claim 3, wherein said agitation time is 30-60 min.
7. The application method of the fluorite anionic-nonionic associated body collector is characterized in that the fluorite anionic-nonionic associated body collector can be used for flotation of fluorite and calcite minerals.
8. An application method of a fluorite anion-nonionic associated body collector is characterized by comprising the following steps:
s1: preparing a fluorite anion-nonionic associated body collecting agent according to the proportion;
s2: weighing fluorite or calcite minerals, adding deionized water, adjusting the pH value of ore pulp, and adding a proper amount of fluorite anion-nonionic associated body collecting agent for flotation;
s3: and respectively filtering, drying and weighing the foam product and the tailings, and calculating the recovery rate of fluorite or calcite.
9. The method of using a fluorite anionic-nonionic associative collector according to claim 8, wherein said fluorite anionic-nonionic associative collector is formulated at a concentration of 8 x 10 in step S1-4mol/L-2.4×10-3mol/L。
10. The method of claim 8 wherein said fluorite or calcite mineral of step S2 has a particle size of 0.038mm to 0.074mm, a flotation pH of 7 to 8, a pH adjusting agent of 1% hydrochloric acid or sodium carbonate solution, and the amount of anionic-nonionic associative collector is 2 to 6 x 10-5mol/L。
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Application publication date: 20210910 |