CN115025886B - Lepidolite flotation reagent and application - Google Patents
Lepidolite flotation reagent and application Download PDFInfo
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- CN115025886B CN115025886B CN202210721486.2A CN202210721486A CN115025886B CN 115025886 B CN115025886 B CN 115025886B CN 202210721486 A CN202210721486 A CN 202210721486A CN 115025886 B CN115025886 B CN 115025886B
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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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 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 floatation effect on lepidolite at low temperature is remarkable, and the floatation recovery effect of lepidolite is greatly improved.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a lepidolite flotation reagent and application.
Background
Lithium and its compounds have a variety of industrial applications including heat resistant glass, ceramics, lithium grease lubricants, flux additives for iron, steel and aluminum production, lithium batteries and lithium ion batteries. Lithium is a very strategic value as an energy metal in the 21 st century. In recent years, the importance of the new energy automobile industry in China has led to the increase of the demand of lithium resources year by year. Lepidolite, the most common lithium-containing mineral, is one of the important minerals for lithium extraction. Therefore, the improvement of the development and utilization level of lepidolite is of great significance in promoting the development of the lithium industry in China.
Patent CN103240185a provides a novel lepidolite flotation process and a combined collector and use 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 three-time cyclone desliming, primary roughing, secondary concentration and primary scavenging, hydrochloric acid is added to adjust the pH value of ore pulp to 2-3 before flotation, a collector XLD-152 (roughing 3000-4800g/t and scavenging 1000-2000 g/t) is added in roughing and scavenging operations, and water glass (150-300 g/t in total) is added in concentrating operations to serve as gangue inhibitors. The flotation process is complex, the dosage of the agent is large, the applicability of the mineral mud of the collector is poor, inhibitor water glass is still required to be added after three desliming to reduce the influence of gangue minerals on lepidolite flotation, and the strong acid flotation environment has the defects of high corrosion resistance requirement on equipment, 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 ore slurry, enhance electrostatic repulsive force of like charges among fine ore particles in the tailings, keep the fine ore particles in a dispersed state, and cause difficult sedimentation of the tailings water.
Patent CN 107008567A provides a method for using laurylamine polyoxyethylene ether as collectorLepidolite is selected by a secondary cyclone desliming process, a primary roughing process, a secondary refining process and a primary scavenging process. The method specifically comprises the following steps: crushing raw ore, performing wet ball milling to obtain ore pulp, adjusting pH to 3-4 by taking sulfuric acid as an adjusting agent, and performing flotation separation on the ore pulp by taking laurylamine polyoxyethylene ether as a collecting agent (120-160 g/t) to obtain Li in lepidolite concentrate 2 O grade 3.17%, li 2 The recovery rate of O is 66.38%. Although the flotation process has good adaptability to mineral mud, high Li can be obtained 2 The lepidolite concentrate of O grade, but the flotation process is complex, desliming leads to Li 2 O loss (Li) 2 O recovery is low); and all flotation operations need to add sulfuric acid to keep the environment of the floatation ore pulp of the lepidolite to be strong acid, and the strong acid floatation environment has the defects of high corrosion resistance requirement on equipment, poor floatation working environment, high wastewater treatment cost and the like. In addition, li in the obtained lepidolite concentrate 2 The grade and recovery of O still need 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 and shortcomings of the prior art and provides a lepidolite flotation reagent for efficient flotation recovery and application. The invention is realized based on the following technical scheme:
the invention aims at providing 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 derivative;
the ionic liquid consists of cations and anions, wherein the cations are selected from any one or more of cations shown in formulas 2-1 to 2-11:
therein, R, R 1 、R 2 、R 3 、R 4 Each independently selected from alkyl groups having 0 to 20 carbon atoms or substituted alkyl groups or aromatic groups, the substituents of the substituted alkyl groups and the aromatic groups each independently selected from ether groups, aldehyde groupsOne or more of a ketone group, an amine group, an alkenyl group, a phenyl group, an amide group, and a sulfonic acid group.
The flotation reagent provided by the invention comprises the anionic collector, the cationic collector and the nonionic collector, and the combination of the three components plays a synergistic role, so that the lepidolite flotation recovery effect is greatly improved.
