CN112371347B - Collecting agent for scheelite normal temperature flotation and beneficiation method - Google Patents
Collecting agent for scheelite normal temperature flotation and beneficiation method Download PDFInfo
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- CN112371347B CN112371347B CN202011288065.2A CN202011288065A CN112371347B CN 112371347 B CN112371347 B CN 112371347B CN 202011288065 A CN202011288065 A CN 202011288065A CN 112371347 B CN112371347 B CN 112371347B
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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
- B03D1/004—Organic compounds
- B03D1/012—Organic compounds containing sulfur
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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
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/082—Subsequent treatment of concentrated product of the froth product, e.g. washing
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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
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/087—Subsequent treatment of concentrated product of the sediment, e.g. regrinding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
- B03D2203/04—Non-sulfide ores
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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
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a collecting agent for scheelite normal-temperature flotation and a beneficiation method, wherein the collecting agent comprises saponified oleic acid, hydroxyoleic acid, sulfonated oleic acid and an emulsifier, wherein the mass ratio of the sum of the hydroxyoleic acid and the sulfonated oleic acid to the saponified oleic acid is (2.5-10) to (1-5). The collecting agent provided by the invention strengthens the collecting capability of scheelite in the rough concentration stage, and lays a foundation for the efficient recovery of scheelite. The beneficiation method provided by the invention replaces the conventional primary roughing, secondary scavenging and tertiary concentration processes with the open-circuit flotation process, greatly shortens the flotation process, avoids the defects of large cycle load and long process in the conventional scheelite flotation process, and realizes the high-efficiency recovery of the scheelite.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a collecting agent for normal-temperature flotation of scheelite and a mineral separation method.
Background
The tungsten ore resources mainly comprise wolframite, scheelite and wolframite and scheelite mixed ore, wherein the scheelite accounts for a larger proportion of the tungsten ore resources, and the flotation process is the most main beneficiation method of the scheelite. Because scheelite also generally contains a small amount of sulfide minerals, the removal of sulfide minerals in advance is conventionally required prior to scheelite flotation. At present, the conventional flow of scheelite flotation is 'sulfide ore removal-scheelite normal temperature flotation concentrate heating concentration'.
The normal-temperature flotation of the scheelite is usually carried out by adopting the processes of primary roughing, secondary scavenging and tertiary concentration, and middling is returned sequentially to obtain the scheelite normal-temperature flotation concentrate. However, as scheelite is often closely symbiotic with calcium-containing minerals such as fluorite and calcite, and the floatability of the calcium-containing minerals is similar, the cycle load of middlings is large during the scheelite normal-temperature flotation, and even normal-temperature flotation operation is deteriorated, so that the grade and recovery rate of the scheelite normal-temperature flotation rough concentrate are influenced. Namely, the existing scheelite normal temperature flotation has the technical defects of high cycle load of middling and long sorting process, and needs to be further improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a collecting agent for normal-temperature flotation of scheelite and a beneficiation method.
The invention adopts the following technical scheme:
the invention provides a collecting agent for scheelite normal-temperature flotation, which comprises saponified oleic acid, hydroxyoleic acid, sulfonated oleic acid and an emulsifier, wherein the mass ratio of the sum of the hydroxyoleic acid and the sulfonated oleic acid to the saponified oleic acid is (2.5-10) to (1-5).
In the prior art, oxidized paraffin soap and/or oleic acid are mostly adopted as a collector for scheelite flotation, but the collection capability is weaker, and the scheelite enrichment ratio in the conventional concentration process is low, so that scheelite with higher grade and recovery rate can be obtained by multiple scavenging and multiple concentration. The inventor researches and discovers that the saponified oleic acid, the hydroxyoleic acid and the sulfonated oleic acid are compounded and added with a proper amount of emulsifier, and the obtained collecting agent can capture more scheelite in the rough concentration stage, so that the simplified process is facilitated on the premise of ensuring the same grade of scheelite. Furthermore, the inventors found that the mass ratio of the sum of hydroxyoleic acid and sulfonated oleic acid to saponified oleic acid must be controlled within the above range, otherwise the improvement of the scheelite rougher recovery is affected and scheelite is easily lost in the beneficiated tailings in the subsequent beneficiating operation.
