CN109647629B - Modifier combination for flotation recovery of rutile from rutile gravity middlings - Google Patents
Modifier combination for flotation recovery of rutile from rutile gravity middlings Download PDFInfo
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- CN109647629B CN109647629B CN201811550074.7A CN201811550074A CN109647629B CN 109647629 B CN109647629 B CN 109647629B CN 201811550074 A CN201811550074 A CN 201811550074A CN 109647629 B CN109647629 B CN 109647629B
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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
- B03D2201/007—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
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
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Abstract
The invention provides a regulator composition for flotation and recovery of rutile from rutile gravity concentration middlings, which belongs to the technical field of mineral separation and comprises, by weight, 5-15 parts of nitrilotriacetic acid, 1-5 parts of di-sec-octyl maleate sodium sulfonate, 50-60 parts of Pb-MOFs, and Pb (NO)3)220-45 parts. The conditioning agent provided by the invention has the advantages of small combined using amount and high selectivity, can effectively purify the flotation environment, reduce the influence of impurity metal ions on the flotation index, reduce the flotation cost, improve the quality of the concentrate product and solve the problem of waste of the traditional mineral separation collecting agent; the Pb-MOFs and the nitrilotriacetic acid in the regulator combination purify the flotation environment to a greater extent, reduce the adverse effect of impurity ions on the flotation process, improve the separation efficiency of valuable minerals and gangue minerals, and reduce the consumption of the impurity ions on a collecting agent in the subsequent flotation process; the modifier combination provided by the invention can improve the grade and recovery rate of rutile concentrate by more than 2 percent and 5 percent respectively.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a regulator composition for recovering rutile from rutile gravity separation middlings through flotation.
Background
In China, the protorutile ore has the mineralogy characteristics of low grade, fine embedded granularity of useful minerals and complex composition, so that the ore dressing practice of the protorutile ore generally adopts the combination of processes such as gravity separation, magnetic separation, electric separation, flotation and the like to obtain high-grade rutile concentrate. Production practice shows that except the flotation process, the ore treated by other beneficiation processes has thicker lower granularity limit and poorer separation effect on fine-grained minerals, and particularly, a great amount of TiO with fine granularity and TiO generated in the gravity beneficiation link2Low gradeThe middling of (1). Because the part of middling products are difficult to process and have lower price, most of the conventional ore dressing plants adopt natural stockpiling treatment measures for the products, and valuable rutile minerals are greatly lost along with the lapse of time. Experimental research shows that the flotation process is one of the most promising processes for treating the products, and the research and development of efficient beneficiation reagents are the premise that the fine-grained complex rutile flotation obtains good grading indexes. For a long time, Pb is generally adopted in the traditional rutile mineral separation field2+As activators for rutile, fatty acid based agents act as collectors to recover the rutile mineral. The conventional process has the following disadvantages:
(1) due to Pb2+The hydration capability is very strong, when the mineral is added into flotation pulp, the mineral is immediately combined with water molecules to generate hydration products, the adsorption capability of the mineral on the surface is reduced, the activation effect is weakened, and Pb must be increased to achieve better mineral separation indexes2+In turn, lead to a large amount of Pb in the wastewater discharged from the plant2+;
(2) The rutile gravity separation middlings in China contain a large number of intergrowths, and the products need to be finely ground before being treated by a flotation process, wherein the associated main nonmetallic mineral gangue is mainly silicate minerals, and the associated metallic mineral gangue is mainly Fe2O3、Al2O3CaO, MgO, etc., so that a large amount of Fe exists in the flotation pulp after fine grinding3+、Al3+、Ca2+、Mg2+And the existence of the metal ions not only consumes a large amount of collecting agents, but also plays an activating role in the flotation of silicate gangue minerals, so that the flotation environment is deteriorated, and the final rutile concentrate contains a large amount of silicate impurities to cause the waste of the flotation collecting agents.
