CN115025886A - Lepidolite flotation reagent and application - Google Patents
Lepidolite flotation reagent and application Download PDFInfo
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- CN115025886A CN115025886A CN202210721486.2A CN202210721486A CN115025886A CN 115025886 A CN115025886 A CN 115025886A CN 202210721486 A CN202210721486 A CN 202210721486A CN 115025886 A CN115025886 A CN 115025886A
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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Abstract
The invention relates to the technical field of mineral separation, and provides a lepidolite flotation reagent which comprises the following raw materials in parts by weight: 1-10 parts of ionic liquid, 15-50 parts of polyoxyethylene ether and 10-30 parts of lignin derivative. The flotation reagent disclosed by the invention is applied to lepidolite ore flotation, pH adjustment and inhibitor addition are not needed, the flotation temperature range is wide, the process is simple, the dosage of the flotation reagent is small, the selective collecting capability and the mud resistance are strong, the flotation effect on lepidolite is obvious at low temperature, and the lepidolite flotation recovery effect is greatly improved.
Description
Technical Field
The invention relates to the technical field of mineral separation, and particularly relates to a lepidolite flotation reagent and application thereof.
Background
Lithium and its compounds have a variety of industrial applications, including heat-resistant glasses, ceramics, lithium grease lubricants, flux additives for iron, steel and aluminum production, lithium batteries and lithium ion batteries. Lithium is a strategic value of being an energy metal in the 21 st century. In recent years, the demand of lithium resources is increasing year by year due to the attention of our country to the new energy automobile industry. Lepidolite, the most common lithium-containing mineral, is one of the important minerals for extracting lithium. Therefore, the improvement of the development and utilization level of the lepidolite has important significance for promoting the development of the lithium industry in China.
Patent CN103240185A provides a novel lepidolite flotation method and a combined collector and application thereof. The combined collector XLD-152 comprises, by mass, 1% of dodecylamine or cocoamine, 1-5% of alcohol, 1-2% of hydrochloric acid and 92-97% of water. The lepidolite flotation method comprises tertiary cyclone desliming, primary roughing, secondary concentration and primary scavenging, hydrochloric acid is added before flotation to adjust the pH value of ore pulp to 2-3, collecting agents XLD-152 (rougher flotation 3000-. The flotation process is complex, the dosage of the reagents is large, the applicability of the slime of the collecting agent is poor, inhibitor water glass still needs to be added after three times of desliming to reduce the influence of gangue minerals on lepidolite flotation, and the strong acid flotation environment has the defects of high requirement on equipment corrosion resistance, poor flotation working environment, high wastewater treatment cost and the like. The addition of a large amount of water glass can greatly improve the absolute value of negative potential on the surface of the slime, enhance the electrostatic repulsion force of like charges among fine ore particles in tailings, keep the fine ore particles in a dispersed state and cause difficult tailing water sedimentation.
Patent CN 107008567 a provides a method for separating lepidolite by using laurylamine polyoxyethylene ether as a collecting agent, wherein the separation process comprises secondary cyclone desliming, primary roughing, secondary concentrating and primary scavenging. The method specifically comprises the following steps: crushing raw ore, performing wet ball milling to obtain ore pulp, adjusting the pH to 3-4 by taking sulfuric acid as an adjusting agent, performing flotation separation on the ore pulp by taking laurylamine polyoxyethylene ether as a collecting agent (120-160g/t), and obtaining Li in lepidolite concentrate 2 O grade 3.17%, Li 2 The O recovery rate is 66.38 percent. Although the flotation process has good adaptability to the slime, high Li can be obtained 2 O-grade lepidolite concentrate, but the flotation process is complicated and de-sliming leads to Li 2 Loss of O (Li) 2 Low recovery of O); sulfuric acid is required to be added in all flotation operations to keep the flotation pulp environment of the lepidolite to be strong acid, and the strong acid flotation environment has the defects of high requirement on equipment corrosion resistance, poor flotation working environment, high wastewater treatment cost and the like. In addition, Li in the obtained lepidolite concentrate 2 The grade and recovery of O remains to be improved and further optimization of the collector is required.