According to the collector for the scheelite normal-temperature flotation provided by the invention, the mass ratio of the hydroxyoleic acid to the sulfonated oleic acid is (0.5-2) to (2-8).
According to the collector for the scheelite normal-temperature flotation provided by the invention, the emulsifier is one or two of span 80, tween 60, polyoxyethylene ether and betaine.
According to the collector for the normal-temperature flotation of the scheelite, which is provided by the invention, the collector comprises the following components in parts by weight: 1-5 parts of saponified oleic acid, 0.5-2 parts of hydroxy oleic acid, 2-8 parts of sulfonated oleic acid and 1-4 parts of emulsifier.
In a preferred embodiment of the invention, the collector consists of 4 parts of saponified oleic acid, 1 part of hydroxyoleic acid, 6 parts of sulfonated oleic acid and 3 parts of emulsifier.
The invention also provides a beneficiation method for the scheelite normal-temperature flotation, which comprises a scheelite normal-temperature roughing procedure, wherein any one of the collecting agents is adopted in the scheelite normal-temperature roughing procedure.
The beneficiation method provided by the invention adopts the collecting agent in the normal-temperature rough concentration process of the scheelite, so that the collecting capability of the scheelite can be enhanced, and the recovery efficiency is improved.
According to the scheelite normal-temperature flotation beneficiation method provided by the invention, the beneficiation method specifically comprises the following steps: and performing primary white tungsten normal-temperature rough concentration on the fed ore to obtain white tungsten normal-temperature flotation rough concentrate, and performing primary concentration on the white tungsten normal-temperature flotation rough concentrate to obtain white tungsten normal-temperature flotation concentrate.
The open-circuit flotation process of 'primary normal-temperature roughing of scheelite-primary concentration of scheelite normal-temperature flotation rough concentrates' is adopted to replace the conventional primary roughing, secondary scavenging and tertiary concentration processes, so that the flotation process is greatly shortened, the problem of high cycle load of middlings is solved, and the grade and the recovery rate of the scheelite finally obtained are improved.
According to the beneficiation method for the scheelite normal-temperature flotation provided by the invention, when the primary scheelite normal-temperature rough flotation is carried out, the using amount of the collecting agent is 100-1000 g/t.
According to the beneficiation method for scheelite normal-temperature flotation provided by the invention, 1000-5000 g/t of inhibitor water glass is added and stirred for 15-60 min during primary concentration.
In the fine selection operation of the invention, the water glass is used as the inhibitor and the stirring time is prolonged, which is beneficial to the high-efficiency separation of the scheelite and the gangue minerals.
According to the beneficiation method for normal-temperature flotation of scheelite provided by the invention, the scheelite is WO30.1 to 1.0% grade ore.
The invention has the beneficial effects that:
the collecting agent provided by the invention strengthens the collecting capability of scheelite in the rough concentration stage, and lays a foundation for the efficient recovery of scheelite. The ore dressing method provided by the invention replaces the conventional primary roughing, secondary scavenging and tertiary concentration processes with the open-circuit flotation process, greatly shortens the flotation process, avoids the defects of large cyclic load and long process of middling in the conventional scheelite flotation process, realizes the high-efficiency recovery of scheelite, and improves the grade and the recovery rate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a schematic flow chart of a beneficiation method for normal temperature flotation of scheelite according to embodiment 3 of the present invention;
fig. 2 is a schematic flow chart of a conventional beneficiation method for atmospheric temperature flotation of scheelite according to comparative example 2 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Example 1
The embodiment provides a collector for scheelite normal-temperature flotation, which comprises 4 parts of saponified oleic acid, 1 part of hydroxy oleic acid, 6 parts of sulfonated oleic acid and 3 parts of emulsifier (polyoxyethylene ether) as raw materials, and the target collector is obtained by uniformly stirring and mixing the raw materials at normal temperature.