Heretofore, it has been reported (CN 112058090 a) that an ionic liquid is applied to an extraction solvent system for lithium, wherein the organic extraction phase comprises an extractant, an ionic liquid and a diluent mixed with each other, and the lithium salt solution phase is an aqueous solution of lithium salt. In view of the extraction promotion effect of the ionic liquid on the lithium salt solution, the ionic liquid is applied to floatation of lepidolite minerals, cations of the ionic liquid have a structure similar to amines, the ionic liquid belongs to a cationic collector, the surface of the lepidolite minerals is negatively charged, and the ionic liquid is mainly adsorbed on the surface of the minerals through electrostatic adsorption, so that 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 interaction between surfactants can participate in forming mixed micelles. The ionic liquid obviously improves the surface activity of the flotation reagent, has both mineral-philic groups (cations) and hydrophobic groups (alkyl, double bonds and the like), ensures that the flotation reagent has excellent water solubility and dispersibility at low temperature, can reduce the flotation temperature, reduces the dosage of the flotation reagent, improves the flotation effect on lepidolite at low temperature, has strong collecting capability and good selectivity, and improves the grade and 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 critical micelle concentration, so that the polyoxyethylene ether has good wetting, emulsifying, dispersing, penetrating, hard water resisting, degreasing and solubilizing capabilities, and compared with an anionic surfactant, the nonionic surfactant has lower foam. Is resistant to acid, alkali and high temperature, has good chemical stability, and has fast foam eliminating speed and good effect. When the water is dispersed on the surface of a dispersoid, a film or an electric double layer is formed, so that the disperse phase can be charged, the mutual condensation of small liquid drops of the disperse phase is prevented, the surface tension of the dispersoid can be obviously reduced by polyoxyethylene ether, an emulsifying system formed by ionic liquid and lignin derivatives can be more dispersed and stabilized, the surface activity is stronger, the critical micelle concentration is lower, the hydrophilicity of a flotation reagent is improved, and the selective collection performance of the flotation reagent is enhanced; the stability of the flotation froth is enhanced, and the tension of the flotation froth is enhanced. The polyoxyethylene ether has high floatation efficiency, good adaptability to mineral mud, fragile foam, no stickiness, simple preparation of the medicament and lower cost.
The lignin derivative belongs to an anionic collector, and the cost is low. Lignin is a second rich polyphenol polymer in plants, also contains a plurality of alcoholic hydroxyl groups, carbon-based conjugated double bonds, carboxyl groups and aromatic ring structures, has good diffusion performance, but has poor water solubility, and lignin derivatives are obtained through chemical modification such as acetylation, epoxidation, methylolation, ammonification and the like, so that the water solubility and electrostatic interaction of lignin can be enhanced, and the surface activity is improved. The phenolic hydroxyl and carboxyl groups enable lignin derivatives and lepidolite to generate strong adsorption, and the space effect generated by the adsorption layer plays a strong dispersing role on lepidolite, so that flotation ore pulp is effectively dispersed, and the cover of mineral mud on the surface of lepidolite is greatly weakened. Lignin derivatives are also high-efficiency inhibitors of gangue minerals (such as calcium carbonate, sodium silicate and barite) such as silicate, sulfate and carbonate, phenolic hydroxyl groups are chemically and physically adsorbed on the surfaces of the gangue minerals, polar groups such as the phenolic hydroxyl groups and carboxyl groups extend to media to associate with water molecules, so that the surfaces of gangue particles form strong hydrophilic films to be inhibited. Similar to tannins (but tannins are inhibitors), lignin derivatives belong to organic high polymer materials, have large relative molecular mass and high branch and bend degrees, not only form a hydrophilic layer on the surface of gangue minerals, but also can mask a collector hydrophobic layer on the surface of the gangue minerals, so that the gangue minerals are strongly inhibited. The addition of lignin derivative realizes the collection of lepidolite under neutral condition, and has strong mud resistance without prior desliming.
Preferably, the ionic liquid has an anion 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 the following.
Preferably, the ionic liquid has cations 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 group or an aromatic group having 2 to 20 carbon atoms. More preferably, the substituent of the substituted alkyl group or the aromatic group includes at least one of an ether group, a ketone group, an alkenyl group, a phenyl group, a sulfonic 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 nonionic in alkaline or neutral medium, is weak cation in acidic medium, and has excellent leveling and diffusion properties. The fatty amine polyoxyethylene ether is used as a collector, has high floatation efficiency, good adaptability to mineral mud, fragile foam, no stickiness, simple preparation of the reagent and lower cost. More preferably, the polyoxyethylene ether employs a tailored AC-1815, which has greatly increased emulsifying and spreading effects.