Disclosure of Invention
The invention aims to overcome at least one of the defects in the prior art and provide a lepidolite flotation reagent for efficient flotation recovery and application thereof. The purpose of the invention is realized based on the following technical scheme:
in one aspect of the invention, the lepidolite flotation reagent comprises the following raw materials in parts by weight: 3-12 parts of ionic liquid, 15-50 parts of polyoxyethylene ether and 10-30 parts of lignin derivatives;
the ionic liquid is composed of cation and anion, wherein the cation is selected from any one or more of cations shown in formulas 2-1 to 2-11:
wherein, R, R 1 、R 2 、R 3 、R 4 The alkyl group, the substituted alkyl group or the aromatic group with 0-20 carbon atoms are respectively and independently selected, and the substituent of the substituted alkyl group and the aromatic group is respectively and independently selected from one or more of ether group, aldehyde group, ketone group, amino group, alkenyl group, phenyl group, amido group and sulfonic group.
The flotation reagent disclosed by the invention contains an anionic collector, a cationic collector and a non-ionic collector, and the combination of the anionic collector, the cationic collector and the non-ionic collector plays a synergistic effect, so that the flotation and recovery effects of lepidolite are greatly improved.
Heretofore, it has been reported (CN 112058090A) to apply an ionic liquid to an extraction solvent system of lithium, wherein an organic extraction phase includes an extractant, an ionic liquid and a diluent mixed with each other, and a lithium salt solution phase is an aqueous solution of a lithium salt. In view of the extraction promoting effect of the ionic liquid on the lithium salt solution, the ionic liquid is applied to the flotation of the lepidolite mineral, the cation of the lepidolite mineral has a structure similar to that of amine, the lepidolite mineral belongs to a cationic collecting agent, the surface of the lepidolite mineral is negatively charged, the ionic liquid is adsorbed on the surface of the mineral mainly through the electrostatic adsorption effect, and the selectivity is high. By adding a small amount of ionic liquid, the critical micelle concentration of other surfactants is significantly reduced, because electrostatic attraction and hydrophobic interactions between the surfactants can participate in the formation of mixed micelles. The ionic liquid obviously improves the surface activity of the flotation reagent, has a mineral-philic group (cation) and a hydrophobic group (alkyl, double bond and the like), ensures that the flotation reagent has excellent water solubility and dispersibility at low temperature, can reduce the flotation temperature, reduce the dosage of the flotation reagent, improve the flotation effect on lepidolite at low temperature, has strong collecting capability and good selectivity, and improves the grade and the recovery rate of lepidolite ore.
The polyoxyethylene ether belongs to a nonionic surfactant, is easy to dissolve in water, has higher surface activity, and has lower surface tension and lower critical micelle concentration, thereby leading to better wetting, emulsifying, dispersing, permeating, hard water resisting, degreasing and solubilizing abilities. Acid, alkali and high temperature resistance, good chemical stability, high foam eliminating speed and good effect. The ionic liquid does not ionize in water, when the ionic liquid is dispersed on the surface of a dispersoid, a thin film or an electric double layer is formed, the dispersed phase can have charges, small droplets of the dispersed phase are prevented from mutually coagulating, and the polyoxyethylene ether can obviously reduce the surface tension of the dispersoid, so that an emulsification system formed by the ionic liquid and a lignin derivative is more dispersed and stable, has stronger surface activity and lower critical micelle concentration, and simultaneously improves the hydrophilicity of a flotation reagent and enhances the selective collection performance of the flotation reagent; the stability of flotation froth is enhanced, and the flotation froth tension is strengthened. The polyoxyethylene ether has high flotation efficiency, good adaptability to slime, fragile and non-sticky foam, simple preparation and lower cost.