Example 2
The embodiment provides a collector for scheelite normal-temperature flotation, which comprises 4 parts of saponified oleic acid, 0.5 part of hydroxy oleic acid, 10 parts of sulfonated oleic acid and 3 parts of emulsifier (span 80), and is stirred and uniformly mixed at normal temperature to obtain the target collector.
Example 3
The embodiment provides a beneficiation method for scheelite normal temperature flotation,
wherein the average grade of the raw ore is as follows: WO3The grade is 0.55 percent, the main metal minerals are scheelite and a small amount of pyrite, the non-metal minerals are silicate gangue minerals such as fluorite, calcite, feldspar and quartz, and the raw ore belongs to low-grade scheelite.
The schematic diagram of the beneficiation flow is shown in figure 1, and the specific steps are as follows:
(1) roughing the scheelite at normal temperature: adding 1000g/t of pulp pH value regulator sodium carbonate into the white tungsten normal-temperature flotation feeding ore (namely flotation pulp for pre-selecting and removing sulfide ore) and stirring for 2min, then adding 6000g/t of gangue inhibitor water glass and stirring for 2min, and finally adding 500g/t of the collecting agent in the embodiment 1 and stirring for 2 min; carrying out primary scheelite normal temperature roughing for 6min to obtain scheelite normal temperature flotation rough concentrate and tailings I;
the yield of the scheelite normal temperature flotation rough concentrate to ore feeding operation is 36.87 percent, and the WO3Grade 1.41%, WO3The recovery rate is 94.26%; the yield of the tailings I to the feeding operation is 63.13 percent, and the yield of the tailings I to the feeding operation is WO3Grade 0.050%, WO3The recovery rate was 5.73%.
(2) And (3) white tungsten normal-temperature flotation rough concentrate concentration: adding 3000g/t of inhibitor water glass into the scheelite normal-temperature flotation rough concentrate, stirring for 30min, and concentrating for 6min to obtain scheelite normal-temperature flotation concentrate and tailings II;
the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is 6.88 percent, and the WO3Grade 7.15%, WO3The recovery rate is 89.42%; the yield of tailings II to feeding operation is 29.99 percent, and WO3Grade 0.089％、WO3The recovery rate was 4.85%.
Comparative example 1
The comparative example provides a collecting agent, and raw materials comprise 15 parts of saponified oleic acid, 1 part of hydroxy oleic acid, 6 parts of sulfonated oleic acid and 3 parts of an emulsifier.
Comparative example 2
The comparative example provides a conventional beneficiation method for scheelite normal-temperature flotation, wherein ore feeding is the same as that in example 3, a beneficiation flow diagram is shown in fig. 2, and the method comprises the following specific steps:
(1) roughing white tungsten: adding 1000g/t of pulp pH value regulator sodium carbonate into the white tungsten normal-temperature flotation feeding (namely flotation pulp for pre-selecting and removing sulfide ore) and stirring for 2min, then adding 6000g/t of gangue inhibitor water glass and stirring for 2min, and finally adding 731 (oxidized paraffin soap) serving as a white tungsten collecting agent, wherein the dosage of 731 is 300g/t and stirring for 2 min; performing primary scheelite normal-temperature roughing for 6min to obtain scheelite normal-temperature flotation rough concentrate and rougher tailings;
(2) white tungsten scavenging: adding a white tungsten collecting agent 731 into the roughed tailings obtained in the step (1) in sequence, stirring for 2min, wherein the dosage of 731 is 60g/t and 40g/t respectively, and performing two times of white tungsten scavenging for 4 min; returning primary scavenging foam to the scheelite roughing, returning secondary scavenging foam to the primary scavenging, and taking secondary scavenging tailings as final tailings;
(3) selecting white tungsten: adding 300g/t of gangue inhibitor water glass into the scheelite normal-temperature flotation rough concentrate obtained in the step (1), stirring for 2min, and carrying out primary concentration for 4 min; the primary concentration foam enters secondary concentration, and primary concentration underflow returns to scheelite roughing;
adding gangue inhibitor water glass 150g/t into the primary fine selection foam, stirring for 2min, and performing secondary fine selection for 3 min; the secondary selection foam enters tertiary selection, and the secondary selection underflow returns to primary selection;
adding 75g/t of gangue inhibitor water glass into the secondary selection foam, stirring for 2min, and performing tertiary selection for 3 min; and the third concentration foam is the final scheelite normal temperature flotation concentrate, and the third concentration underflow returns to the second concentration.