Preferably, the lignin derivative comprises lignin sulfonate and/or an aminoenzymatic lignin. The lignosulfonate contains a phenylpropane hydrophobic skeleton and hydrophilic groups such as sulfonic acid groups, alcoholic hydroxyl groups and carboxyl groups, so that selective collection is realized, preferably, the lignosulfonate comprises at least one of oxidized, methylolated and sulfomethylated lignosulfonate, both the methylolated and sulfomethylated lignosulfonates can improve the surface activity and foaming capacity of the lignosulfonate, and the oxidizing capacity can greatly improve the adsorption capacity and dispersion capacity of the lignosulfonate and the sulfomethylation degree. The amino enzymatic hydrolysis lignin is obtained by the reaction of enzymatic hydrolysis lignin, lysine and glyoxal, and amino groups are introduced at the ortho-position of the phenolic hydroxyl groups of the lignin, so that the electrostatic interaction of the lignin can be improved.
In another aspect of the object of the present invention, there is provided the 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 as a collector in the ore pulp, and adopting the flotation processes of primary roughing, primary scavenging, secondary concentration and sequential return to obtain lepidolite concentrate.
Preferably, the addition amount of the lepidolite flotation reagent is 100-300 g/t for the primary roughing, and roughing concentrate and roughing tailings are obtained; scavenging the roughing tailings by one-time scavenging, wherein the adding amount of the lepidolite flotation reagent is 15-50 g/t, and scavenging concentrate and scavenging tailings are obtained; the first concentration, the adding amount of lepidolite flotation reagent is 20-100 g/t, and a concentrate and a middling are obtained; and (3) carrying out secondary concentration without adding lepidolite flotation agents to obtain concentrated secondary concentrate and concentrated secondary middling.
Preferably, the temperature of the flotation is between 0 and 40 ℃.
Preferably, the grade of the lepidolite raw ore is more than or equal to 0.4.
The invention can at least obtain 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, does not need to adjust pH and add inhibitors, has wide flotation temperature range, simple process, small dosage of the flotation reagent, strong selective collecting capability and mud resistance, and has obvious flotation effect on lepidolite at low temperature; the invention can realize the raw ore Li 2 Effective flotation recovery of lepidolite with O grade more than or equal to 0.4, the obtained lepidolite concentrate has grade more than 4, and Li 2 The O recovery rate is more than 70%. 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 the emulsifier, the floatation efficiency is high, the adaptability to the mineral mud is good, and the foam is fragile and does not developThe adhesive is simple in preparation and low in cost; the surface tension of dispersoids can be obviously reduced, an emulsifying system formed by the ionic liquid and the lignin derivative can be 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 collection performance of the flotation reagent is enhanced. The lignin derivative belongs to an anionic surfactant and a regulator with strong dispersion and inhibition properties, can effectively weaken the cover of mineral mud on the surface of the lepidolite mineral, strengthen the surface collecting effect of a flotation reagent and the lepidolite, can effectively inhibit gangue mineral, realize non-desliming flotation, and effectively avoid Li caused by desliming 2 O loss problem.
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 high-efficiency floatation recovery of the lepidolite ore at low temperature, improves the grade and recovery rate of the lepidolite ore, solves the technical problems of large consumption of the collector and low grade and recovery rate of the lepidolite concentrate caused by poor solubility of the traditional ammonium salt at low temperature, and has good popularization and application values.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preferred embodiment of 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 derivative. Wherein:
the ionic liquid is composed of cations and anions, wherein the cations are selected from any one or more of cations shown in formulas 2-1 to 2-12:
therein, R, R 1 、R 2 、R 3 、R 4 Each of the substituents is independently selected from alkyl or substituted alkyl or aryl with 0-20 carbon atoms, and each of the substituents 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 acid group. The anions are 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 the following. Preferably, the cation is selected from one or more of cations shown in formulas 2-1, 2-4, 2-7-2-12, wherein R, R 1 、R 2 、R 3 、R 4 At least one of them includes a substituted alkyl group or an aromatic group having 2 to 20 carbon atoms. More preferably, the substituent of the substituted alkyl group or the aromatic group includes at least one of an ether group, a ketone group, an alkenyl group, a phenyl group, a sulfonic 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 employs a tailored AC-1815, which has greatly increased emulsifying and spreading effects.
The lignin derivatives comprise lignin sulfonate and/or amino enzymatic lignin, preferably lignin sulfonate comprises oxidized, methylolated and sulfomethylated lignin sulfonate, and amino enzymatic lignin is obtained by the reaction of enzymatic lignin, lysine and glyoxal.
The application of this lepidolite flotation reagent is described below with reference to specific examples.