The lignin derivative belongs to an anionic collector, and has lower cost. Lignin is the second most abundant polyphenol polymer in plants, also contains hydroxyl, carbon-based conjugated double bond, carboxyl and aromatic ring structure of polyhydric alcohol, has good diffusion performance, but has poor water solubility, and is obtained by chemical modification such as acetylation, epoxidation, hydroxymethylation, ammoniation and the like, so that the water solubility and electrostatic interaction of the lignin can be enhanced, and the surface activity is improved. The phenolic hydroxyl and the carboxyl enable the lignin derivatives and the lepidolite to generate a strong adsorption effect, the space effect generated by the adsorption layer plays a strong dispersion effect on the lepidolite, flotation ore pulp is effectively dispersed, and the cover of the slime on the surface of the lepidolite is greatly weakened. The lignin derivative is also a high-efficiency inhibitor for gangue minerals (such as calcium carbonate, sodium silicate and barite) such as silicate, sulfate and carbonate, phenolic hydroxyl groups are chemically adsorbed and physically adsorbed on the surface of the gangue minerals, and polar groups such as alcoholic hydroxyl groups and carboxyl groups extend to a medium to be associated with water molecules, so that a strong hydrophilic film is formed on the surface of gangue mineral particles to inhibit the formation of the strong hydrophilic film. Similar to tannin (but the tannin is only an inhibitor), the lignin derivative belongs to an organic polymer material, has large relative molecular mass and high branch and bend degrees, not only forms a hydrophilic layer on the surface of the gangue mineral, but also can cover a hydrophobic layer of a collecting agent on the surface of the gangue mineral, so that the gangue mineral is strongly inhibited. The addition of the lignin derivatives realizes the collection of lepidolite under a neutral condition, and the lepidolite has strong mud resistance and does not need to be deslimed in advance.
Preferably, the ionic liquid, the anion of which is selected from Cl - 、Br - 、[BF 4 ] - 、[HSO 4 ] - 、[PF 6 ] - 、[TFSI] - 、[(SO 2 CF 2 CF 3 ) 2 N] - 、[CF 3 SO 3 ] - 、[CH 3 COO] - One or more of (a).
Preferably, the cation of the ionic liquid is selected from one or more of the cations shown in formulas 2-1, 2-4 and 2-7-2-12, wherein R, R 1 、R 2 、R 3 、R 4 At least one of them includes a substituted alkyl or aryl group having 2 to 20 carbon atoms. More preferably, the substituent of the substituted alkyl or aromatic group includes at least one of an ether group, a ketone group, an alkenyl group, a phenyl group, a sulfonic acid group, or an amide group.
Preferably, the polyoxyethylene ether is fatty amine polyoxyethylene ether. The fatty amine polyoxyethylene ether comprises one or more of AC-1802, AC-1805, AC-1810, AC-1812, AC-1815, AC-1820 and AC-1830. The fatty amine polyoxyethylene ether is dissolved in water, is in a non-ionic type in an alkaline medium or a neutral medium, is in a weak cationic type in an acidic medium, and has excellent level dyeing and diffusion properties. The fatty amine polyoxyethylene ether is used as a collecting agent, so that the flotation efficiency is high, the adaptability to slime is good, foams are fragile and do not become sticky, the preparation of the agent is simple, and the cost is lower. More preferably, the polyoxyethylene ether is a specially prepared AC-1815, which greatly increases the emulsifying and spreading effect.
Preferably, the lignin derivative comprises lignosulphonate and/or aminated enzymatic lignin. The lignosulfonate contains a phenylpropane hydrophobic framework and hydrophilic groups such as sulfonic acid groups, alcoholic hydroxyl groups, carboxyl groups and the like, selective collection is realized, the lignosulfonate is preferably selected to comprise at least one of oxidized lignosulfonate, hydroxymethylated lignosulfonate and sulfomethylated lignosulfonate, the hydroxymethylated lignosulfonate and the sulfomethylated lignosulfonate can improve the surface activity and the foaming capacity of the lignosulfonate, the adsorption capacity and the dispersing capacity of the lignosulfonate can be greatly improved by oxidation, and the sulfomethylated lignosulfonate is inferior. The aminated enzymatic lignin is obtained by reacting enzymatic lignin, lysine and glyoxal, and an amino group is introduced to the ortho-position of a phenolic hydroxyl group of lignin, so that the electrostatic interaction of the lignin can be improved.