As a result, the yield of the atmospheric temperature flotation concentrate of the scheelite to the feeding operation is 7.28%, WO3Grade 6.54%, WO3The recovery rate is 86.81%; the yield of tailings to feeding operation is 92.72 percent, and WO3Grade 0.078%, WO3The recovery rate is 13.19%.
Comparative example 3
The present comparative example provides a beneficiation method of scheelite atmospheric temperature flotation, which is different from example 3 in that the collector of comparative example 1 is used.
As a result, the yield of the scheelite normal temperature flotation rough concentrate to feeding operation is 36.23%, WO3Grade 1.36%, WO3The recovery rate is 89.05 percent; the yield of the tailings I to the feeding operation is 63.77 percent, and the yield of the tailings I to the feeding operation is WO3Grade 0.095%, WO3The recovery rate is 10.95 percent;
the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is 6.67 percent, and the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is WO3Grade 6.86%, WO3The recovery rate is 82.64 percent; the yield of tailings II to feeding operation is 29.56 percent, and WO3Grade 0.12%, WO3The recovery rate was 6.41%.
Comparative example 4
This comparative example provides a beneficiation method of scheelite atmospheric temperature flotation, which is different from example 3 in that paraffin soap 731 is oxidized using a collector.
As a result, the yield of the scheelite normal temperature flotation rough concentrate to ore feeding operation is 34.23%, WO3Grade 1.47%, WO3The recovery rate is 91.06 percent; the yield of the tailing I to the feeding operation is 65.77 percent, and the yield of the WO to the feeding operation is3Grade 0.075%, WO3The recovery rate is 8.94%;
the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is 6.33 percent, and WO3Grade 7.23%, WO3The recovery rate is 82.97%; the yield of tailings II to feeding operation is 27.90 percent, and WO3Grade 0.16%, WO3The recovery rate was 8.09%.
Comparative example 5
The difference between the ore dressing method for scheelite normal temperature flotation and the ore dressing method in the embodiment 3 is that the collector is different from the collector, and the collector in the comparative example is prepared as follows:
weighing 45 parts of sulfonated oleic acid, 15 parts of hydroxy oleic acid, 5 parts of benzohydroxamic acid and 5 parts of-20 # diesel oil, mixing and stirring at room temperature for 20min, then adding 7 parts of foaming agent terpineol oil, and continuously stirring for 20min to obtain a uniform mixture. Dissolving 15 parts of sodium hydroxide in 100 parts of water, slowly adding the sodium hydroxide into the mixture, and uniformly stirring and reacting at 30 ℃ for 90min to fully saponify the mixture to obtain the sodium hydroxide.
As a result, the yield of the scheelite normal temperature flotation rough concentrate to ore feeding operation is 29.50 percent, and WO3Grade 1.69%, WO3The recovery rate is 90.55 percent; the yield of the tailings I to the feeding operation is 70.50 percent, and the yield of the tailings I to the feeding operation is WO3Grade 0.074%, WO3The recovery rate is 9.46 percent;
the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is 6.60 percent, and the yield of the scheelite normal temperature flotation concentrate to ore feeding operation is WO3Grade 7.12%, WO3The recovery rate is 85.15 percent; the yield of tailings II to feeding operation is 22.90 percent, and WO3Grade 0.13%, WO3The recovery rate was 5.39%.