Li of raw ore 2 The grade of O is more than or equal to 0.4, ball milling is carried out until the granularity is 75% of-200 meshes, and water is added for size mixing to 30% of mass concentration. The amount 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 methylolated sodium lignin sulfonate. The ionic liquid comprises the following structure:
flotation test: li of raw ore 2 O content is 0.43%, grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 120g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 20g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration, the adding amount of lepidolite flotation reagent is 50g/t, a concentrate and a middling are obtained, and the middling is returned to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 20.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are as follows:
TABLE 1
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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, 10 parts of sodium hydroxymethylated lignin sulfonate, and 10 parts of amino enzymolysis lignin. Wherein, the aminated lignin is obtained by the reaction of enzymolysis lignin, lysine and glyoxal; the ionic liquid has the structure that:
r=och in ionic liquid 1 3 R=no in ionic liquid 2 2 . Ionic liquid 1:ionic liquid 2 mass ratio = 1:1.
Flotation test: li of raw ore 2 O content is 0.47%, grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 150g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 30g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration is carried out, the scavenging concentrate is concentrated, the adding amount of lepidolite flotation reagent is 60g/t, a concentrated primary concentrate and a concentrated primary middling are obtained, and the concentrated primary middling returns to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 25.+ -. 3 ℃, 15.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are as follows:
TABLE 2
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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, 8 parts of AC-181240 parts of sulfomethylated lignin sodium sulfonate and 25 parts of sodium sulfomethylated lignin sulfonate. The ionic liquid comprises the following structure:
flotation test: li of raw ore 2 O content is 0.57%, grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 200g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 25g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration is carried out, the scavenging concentrate is concentrated, the adding amount of lepidolite flotation reagent is 60g/t, a concentrated primary concentrate and a concentrated primary middling are obtained, and the concentrated primary middling returns to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 25.+ -. 3 ℃, 15.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are as follows:
TABLE 3 Table 3
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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, 11 parts of AC-183045 parts of oxidized sodium lignin sulfonate and 15 parts of oxidized sodium lignin sulfonate. The ionic liquid comprises the following structure:
flotation test: li of raw ore 2 O content is 0.66%, grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 225g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 50g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration is carried out, the scavenging concentrate is concentrated, the adding amount of lepidolite flotation reagent is 100g/t, a concentrated primary concentrate and a concentrated primary middling are obtained, and the concentrated primary middling returns to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 25.+ -. 3 ℃, 15.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are as follows:
TABLE 4 Table 4
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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, 5 parts of AC-1810 50 parts of amino enzymatic lignin, 15 parts of oxidized sodium lignin sulfonate and 15 parts of sodium lignin sulfonate. Wherein, the aminated lignin is obtained by the reaction of enzymolysis lignin, lysine and glyoxal; ion(s)The liquid being C 12 mimBr。
Flotation test: li of raw ore 2 O content is 0.53%, grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 250g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 40g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration is carried out, the scavenging concentrate is concentrated, the adding amount of lepidolite flotation reagent is 30g/t, a concentrated primary concentrate and a concentrated primary middling are obtained, and the concentrated primary middling returns to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 25.+ -. 3 ℃, 15.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are 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, 15 parts of sodium hydroxymethylated lignin sulfonate and 20 parts of amino enzymolysis lignin. Wherein, the aminated lignin is obtained by the reaction of enzymolysis lignin, lysine and glyoxal; the ionic liquid is 1-propenyl-3-butyl imidazole acetate.
Flotation test: li of raw ore 2 O content is 0.95%Grinding lepidolite raw ore, adding water to prepare ore pulp, and pouring the ore pulp into a flotation tank for a flotation test (the flotation temperature is 35+/-3 ℃).
1) The addition amount of the lepidolite flotation reagent is 180g/t, and rougher concentrate and rougher tailings are obtained;
2) Scavenging the roughing tailings for one time, wherein the adding amount of the lepidolite flotation reagent is 35g/t, and scavenging concentrate and scavenging tailings are obtained;
3) The first concentration is carried out, the scavenging concentrate is concentrated, the adding amount of lepidolite flotation reagent is 80g/t, a concentrated primary concentrate and a concentrated primary middling are obtained, and the concentrated primary middling returns to the primary roughing process;
4) And (3) carrying out secondary concentration, namely carrying out concentration on the concentrated primary concentrate without adding lepidolite flotation reagent, so as to obtain concentrated secondary concentrate and concentrated secondary middling, and returning the concentrated secondary middling to the primary concentration process.