In another aspect of the present invention, there is provided a use of a lepidolite flotation reagent in lepidolite ore flotation, comprising: grinding lepidolite raw ore, adding water to prepare ore pulp, adding the lepidolite flotation reagent according to any one of claims 1 to 6 into the ore pulp to serve as a collecting agent, and performing flotation processes of primary roughing, primary scavenging, secondary concentrating and sequential return to obtain lepidolite concentrate.
Preferably, the adding amount of the lepidolite flotation agent in the primary roughing is 100-300 g/t, and roughing concentrate and roughing tailings are obtained; performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 15-50 g/t, so as to obtain scavenged concentrate and scavenged tailings; for the first concentration, the adding amount of a lepidolite flotation reagent is 20-100 g/t, and first concentrated ore concentrate and first concentrated middling are obtained; and (5) performing secondary concentration, namely obtaining second concentrate and second middling of concentration without adding a lepidolite flotation reagent.
Preferably, the temperature of the flotation is 0-40 ℃.
Preferably, the grade of the lepidolite raw ore is not less than 0.4.
The invention can obtain at least one of the following beneficial effects:
the invention is a combined flotation reagent prepared by taking ionic liquid, polyoxyethylene ether and lignin derivatives as raw materials, and does not need to adjust pH and add inhibitionThe agent has the advantages of wide flotation temperature range, simple process, small dosage of flotation agent, strong selective collecting capability and mud resistance, and obvious flotation effect on lepidolite at low temperature; the invention can realize the Li of the raw ore 2 Effective flotation recovery of lepidolite with O grade not less than 0.4, and obtained lepidolite concentrate has grade more than 4, and Li 2 The O recovery rate is more than 70 percent. The ionic liquid obviously improves the surface activity of the flotation reagent, so that the flotation reagent has excellent water solubility and dispersibility at low temperature, the flotation temperature can be reduced, the dosage of the flotation reagent is reduced, the flotation effect on lepidolite at low temperature is improved, the collecting capability is strong, the selectivity is good, and the grade and the recovery rate of lepidolite ore are improved. The polyoxyethylene ether is used as an emulsifier, so that the flotation efficiency is high, the adaptability to slime is good, the foam is fragile and does not become sticky, the preparation of the agent is simple, and the cost is lower; the surface tension of the dispersoid can be obviously reduced, an emulsification system formed by the ionic liquid and the lignin derivative is more dispersed and stable, the surface activity is stronger, the critical micelle concentration is lower, the hydrophilicity of the flotation reagent is improved, and the selective collecting performance of the flotation reagent is enhanced. The lignin derivative belongs to an anionic surfactant and a regulator with strong dispersion and inhibition performance, can effectively weaken the cover of slime on the surface of lepidolite mineral, strengthen the surface collecting effect of a flotation reagent and lepidolite, can also effectively inhibit gangue mineral, realizes desliming flotation, and effectively avoids Li caused by desliming 2 The problem of O loss.