From the results, the collecting capability of the collector provided by the invention on scheelite is enhanced in the rough concentration stage, and a foundation is laid for efficient recovery of scheelite. The beneficiation method provided by the invention replaces the conventional primary roughing, secondary scavenging and tertiary concentration processes with the open-circuit flotation process, greatly shortens the flotation process, avoids the defects of large cycle load and long process in the conventional scheelite flotation process, and realizes the high-efficiency recovery of the scheelite.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. The collector is used in a scheelite normal-temperature flotation process and comprises saponified oleic acid, hydroxyoleic acid, sulfonated oleic acid and an emulsifier, wherein the mass ratio of the sum of the hydroxyoleic acid and the sulfonated oleic acid to the saponified oleic acid is (2.5-10): 1-5, and the mass ratio of the hydroxyoleic acid to the sulfonated oleic acid is (0.5-2): 2-8.
2. The collector for scheelite normal temperature flotation according to claim 1, wherein the emulsifier is one or two of span 80, tween 60, polyoxyethylene ether and betaine.
3. A collector for use in the atmospheric temperature flotation of scheelite according to claim 1 or 2, wherein the collector comprises, in parts by weight: 1-5 parts of saponified oleic acid, 0.5-2 parts of hydroxy oleic acid, 2-8 parts of sulfonated oleic acid and 1-4 parts of emulsifier.
4. A beneficiation method for scheelite normal-temperature flotation comprises a scheelite normal-temperature roughing process, and is characterized in that the collector of any one of claims 1 to 3 is adopted in the scheelite normal-temperature roughing process.
5. The scheelite normal-temperature flotation beneficiation method according to claim 4, wherein the beneficiation method specifically comprises: and performing primary white tungsten normal-temperature rough concentration on the fed ore to obtain white tungsten normal-temperature flotation rough concentrate, and performing primary concentration on the white tungsten normal-temperature flotation rough concentrate to obtain white tungsten normal-temperature flotation concentrate.
6. The beneficiation method for scheelite normal-temperature flotation according to claim 5, wherein the amount of the collecting agent is 100-1000 g/t during the primary scheelite normal-temperature roughing.
7. The scheelite normal temperature flotation beneficiation method according to claim 5, wherein the primary concentration is performed by adding 1000-5000 g/t of inhibitor water glass and stirring for 15-60 min.
8. The scheelite atmospheric temperature flotation beneficiation method according to any one of claims 4 to 7,the scheelite is WO30.1 to 1.0% grade ore.
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| WO2024058981A1 (en) * | 2022-09-12 | 2024-03-21 | Ecolab Usa Inc. | Methods and compositions for lithium ore beneficiation |
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| US4208275A (en) * | 1979-01-24 | 1980-06-17 | The United States Of America As Represented By The Secretary Of The Interior | Froth flotation using lanolin modifier |
| US4366050A (en) * | 1981-01-19 | 1982-12-28 | Amax Inc. | Scheelite flotation |
| CN101269353A (en) * | 2008-05-05 | 2008-09-24 | 广州有色金属研究院 | Beneficiation method for recycling scheelite from tungsten ore rich in mispickel |
| CN101507950A (en) * | 2009-03-20 | 2009-08-19 | 中南大学 | Mineral separation process capable of recovering micro scheelite from scheelite flotation tailings |
| CN102489407B (en) * | 2011-11-30 | 2013-09-18 | 长沙矿冶研究院有限责任公司 | Mineral processing method for recycling scheelite/molybdenum oxide ores from molybdenum sulfide flotation tailings |
| CN102764700B (en) * | 2012-08-01 | 2013-09-25 | 中钢集团马鞍山矿山研究院有限公司 | Preparation method of low temperature resisting fluorite flotation collector |
| CN106311488B (en) * | 2016-10-25 | 2018-08-03 | 洛阳栾川钼业集团股份有限公司 | The beneficiation method of Fluorite recovery in a kind of white tungsten heating concentration tailing |
| CN108480055B (en) * | 2018-04-13 | 2020-11-10 | 北京矿冶科技集团有限公司 | Scheelite flotation collector and preparation method thereof |
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