Disclosure of Invention
In view of the above, the invention provides a modifier composition for recovering rutile from rutile gravity separation middlings through flotation, which has the advantages of low dosage, high selectivity, effective purification of flotation environment, reduction of influence of impurity metal ions on flotation indexes, reduction of flotation cost and improvement of concentrate product quality.
The invention provides a regulator composition for flotation and recovery of rutile from rutile gravity middlings, which comprises, by weight, 5-15 parts of nitrilotriacetic acid, 1-5 parts of di-sec-octyl maleate sodium sulfonate, 50-60 parts of Pb-MOFs (Metal organic frameworks), Pb (NO)3)220-45 parts.
Further, the Pb-MOFs consist of Pb2+Trimesic acid and 4, 4' -bipyridine.
Further, the Pb is2+The source of (A) is lead nitrate or lead oxalate.
Further, the composition comprises 5 parts of nitrilotriacetic acid, 3 parts of di-sec-octyl maleate sodium sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)232 parts of.
Further, the composition comprises 8 parts of nitrilotriacetic acid, 1 part of di-sec-octyl maleate sodium sulfonate, 55 parts of Pb-MOFs and Pb (NO)3)236 parts of (A).
Further, the composition comprises 10 parts of nitrilotriacetic acid, 4 parts of di-sec-octyl maleate sodium sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)226 parts of (A).
Further, the composition comprises 10 parts of nitrilotriacetic acid, 5 parts of di-sec-octyl maleate sodium sulfonate, 55 parts of Pb-MOFs and Pb (NO)3)240 parts of the components.
Further, the composition comprises 15 parts of nitrilotriacetic acid, 2 parts of di-sec-octyl maleate sodium sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)223 parts.
Further, the nitrilotriacetic acid, sodium di-sec-octyl maleate sulfonate, Pb-MOFs and Pb (NO)3)2And sequentially adding the mixture into the ore pulp.
The technical scheme provided by the invention has the beneficial effects that:
1. the conditioning agent combination provided by the invention comprises nitrilotriacetic acid with strong coordination and chelating capacity, and the nitrilotriacetic acid is added into ore pulp and can be mixed with Fe in the ore pulp3+、Al3+、Ca2+、Mg2+Chelating and coordinating impurity ions to generate hydrophilic precipitates, so that the activation effect of the impurity ions on gangue minerals is reduced;
2. the conditioning agent composition provided by the invention comprises di-sec-octyl maleate sodium sulfonate, and the addition of the di-sec-octyl maleate sodium sulfonate into ore pulp can precipitate partial metal ions and reduce the surface tension of the ore pulp to a certain extent, so that the solubility of the subsequently added Pb-MOFs in the ore pulp is increased, and the activation effect of the Pb-MOFs is further enhanced;
3. Pb-MOFs in the regulator combination provided by the invention has a three-dimensional space network structure, the Pb-MOFs is added into ore pulp and can adsorb residual impurity ions in the ore pulp, and the impurity ions enter meshes of the Pb-MOFs and are combined with oxygen atoms and nitrogen atoms with higher electron cloud density; the Pb-MOFs and the nitrilotriacetic acid synergistically act to purify the flotation environment to a greater extent, reduce the adverse effect of impurity ions on the flotation process, improve the separation efficiency of valuable minerals and gangue minerals, and reduce the consumption of the impurity ions on a collecting agent in the subsequent flotation process; in addition, Pb-MOFs can utilize lead ions of which the valence bonds on one side of the structure are not saturated to be adsorbed on the surface of the mineral, and lead ions on the other sides of the structure act with a collecting agent in the ore pulp, so that the lead ions in the Pb-MOFs obtain certain valence bond and coordination bond saturation, the hydration capacity of the lead ions is greatly reduced, the lead ions are selectively enriched on the surface of the mineral, the distribution of the lead ions in the ore pulp is reduced, and the activation efficiency of the Pb-MOFs is improved;
4. because different Pb-MOFs molecules have certain steric hindrance, only one activator of the Pb-MOFs can not completely cover the surface of rutile, so certain Pb (NO) is simultaneously added into the regulator composition provided by the invention3)2To enhance the activation effect of the combination;
5. the modifier combination provided by the invention can improve the grade and recovery rate of rutile concentrate by more than 2 percent and 5 percent respectively.