The flotation process of the invention does not need strong acid condition, is more friendly to equipment and environment, and is safe and reliable. The invention also realizes the efficient flotation and recovery of the lepidolite ore at low temperature, improves the grade and recovery rate of the lepidolite ore, solves the technical problems of large using amount of the collecting agent and low grade and recovery rate of lepidolite concentrate caused by poor solubility of the traditional ammonium salt at low temperature, and has good popularization and application values.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a lepidolite flotation reagent which comprises the following raw materials in parts by weight: 3-12 parts of ionic liquid, 15-50 parts of polyoxyethylene ether and 10-30 parts of lignin derivatives. Wherein:
the ionic liquid is composed of a cation and an anion, wherein the cation is selected from any one or more of cations shown in formulas 2-1 to 2-12:
wherein, R, R 1 、R 2 、R 3 、R 4 The organic silicon dioxide is independently selected from alkyl or substituted alkyl or aryl with 0-20 carbon atoms, and the substituent of the substituted alkyl and aryl is independently selected from one or more of ether group, aldehyde group, ketone group, amino group, alkenyl group, amide group and sulfonic group. The anion is selected from Br - 、[BF 4 ] - 、[HSO 4 ] - 、[PF 6 ] - 、[Tf 2 N] - 、[(SO 2 CF 2 CF 3 ) 2 N] - 、[CF 3 SO 3 ] - 、[CH 3 COO] - One or more of (a). Preferably, the cation is selected from one or more of cations shown in formulas 2-1, 2-4 and 2-7-2-12, wherein R, R 1 、R 2 、R 3 、R 4 At least one of them includes a substituted alkyl or aryl group having 2 to 20 carbon atoms. More preferably, the substituent of the substituted alkyl or aromatic group includes at least one of an ether group, a ketone group, an alkenyl group, a phenyl group, a sulfonic acid group, and an amide group.
The polyoxyethylene ether is fatty amine polyoxyethylene ether, and comprises one or more of AC-1802, AC-1805, AC-1810, AC-1812, AC-1815, AC-1820 and AC-1830. More preferably, the polyoxyethylene ether is a specially prepared AC-1815, which greatly increases the emulsifying and spreading effect.
The lignin derivative comprises lignosulphonate and/or aminated enzymatic lignin, preferably lignosulphonate comprising oxidized, hydroxymethylated and sulfomethylated lignosulphonate, and the aminated enzymatic lignin is obtained by reacting enzymatic lignin, lysine and glyoxal.
The application of the lepidolite flotation reagent will be described below with reference to specific examples.
Li of raw ore 2 The grade of O is more than or equal to 0.4, the ball milling is carried out until the granularity is minus 200 meshes and accounts for 75 percent, and water is added for size mixing until the mass concentration is 30 percent. The dosage of the flotation reagent is calculated by the mass of the raw ore.
Example 1
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 4 parts of ionic liquid, AC-180220 parts and 11 parts of sodium hydroxymethylated lignin sulfonate. Wherein, the structure of the ionic liquid is as follows:
flotation test: li of raw ore 2 The O content is 0.43 percent, the lepidolite raw ore is ground and added with water to prepare ore pulp, and the ore pulp is poured into a flotation tank to carry out flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 120g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 20g/t, and obtaining scavenged concentrate and scavenged tailings;
3) for the first time of concentration, the adding amount of a lepidolite flotation reagent is 50g/t, so that concentrated first concentrate and concentrated first middlings are obtained, and the concentrated first middlings are returned to the first roughing process;
4) and (4) carrying out secondary concentration, namely, concentrating the first concentrate without adding a lepidolite flotation agent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 20. + -. 3 ℃ and 5. + -. 3 ℃ without changing other conditions. Flotation results at each temperature were as follows:
TABLE 1
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 4.21 | 72.18 |
| 20±3℃ | 4.18 | 71.54 |
| 5±3℃ | 4.09 | 70.72 |
Example 2
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 9 parts of ionic liquid, AC-181535 parts, 10 parts of hydroxymethylation sodium lignin sulfonate and 10 parts of amination enzymatic hydrolysis lignin. Wherein, the amination lignin is obtained by the reaction of enzymolysis lignin, lysine and glyoxal; the structure of the ionic liquid is as follows:
Flotation test: li of raw ore 2 The O content is 0.47 percent, the lepidolite raw ore is ground and added with water to prepare ore pulp, and the ore pulp is poured into a flotation tank to carry out flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 150g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 30g/t, and obtaining scavenged concentrate and scavenged tailings;