The lepidolite ore was floated at a temperature of 25.+ -. 3 ℃, 15.+ -. 3 ℃ and 5.+ -. 3 ℃ without changing other conditions. The flotation results at each temperature are as follows:
TABLE 6
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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 (conventional cationic collector) and the rest of the experimental conditions were the same as in example 1. The flotation results at each temperature are as follows:
TABLE 8
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 35±3℃ | 3.22 | 35.54 |
| 20±3℃ | 3.04 | 33.78 |
| 5±3℃ | 2.35 | 23.85 |
Comparative example 2
The lignin derivative was replaced with tannin (inhibitor) and the rest of the experimental conditions were the same as in example 1. The flotation results at each temperature are as follows:
TABLE 9
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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. The flotation results at each temperature are as follows:
TABLE 11
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 35±3℃ | 2.34 | 32.41 |
| 20±3℃ | 2.23 | 26.75 |
| 5±3℃ | 1.45 | 20.11 |
Comparative example 4
Lignin derivatives were removed and the rest of the experimental conditions were the same as in example 1. The flotation results at each temperature are as follows:
table 12
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 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 rest of the experimental conditions were the same as in example 1. The flotation results at each temperature are as follows:
TABLE 11
| Lepidolite concentrate Li 2 Grade of O/% | Lepidolite concentrate Li 2 O recovery/% | |
| 35±3℃ | 2.11 | 22.54 |
| 20±3℃ | 2.02 | 23.12 |
| 5±3℃ | 1.96 | 20.31 |
The flotation reagent has wide flotation temperature range, strong selective collection capacity and mud resistance, and obvious flotation effect on lepidolite under the low-temperature condition; the obtained lepidolite concentrate has a grade of more than 4 and Li 2 The O recovery is greater than 70%, especially the flotation of example 2 is best. Comparative example 1 and comparative examples 1 to 5, the results show that the ionic liquid was resistant to Li at low temperature 2 The influence of the grade and the recovery rate of O is the greatest, and the low-temperature performance of the flotation reagent can be improved; lignin derivatives vs Li 2 The O grade and the recovery rate have certain influence, and the influence on the grade is larger; polyoxyethylene ether is used for preparing Li in a wider temperature range 2 Both the grade and recovery of O play a decisive role.
Finally, it should be noted that: the foregoing description is only illustrative of the preferred embodiments of the present invention, and 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 described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements or changes may be made without departing from the spirit and principles of the present invention.
Claims (10)
1. The 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 derivative;
the ionic liquid consists of cations and anions, wherein the cations are selected from any one or more of cations shown in formulas 2-1 to 2-12:
；
therein, R, R 1 、R 2 、R 3 、R 4 Each independently selected from the group consisting of 0 to20, and each substituent of the substituted alkyl group and the aryl group is 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 ci - 、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 the following.
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 formulas 2-1, 2-4, 2-7~2-12, wherein R, R 1 、R 2 、R 3 、R 4 At least one of them includes a substituted alkyl group or an aromatic group having 2 to 20 carbon atoms.
4. The lepidolite flotation reagent of claim 1, wherein the polyoxyethylene ether is an aliphatic amine polyoxyethylene ether.
5. The lepidolite flotation reagent of claim 4 wherein the fatty amine polyoxyethylene ether is 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 is lignin sulfonate and/or an aminolysis lignin.
7. The application of the lepidolite flotation reagent in lepidolite ore flotation is characterized in that after the lepidolite raw ore is ground, water is added into the ore pulp to prepare ore pulp, the lepidolite flotation reagent as claimed in any one of claims 1 to 6 is added into the ore pulp as a collector, 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 in lepidolite ore flotation according to claim 7, wherein the addition amount of the lepidolite flotation reagent is 100-300 g/t for one rougher flotation to obtain rougher concentrate and rougher tailings; scavenging the roughing tailings by one-time scavenging, wherein the adding amount of the lepidolite flotation reagent is 15-50 g/t, and scavenging concentrate and scavenging tailings are obtained; the method comprises the steps of (1) carrying out first concentration, wherein the adding amount of lepidolite flotation agents is 20-100 g/t, so as to obtain a concentrate and a middling; and (3) carrying out secondary concentration without adding lepidolite flotation agents to obtain concentrated secondary concentrate and concentrated secondary middling.
9. The use of a lepidolite flotation reagent according to claim 7 in lepidolite ore flotation, wherein the temperature of the flotation is 0-40 ℃.
10. The use of a lepidolite flotation reagent according to claim 7 in lepidolite ore flotation, wherein the grade of the lepidolite raw ore is not less than 0.4.
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