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FIG. 1 is a schematic diagram of a closed circuit test procedure for the flotation recovery of rutile from a rutile gravity middling using a combination of modifiers provided by the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
The embodiment of the invention provides a regulator composition for flotation and recovery of rutile from rutile gravity middling, which comprises 5-15 parts by weight of nitrilotriacetic acid, 1-5 parts by weight of di-sec-octyl maleate sodium sulfonate, 50-60 parts by weight of Pb-MOFs (Metal Organic Frameworks), Pb (NO) framework compound)3)220-45 parts.
The appearance of the nitrilotriacetic acid is white prismatic crystal or powder, which can provide four coordination bonds for metal ions, and the molecule of the nitrilotriacetic acid is small, so that the nitrilotriacetic acid has very strong complexing ability and can form stable chelate with various metal ions.
The sodium di-sec-octyl maleate sulfonate is a yellowish to brown viscous oily liquid, is easy to dissolve in water, has high permeability, is rapid and uniform in permeability, and has good lubricity, emulsibility and foamability.
Pb-MOFs is prepared from lead nitrate or oxalate and trimesic acid (1,3, 5-H)3BTC), 4 '-bipyridine (4, 4' -bipy) and has a three-dimensional space network structure.
In order to make the objects, technical solutions and advantages of the present invention more apparent, a combination of modifiers for flotation recovery of rutile from a rutile gravity concentrate provided by the present invention will be further described with reference to examples.
Example 1:
5 parts of nitrilotriacetic acid, 3 parts of di-sec-octyl maleate sodium sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)232 parts of.
Example 2:
8 parts of nitrilotriacetic acid, 1 part of di-sec-octyl maleate sodium sulfonate, 55 parts of Pb-MOFs and Pb (NO)3)236 parts of (A).
Example 3:
10 parts of nitrilotriacetic acid, 4 parts of sodium di-sec-octyl maleate sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)226 parts of (A).
Example 4:
10 parts of nitrilotriacetic acid, 5 parts of di-sec-octyl maleate sodium sulfonate, 55 parts of Pb-MOFs and Pb (NO)3)240 parts of the components.
Example 5:
15 parts of nitrilotriacetic acid, 2 parts of di-sec-octyl maleate sodium sulfonate, 60 parts of Pb-MOFs and Pb (NO)3)223 parts.
Example 6:
6 parts of nitrilotriacetic acid, 2 parts of di-sec-octyl maleate sodium sulfonate, 52 parts of Pb-MOFs and Pb (NO)3)221 parts.
Example 7:
13 parts of nitrilotriacetic acid, 4 parts of sodium di-sec-octyl maleate sulfonate, Pb-MOFs58 parts and Pb (NO)3)244 parts.
The ore samples processed in the embodiments 1 to 7 of the invention are middlings generated in a gravity separation link in a rutile ore dressing process in Shaanxi, a laboratory closed flotation test is adopted, the test process and a medicament system are shown in figure 1, and the specific process of the test process is as follows: grinding the re-selected rutile middlings to 88% of-0.045 mm, then making the re-selected rutile middlings into ore pulp with proper concentration, and adding H2SO41000g/t, 500g/t of carboxymethyl cellulose (CMC), 500g/t of sodium hexametaphosphate, 600g/t of regulator combination and 800g/t of sodium oleate are subjected to rough concentration to obtain rough concentrate and first tailings; making the rough concentrate into ore pulp with proper concentration and adding H2SO4Carrying out first concentration on 800g/t, 300g/t of CMC, 300g/t of sodium hexametaphosphate, 400g/t of regulator combination and 600g/t of sodium oleate to obtain first concentrate and first fine tail; preparing the first tailings into ore pulp with proper concentration and adding H2SO4Scavenging 500g/t, CMC 300g/t, sodium hexametaphosphate 300g/t, ammonium fluorosilicate 600g/t and sodium oleate 400g/t to obtain scavenging concentrateAnd second tailings; merging the first fine tailings and the scavenging concentrate, grinding the ore until the ore accounts for 85% of the ore with the granularity of-0.037 mm, and returning ore pulp obtained after grinding to the roughing operation; making the first concentrate into ore pulp with proper concentration and adding H2SO4Performing secondary concentration on 600g/t, 250g/t of CMC, 300g/t of sodium hexametaphosphate, 300g/t of regulator combination and 400g/t of sodium oleate to obtain second concentrate and second fine tail, and returning the second fine tail to the primary concentration operation; making the second concentrate into pulp with proper concentration and adding H2SO4Performing third concentration on 600g/t, 250g/t of CMC, 200g/t of sodium hexametaphosphate, 200g/t of regulator combination and 200g/t of sodium oleate to obtain third concentrate and third fine tail, and returning the third fine tail to the second concentration operation; the dosage of the medicament is based on the weight of the rutile gravity middlings entering the process.