3) first concentration, namely, concentrating the scavenging concentrate, wherein the adding amount of the lepidolite flotation reagent is 60g/t, so that first concentrated concentrate and first concentrated middlings are obtained, and the first concentrated middlings are returned to the first roughing process;
4) and (4) carrying out secondary concentration, namely, concentrating the first concentrate without adding a lepidolite flotation agent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 25. + -. 3 ℃ and 15. + -. 3 ℃ and 5. + -. 3 ℃ without changing other conditions. The flotation results at each temperature were as follows:
TABLE 2
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 4.81 | 77.53 |
| 20±3℃ | 4.64 | 75.15 |
| 5±3℃ | 4.22 | 72.83 |
Example 3
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 8 parts of ionic liquid AC-181240 parts and 25 parts of sulfomethylated sodium lignosulfonate. Wherein, the structure of the ionic liquid is as follows:
flotation test: li of raw ore 2 The O content is 0.57 percent, the lepidolite raw ore is ground and added with water to prepare ore pulp, and the ore pulp is poured into a flotation tank to carry out flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 200g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 25g/t, and obtaining scavenged concentrate and scavenged tailings;
3) first concentration, namely, concentrating the scavenging concentrates, wherein the adding amount of the lepidolite flotation reagent is 60g/t, so that first concentrated concentrate and first concentrated middlings are obtained, and the first concentrated middlings are returned to the first roughing process;
4) and (4) carrying out secondary concentration, namely, concentrating the first concentrate without adding a lepidolite flotation agent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 25. + -. 3 ℃ and 15. + -. 3 ℃ and 5. + -. 3 ℃ without changing other conditions. Flotation results at each temperature were as follows:
TABLE 3
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 4.45 | 72.74 |
| 20±3℃ | 4.31 | 73.09 |
| 5±3℃ | 4.13 | 71.47 |
Example 4
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 11 parts of ionic liquid AC-183045 parts and 15 parts of sodium lignin oxide sulfonate. Wherein, the structure of the ionic liquid is as follows:
flotation test: li of raw ore 2 The content of O is 0.66 percent,grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 225g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 50g/t, and obtaining scavenged concentrate and scavenged tailings;
3) first concentration, namely, concentrating the scavenging concentrate, wherein the adding amount of the lepidolite flotation reagent is 100g/t, so that first concentrated concentrate and first concentrated middlings are obtained, and the first concentrated middlings are returned to the first roughing process;
4) and (4) carrying out secondary concentration, namely, concentrating the first concentrate without adding a lepidolite flotation agent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 25. + -. 3 ℃ and 15. + -. 3 ℃ and 5. + -. 3 ℃ without changing other conditions. Flotation results at each temperature were as follows:
TABLE 4
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 4.32 | 71.36 |
| 20±3℃ | 4.20 | 71.02 |
| 5±3℃ | 4.03 | 70.38 |
Example 5
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 5.5 parts of ionic liquid, AC-181050 parts, 15 parts of amination enzymatic hydrolysis lignin and 15 parts of sodium lignin oxide sulfonate. Wherein, the amination lignin is obtained by the reaction of enzymolysis lignin, lysine and glyoxal; the ionic liquid is C 12 mimBr。
Flotation test: li of raw ore 2 The O content is 0.53 percent, the lepidolite raw ore is ground and added with water to prepare ore pulp, and the ore pulp is poured into a flotation tank to carry out flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 250g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 40g/t, so as to obtain scavenged concentrate and scavenged tailings;
3) first concentration, namely, concentrating the scavenging concentrate, wherein the adding amount of the lepidolite flotation reagent is 30g/t, so that first concentrated concentrate and first concentrated middling are obtained, and the first concentrated middling returns to the first roughing process;
4) and (4) performing secondary concentration, namely performing concentration on the first concentrate without adding a lepidolite flotation reagent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 25. + -. 3 ℃ and 15. + -. 3 ℃ and 5. + -. 3 ℃ without changing other conditions. The flotation results at each temperature were as follows:
TABLE 5
Example 6
The lepidolite flotation reagent provided by the embodiment comprises the following raw materials in parts by weight: 7 parts of ionic liquid, AC-182040 parts, 15 parts of hydroxymethylation sodium lignosulphonate and 20 parts of amination enzymatic hydrolysis lignin. Wherein the aminated lignin is obtained by reacting enzymolysis lignin, lysine and glyoxal; the ionic liquid is 1-propenyl-3-butyl imidazole acetate.
Flotation test: li of raw ore 2 The O content is 0.95 percent, the lepidolite raw ore is ground and added with water to prepare ore pulp, and the ore pulp is poured into a flotation tank to carry out flotation test (the flotation temperature is 35 +/-3 ℃).
1) Performing primary roughing, wherein the adding amount of a lepidolite flotation agent is 180g/t, and obtaining roughed concentrate and roughed tailings;
2) performing primary scavenging, namely scavenging the rougher tailings, wherein the addition amount of the lepidolite flotation agent is 35g/t, and obtaining scavenged concentrate and scavenged tailings;
3) first concentration, namely, concentrating the scavenging concentrate, wherein the adding amount of the lepidolite flotation reagent is 80g/t, so that first concentrated concentrate and first concentrated middlings are obtained, and the first concentrated middlings are returned to the first roughing process;
4) and (4) carrying out secondary concentration, namely, concentrating the first concentrate without adding a lepidolite flotation agent to obtain second concentrate and second middlings, and returning the second middlings to the primary concentration process.
The lepidolite ore was floated at 25. + -. 3 ℃ and 15. + -. 3 ℃ and 5. + -. 3 ℃ without changing the other conditions. Flotation results at each temperature were as follows:
TABLE 6
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery rate/%) | |
| 35±3℃ | 4.53 | 76.31 |
| 20±3℃ | 4.58 | 75.65 |
| 5±3℃ | 4.33 | 72.97 |
Comparative example 1
The ionic liquid was replaced with dodecylamine (a conventional cationic collector) and the rest of the experimental conditions were the same as in example 1. The flotation results at each temperature were as follows:
TABLE 8
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 3.22 | 35.54 |
| 20±3℃ | 3.04 | 33.78 |
| 5±3℃ | 2.35 | 23.85 |
Comparative example 2
The lignin derivatives were replaced by tannins (inhibitors) and the rest of the experimental conditions were the same as in example 1. Flotation results at each temperature were as follows:
TABLE 9
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery rate/%) | |
| 35±3℃ | 3.82 | 52.51 |
| 20±3℃ | 3.67 | 49.74 |
| 5±3℃ | 3.75 | 50.32 |
Comparative example 3
The ionic liquid was removed and the rest of the experimental conditions were the same as in example 1. Flotation results at each temperature were as follows:
TABLE 11
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery rate/%) | |
| 35±3℃ | 2.34 | 32.41 |
| 20±3℃ | 2.23 | 26.75 |
| 5±3℃ | 1.45 | 20.11 |
Comparative example 4
The lignin derivatives were removed and the rest of the experimental conditions were the same as in example 1. Flotation results at each temperature were as follows:
TABLE 12
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrate Li 2 O recovery/The | |
| 35±3℃ | 3.31 | 50.22 |
| 20±3℃ | 3.28 | 48.52 |
| 5±3℃ | 3.24 | 49.03 |
Comparative example 5
The polyoxyethylene ether was removed and the experimental conditions were the same as in example 1. The flotation results at each temperature were as follows:
TABLE 11
| Lepidolite concentrate Li 2 O grade/% | Lepidolite concentrateLi 2 O recovery/The | |
| 35±3℃ | 2.11 | 22.54 |
| 20±3℃ | 2.02 | 23.12 |
| 5±3℃ | 1.96 | 20.31 |