The adding sequence of the regulator combination in the closed-circuit flotation test is that firstly, nitrilotriacetic acid is added and stirred for 2-3 minutes, then, sodium di-sec-octyl maleate sulfonate is added and stirred for 2-3 minutes, then, Pb-MOFs is added and stirred for 2-3 minutes, and finally, Pb (NO) is added3)2。
Table 1 shows TiO in rutile concentrate obtained after closed-circuit flotation using the combination of modifiers of examples 1 to 72The data in table 1 show that, after flotation of rutile gravity middlings using the modifier combination of the invention, TiO in rutile concentrates2The grade of the rutile is 86.54 to 88.67 percent, and the TiO in the rutile concentrate2The recovery rate is 77.26-80.57%.
TABLE 1 TiO in rutile concentrate2Grade and recovery rate of
The conditioning agent combination provided by the invention comprises nitrilotriacetic acid with strong coordination and chelating capacity, and the nitrilotriacetic acid is added into ore pulp and can be mixed with Fe in the ore pulp3+、Al3+、Ca2+、Mg2+Chelating and coordinating impurity ions to generate hydrophilic precipitate, thereby reducing the impurity ionsActivating gangue minerals.
The conditioning agent composition provided by the invention comprises di-sec-octyl maleate sodium sulfonate, and the addition of the di-sec-octyl maleate sodium sulfonate into ore pulp can precipitate partial metal ions and reduce the surface tension of the ore pulp to a certain extent, so that the solubility of the subsequently added Pb-MOFs in the ore pulp is increased, and the activation effect of the Pb-MOFs is further enhanced.
Pb-MOFs in the regulator combination provided by the invention has a three-dimensional space network structure, the Pb-MOFs is added into ore pulp and can adsorb residual impurity ions in the ore pulp, and the impurity ions enter meshes of the Pb-MOFs and are combined with oxygen atoms and nitrogen atoms with higher electron cloud density; the Pb-MOFs and the nitrilotriacetic acid synergistically act to purify the flotation environment to a greater extent, reduce the adverse effect of impurity ions on the flotation process, improve the separation efficiency of valuable minerals and gangue minerals, and reduce the consumption of the impurity ions on a collecting agent in the subsequent flotation process; in addition, Pb-MOFs can utilize lead ions of which the valence bonds on one side of the structure are not saturated to be adsorbed on the surface of the mineral, and lead ions on the other sides of the structure act with a collecting agent in the ore pulp, so that the lead ions in the Pb-MOFs obtain certain valence bond and coordination bond saturation, the hydration capacity of the lead ions is greatly reduced, the lead ions are selectively enriched on the surface of the mineral, the distribution of the lead ions in the ore pulp is reduced, and the activation efficiency of the Pb-MOFs is improved.
Because different Pb-MOFs molecules have certain steric hindrance, only one activator of the Pb-MOFs can not completely cover the surface of rutile, so certain Pb (NO) is simultaneously added into the regulator composition provided by the invention3)2To enhance the activating effect of the combination.