The flotation reagent disclosed by the invention is wide in flotation temperature range, strong in selective collecting capability and mud resistance, and remarkable in flotation effect on lepidolite ore under a low-temperature condition; the obtained lepidolite concentrate has a grade of more than 4, and Li 2 The recovery rate of O is more than 70 percent, and particularly, the flotation effect of the embodiment 2 is best. The results of comparing example 1 with comparative examples 1 to 5 show that the ionic liquid is resistant to Li at low temperature 2 The grade and the recovery rate of O have the greatest influence, and the low-temperature performance of the flotation reagent can be improved; lignin derivatives vs. Li 2 The grade and the recovery rate of O have certain influence, and the influence on the grade is larger; polyoxyethylene ethers to Li over a wide temperature range 2 The grade and recovery of O play a decisive role.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A lepidolite flotation reagent is characterized by comprising the following raw materials in parts by weight: 3-12 parts of ionic liquid, 15-50 parts of polyoxyethylene ether and 10-30 parts of lignin derivatives;
the ionic liquid is composed of cation and anion, wherein the cation is selected from any one or more of cations shown in formulas 2-1 to 2-12:
wherein, R, R 1 、R 2 、R 3 、R 4 The alkyl group, the substituted alkyl group or the aromatic group with 0-20 carbon atoms are respectively and independently selected, and the substituent of the substituted alkyl group and the aromatic group is respectively and independently selected from one or more of ether group, aldehyde group, ketone group, amino group, alkenyl group, phenyl group, amide group and sulfonic group.
2. A lepidolite flotation reagent according to claim 1 wherein the ionic liquid has an anion selected from the group consisting of Cl - 、Br - 、[BF 4 ] - 、[HSO 4 ] - 、[PF 6 ] - 、[TFSI] - 、[(SO 2 CF 2 CF 3 ) 2 N] - 、[CF 3 SO 3 ] - 、[CH 3 COO] - One or more of (a).
3. A lepidolite flotation reagent according to claim 2 wherein the ionic liquid has a cation selected from one or more of the cations of formulae 2-1, 2-4, 2-7 to 2-12 wherein R, R 1 、R 2 、R 3 、R 4 At least one of them includes a substituted alkyl group or an aryl group having 2 to 20 carbon atoms.
4. The lepidolite flotation reagent of claim 1 wherein the polyoxyethylene ether is a fatty amine polyoxyethylene ether.
5. A lepidolite flotation agent according to claim 4 wherein said fatty amine polyoxyethylene ether comprises one or more of AC-1802, AC-1805, AC-1810, AC-1812, AC-1815, AC-1820, AC-1830.
6. A lepidolite flotation reagent according to claim 1 wherein the lignin derivative comprises lignosulfonate and/or aminated enzymatic lignin.
7. The application of a lepidolite flotation reagent in lepidolite ore flotation is characterized in that lepidolite raw ore is ground and added with water to prepare ore pulp, the lepidolite flotation reagent according to any one of claims 1 to 6 is added into the ore pulp to serve as a collecting agent, and a flotation process of primary roughing, primary scavenging, secondary concentration and sequential return is adopted to obtain lepidolite concentrate.
8. The application of the lepidolite flotation reagent according to claim 7, wherein the lepidolite flotation reagent is added in an amount of 100-300 g/t in the primary roughing to obtain a roughed concentrate and roughed tailings; performing primary scavenging, namely performing scavenging on the rougher tailings, wherein the adding amount of the lepidolite flotation agent is 15-50 g/t, and obtaining scavenged concentrate and scavenged tailings; for the first time of concentration, the adding amount of a lepidolite flotation reagent is 20-100 g/t, and first concentration concentrate and first concentration middling are obtained; and (5) performing secondary concentration, namely obtaining second concentrate and second middling of concentration without adding a lepidolite flotation reagent.
9. The use of a lepidolite flotation reagent according to claim 7 wherein the temperature of the flotation is 0 to 40 ℃.
10. The use of a lepidolite flotation reagent according to claim 7 wherein the grade of the lepidolite ore is not less than 0.4.
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