The modifier combination provided by the invention can improve the grade and recovery rate of rutile concentrate by more than 2 percent and 5 percent respectively.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. The regulator composition for flotation and recovery of rutile from rutile gravity separation middlings is characterized by comprising, by weight, 5-15 parts of nitrilotriacetic acid, 1-5 parts of di-sec-octyl maleate sodium sulfonate, 50-60 parts of Pb-MOFs and Pb (NO)3)220-45 parts.
2. The conditioning combination for flotation recovery of rutile from a rutile gravity middling as claimed in claim 1, wherein the Pb-MOFs consist of Pb2+Trimesic acid and 4, 4' -bipyridine.
3. The modulator combination for flotation recovery of rutile from a rutile gravity middling as claimed in claim 2, wherein the Pb2+The source of (A) is lead nitrate or lead oxalate.
4. The conditioning composition for flotation recovery of rutile from a rutile gravity middling as claimed in claim 3, comprising 5 parts by weight of nitrilotriacetic acid, 3 parts by weight of sodium di-sec-octyl maleate sulfonate, 60 parts by weight of Pb-MOFs, Pb (NO)3)232 parts of.
5. The conditioning composition for flotation recovery of rutile from a rutile gravity middling as claimed in claim 3, comprising 8 parts by weight of nitrilotriacetic acid, 1 part by weight of sodium di-sec-octyl maleate sulfonate, 55 parts by weight of Pb-MOFs, Pb (NO)3)236 parts of (A).
6. The conditioning composition for flotation recovery of rutile from a rutile gravity middling as claimed in claim 3, comprising 10 parts by weight of nitrilotriacetic acid, 4 parts by weight of sodium di-sec-octyl maleate sulfonate, 60 parts by weight of Pb-MOFs, Pb (NO)3)226 parts of (A).
7. The conditioning composition for flotation recovery of rutile from a rutile gravity middling as claimed in claim 3, comprising, in parts by weight, 10 parts nitrilotriacetic acid, 5 parts sodium di-sec-octyl maleate sulfonate, 55 parts Pb-MOFs, Pb (NO)3)240 parts of the components.
8. The conditioning composition for flotation recovery of rutile from a rutile gravity middling as claimed in claim 3, comprising 15 parts by weight of nitrilotriacetic acid, 2 parts by weight of sodium di-sec-octyl maleate sulfonate, 60 parts by weight of Pb-MOFs, Pb (NO) in weight3)223 parts.
9. A conditioning combination for flotation recovery of rutile from a rutile gravity middling according to claim 1 or any of claims 4 to 8, wherein the nitrilotriacetic acid, sodium di-sec-octyl maleate sulphonate, Pb-MOFs and Pb (NO)3)2And sequentially adding the mixture into the ore pulp.
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WO2011085445A1 (en) * | 2010-01-14 | 2011-07-21 | Teebee Holdings Pty Ltd | Flotation reagents |
CN104289322A (en) * | 2014-09-28 | 2015-01-21 | 安徽澳德矿山机械设备有限公司 | Chalcocite flotation agents and preparation method thereof |
CN104307642A (en) * | 2014-09-28 | 2015-01-28 | 安徽澳德矿山机械设备有限公司 | Low-grade chalcopyrite flotation agent and preparation method thereof |
CN107520058A (en) * | 2017-08-23 | 2017-12-29 | 中南大学 | A kind of rutile ore dressing composite reagent and its beneficiation method |
CN108997383A (en) * | 2018-07-18 | 2018-12-14 | 嘉兴学院 | Metal organic framework compound and its preparation method and application |
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WO2011085445A1 (en) * | 2010-01-14 | 2011-07-21 | Teebee Holdings Pty Ltd | Flotation reagents |
CN104289322A (en) * | 2014-09-28 | 2015-01-21 | 安徽澳德矿山机械设备有限公司 | Chalcocite flotation agents and preparation method thereof |
CN104307642A (en) * | 2014-09-28 | 2015-01-28 | 安徽澳德矿山机械设备有限公司 | Low-grade chalcopyrite flotation agent and preparation method thereof |
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